Autoclaves and High Pressure Work

A U T O C L A V E S A N D
H I G H - P R E S S U R E W O R K
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PLANT MECHANICAL D R A U G H T
By W. H. M I L E S B y J . E . L I S T E R and C , H . HARRIS,
A Typical Low Pressure Works Autoclave,
A U T O C L A V E S A N D
H I G H P R E S S U R E W O R K
B y H A R O L D G O O D W I N , M . S c .
L O N D O N : E R N E S T B E N N L T D .
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P R E F A C E
T H E aim of t h i s little book is d e s i g n e d to meet

the increasing demand for practical information
on the subject with which it deals. The author
hopes he has succeeded in recording his views in
a manner which will be of real help to the ever-
w i d e n i n g c i r c l e of c h e m i s t s and engineers who are
concerned with High Pressure work.
The scope of the book is fully dealt with in

Chapter I and, therefore, there is no need to
enlarge upon the subject here; but the author
would like to avail himself of this opportunity to
tender his most grateful thanks to all t h o s e who
have helped him in various ways, and to whom
i n d i v i d u a l a c k n o w l e d g m e n t is r e c o r d e d throughout
the book.
H . G.
May, 1925.
vii
C O N T E N T S
C H A P T E R I
INTRODUCTORY 1
C H A P T E R II
LABORATORY AUTOCLAVES—CONSTRUCTION . 27
C H A P T E R III
LABORATORY AUTOCLAVES—USE . . . 47
C H A P T E R IV
SEMI-LARGE-SCALE PLANT . . . . 65
C H A P T E R V
THE CONSTRUCTION AND USE OF W O R K S AUTO-

CLAVES . . . . . . 81
C H A P T E R VI
THE HIGH PRESSURE WORKS AUTOCLAVE . 103
C H A P T E R VII
THE HEATING OF WORKS AUTOCLAVES . . 1 1 5
C H A P T E R VIII
THE WORKING OP LARGE-SCALE AUTOCLAVES . 131
C H A P T E R I X
. 151
ROUTINE RUNNING OF LARGE-SCALE PLANT
. 165
INDEX
1 * ix
L I S T O F I L L U S T R A T I O N S
no. PAGE
A typical low pressure works autoclave
Frontispiece
1. S e c t i o n of a n o n - a g i t a t o r l a b o r a t o r y autoclave 29
2. Arrangement of geared agitator on cover of
small agitator laboratory autoclave 31
3. Large agitator laboratory autoclave 35
4. y - - r •• J -- J -*- V b o r a t o r y a u t o c l a v e f o r complete
37
o. Anchor design agitator . . . . 40
6. Propeller for stirring t h i n m i x t u r e s . 40
7. A g i t a t o r for re-action requiring little stirring 41
8. G a t e a g i t a t o r for stiff pastes 42
9. D o u b l e a g i t a t o r t y p e of s t i r r i n g 43
10. G e n e r a l a r r a n g e m e n t a n d s e t t i n g of m o d e r a t e l y
69
high pressure non-agitator autoclave .
71
11. High pressure gas fire autoclave section
12. Section of high pressure agitator autoclave
73
semi-large-scale plant .
75
13. Horizontal steam-jacket autoclave .
77
14. Vertical steam-jacket autoclave—section
87
15. S e c t i o n a l e l e v a t i o n of s t e e l a u t o c l a v e
89
16. E x a m p l e of j o i n t s . . . .
91
17. A u t o c l a v e m a n h o l e lid
99
IS. H i g h pressure works pan .
107
19. Safety pressure device
109
20. Special pressure registration device .
21. Safety pressure device a n d special manometer 110
connection . . . . . . 121
22. A r r a n g e m e n t for d i r e c t firing of a n autoclave 122
«J 5* J5 3)
23. 123
24.
25. S h o w i n g " baffle " b e t w e e n f i r e b o s a n d a u t o c l a v e 125
2fi 1°6
27. S e c t i o n a l e l e v a t i o n of a s e t t i n g t o a g a s - h e a t e d
autoclave 127
I N T R O D U C T O R Y
C H A P T E R I
INTRODUCTORY
R E G A R D E D in a general way, an autoclave is a

piece of apparatus designed in order to render it
possible to heat liquids above then* boiling point,
or to carry out some chemical reaction in which
it is essential that the reacting bodies be under a
pressure greater than normal atmospheric pressure.
T h e earliest and simplest forms of autoclave were
based on the principle of Papin's digester, but at
t h e present time there is hi existence a great
v a r i e t y of t y p e s in o r d e r t o m e e t t h e v a r i e d require-
m e n t s of modern chemical processes. N o t only
are autoclaves m a d e from a number of different
m a t e r i a l s , b u t t h e sizes, general design a n d arrange-
m e n t s for heating are so varied t h a t one might well
forgive a chemist, used only to the most common
forms, for failing to recognise some of the rarer
types of modern apparatus as being autoclaves
a t all.
I n order to render this work of the greatest

possible help it is t h o u g h t best to outline at this
stage the scope of the book and the system on
which, it is written. I n the first p l a c e i t is intended
to be of an essentially practical nature, being
designed not only to describe the most important
types of apparatus or p l a n t used on high pressure
work, b u t to give to any chemist coming fresh to
this branch of t e c h n i c a l s c i e n c e j u s t t h a t practical
information which is, a l a s ! generally only learned
i n t h e s c h o o l of b i t t e r experience.
I t is, therefore, because of this outlook that

15
16 Autoclaves and High Pressure Work
very little knowledge of autoclave working is

assumed, for, after all, the word " obvious " is
really very relative. For example : to a m a n
skilled iii t h e firing of pans it is- " o b v i o u s " that
a batch m a y be maintained at a desired tempera-
t u r e , t o w i t h i n o n e degree, for h o u r s by the careful
adjustment of the fire-box door, but the author
has seen m a n y a batch ruined through l a c k of this
elementary p i e c e of t e c h n i c a l knowledge.
I t is p r o p o s e d t o d e a l first i n a g e n e r a l w a y with
the m o s t c o m m o n construction of autoclaves, to
indicate essential features and to lay down the
principles of h i g h p r e s s u r e work.
N e x t some space will be devoted to apparatus

especially designed for laboratory working both
as regards construction and use, before dealing
with w h a t is p e r h a p s the most important branch
of all—plant used for manufacture whether on a
large or small scale. There is, of course, such a
variety of designs of pressure pans that it would
b e q u i t e o u t s i d e t h e s c o p e of t h i s b o o k t o d e a l fully
with every kind, but two particular t y p e s of auto-
claves have been selected as covering the most
i m p o r t a n t r a n g e s of h i g h p r e s s u r e w o r k . These are
(1) The high pressure agitator autoclave, and
(2) The low pressure agitator autoclave of

large size.
Separate chapters will b e given to each of these

pans, in which the p l a n t will be described fully and
any points of s p e c i a l i n t e r e s t i n their working will
be emphasised.
Introductory 17
The next section will he devoted to the diffi-

culties met with in the working of autoclaves
while carrying out a variety of c h e m i c a l reactions,
a n d how best these difficulties can be obviated or
at any rate lessened.
I n conclusion, a chapter will be given to the

economical working of numbers of autoclaves so
as to utilise to best advantage the capital sunk in
such plant, and to those precautions which must
be taken when one is in charge of high pressure
pans, not only to ensure a minimum of Avear-and-
tear losses, but, what is far more important, to
safeguard in as far as h u m a n thought can, the
lives and health of the m e n engaged in working
the plant.
O B S E R V A T I O N S O N A U T O C L A V E S I N G E N E R A L
Autoclaves can be made of cast iron, steel,

copper, b r o n z e or tin, b u t some kind of s t e e l is by
far the most common material used in their manu-
facture on account of i t s g r e a t strength. Modern
practice supports the u s e of nickel steel or nickel
c h r o m e steel for those autoclaves designed to with-
stand very high pressures.
Autoclaves are made over a very large range

of sizes, f r o m s m a l l l a b o r a t o r y iîeces of apparatus
of a few hundred cubic centimetres' capacity to
huge pans capable of holding a charge of two
thousand gallons. Certain sizes, however, have
been found by practice to be most convenient, and
the following table is i n t e n d e d to show the most
general limits of different types of autoclaves as
regards capacity, temperature of heating, and

pressure. These figures must not be regarded as
rigid limits, but rather as an indication of the
extremes fixed by general experience. Special
cases always requii'e special treatment, and these
tables would not be of m u c h help had they been
m a d e t o i n c l u d e all p o s s i b l e examples.
T A B L E 1
Showing the General 'Limits of Various Types of

Autoclaves
Tomp. Pressure
T y p e of A u t o c l a v e . Capacity. Limit. Limit.
Laboratory non-agitator 500 to 500
type. 1 0 0 0 e.c. 500° C. atmos.
Laboratory non-agitator 300 to 1000

type, tubular shape. 5 0 0 c.e. 1 5 0 0 ° C. atmos.
Laboratory agitator 1000 to 300

type. 2 0 0 0 c.c. 3 0 0 ° C. atmos.
Semi-large-scale auto-
clave, agitator type (a) 5 gallons 300° C. 200 a t m .
{b) 2 0 g a l l o n s 3 0 0 ° C. 50 a t m .
Large-scale autoclave, 20O t o 400 300Q C. 100

non-agitator type. gallons atmos.
Large-scale autoclave, 700 200° C. 10

low pressure agitator gallons atmos.
type.
Large-scale autoclave, 400 300° C. 40

high pressure agitator gallons atmos.
type.
Special t y p e horizontal 500 100° C. 40
semi-large-scale agita- gallons atmos.
tor type steam-jacket
heating.
T h e c a p a c i t y figures r e f e r t o t h e a c t u a l c a p a c i t y of t h e
a p p a r a t u s , n o t t o t h e c a p a c i t y of t h e c h a r g e .
T h e pressure figures refer to t h e a c t u a l w o r k i n g pressure.
Introductory 19
A u t o c l a v e s are generally cylindrical in shape,

t l i e height bemg from two to three times the
d i a m e t e r . Tlie bottom is hemispherical in the
l a b o r a t o r y types, but rather more like a shallow
d i s h iii the larger kinds of p a n s . In order to give
s t r e n g t h . , all sharp curves or angles are excluded
f r o m the design. Wherever possible the body of
t h e autoclave is c a s t i n o n e piece, a l t h o u g h in the
m a n u f a c t u r e of works autoclaves it is impossible
t o a v o i d joints. This will be dealt with more
f u l l y w h e n these pans are being considered in
d e t a i l , b u t it is e n o u g h to note here that, although
t h e r e seems to be no theoretical objection to
w e l d i n g , most chemists who have worked auto-
c l a v e s prefer riveted ones. The top of the auto-
c l a v e , k n o w n as the cover, is fixed on to a flange,
c a s t for that purpose in the body of the pan, by
m e a n s of nuts and bolts. The joint between the
c o v e r a n d the body of the autoclave is made
a g a i n s t a ring, sunk in a groove hi the flanged top
o f t l i e body, the joint being either half or full
r e g i s t e r .
M a n y different materials are used for packing

t l i i s joint, which is often a source of leakage. It
is t h e r e f o r e of the greatest importance to have it
m a d e as gas-tight as possible. The commonest
p a c k i n g s are lead, copper, a l u m i n i u m and asbestos.
N o t o n l y does the c h o i c e of m a t e r i a l u s e d depend
o n t l i e type of autoclave, but also largely on the
p r e s s u r e it has t o w i t h s t a n d and t h e n a f a i r e of the
c l i e n i i c a l operation to be carried out inside it.
I l l t h e c o v e r s of a l l a u t o c l a v e s a r e c e r t a i n holes,
generally tapped with screw threads for particular

fittings- The number of these fittings varies with
the type of autoclave, but there are, however,
certain essentially necessary fittings c o m m o n to
all a u t o c l a v e s — s u c h as the manometer, to register
pressure, and the thermometer-tube. The latter
usually contains oil hi which the thermometer
stands, in order to give a more accurate and rapid
temperature reading of the contents of the auto-
clave.
It was at one time the custom to provide two

manometers and two thermometers, especially in
large autoclaves, the idea being to give some indica-
t i o n o f l o c a l a c t i o n if a n y t o o k p l a c e , a n d a s a proof
of t h e efficiency or o t h e r w i s e ol the agitator. As,
however, every joint is a possible source of weak-
ness, m o d e r n practice is rather in favour of one"
manometer and one thermometer-tube.
Again, it was common at one time to fix one or

more safety-valves of the ordinary steam boiler
type to an autoclave, but these were constantly
getting choked with material, either distilled or
splashed into the valve, which rendered them
useless. Devices specially designed for autoclaves
are no\v taking the place of the ordinary safety
valves. T h e most c o m m o n source of leakage in
a n a g i t a t o r a u t o c l a v e is t h e stuffing-box, t h e correct
packing of w h i c h is a most important point. The
construction of t h e stuffing-box has a considerable
influence o n its efficiency. I t is g e n e r a l l y k e p t cool
b y a water-jacket, although this is not essential
for l o w p r e s s u r e s — s a y u p to 30 a t m o s p h e r e s . It is
Introductory 21
v e r y necessary that the stuffing-box be of ample

size, a n d still more necessary that it be easily
accessible for repacking. Often a slight leak
d e v e l o p s when the full pressure is r e a c h e d , which
c a n b e overcome by tightening up the nuts that
c o n t r o l t h e j ) a c k i n g of t h e stuffing-box.
I t should be observed that these are the only

n u t s a n d bolts which it is realty safe to tighten
u n d e r pressure, for, although familiarity breeds
c o n t e m p t and workmen often do tighten up the
bolts of t h e c o v e r or m a n h o l e lid, it is a dangerous
practice, a s t h e s u d d e n s t r i p p i n g of a screw thread
m i g h t lead to disastrous results to the operator.
B e f o r e concluding these general remarks, some

space m u s t be given to the question of linings.
Theoretically, the charge should never come in
c o n t a c t with the inside of the walls of an auto-
clave, but, in practice, this excellent advice is
s e l d o m taken. Indeed, where there is no possi-
bility of chemical action between the charge and
t h e material of which the autoclave is m a d e , it is
d o u b t f u l if t h e u s e of a l i n e r is r e a l l v a necessity.
Still, i n m a n y eases repeated use causes corrosion,
w h i c h undoubtedly shortens the life of the auto-
clave. The liner is a thin-walled vessel made to
fit t h e i n s i d e of t h e a u t o c l a v e a n d i n t e n d e d t o hold
t h e charge.
T h e l i n e r s m a y b e m a d e of l e a d , s h e e t t i n , copper,
iron (plain or enamelled) or sometimes zinc. The
fixing i n p o s i t i o n of t h e l i n e r i s a s o m e w h a t difficult
o p e r a t i o n a n d o n e w h i c h it is e s s e n t i a l t o c a r r y out
correctly, f o r if t h e r e b e a n y air gaps between the
liner and the autoclave walls the transference of

h e a t will b e imperfect. This will lead t o t h e walls
of t h e a u t o c l a v e b e c o m i n g t o o h o t i n p l a c e s a n d m a y
e v e n r e s u l t i n t h e s p l i t t i n g of t h e r i v e t e d seams in
large-scale pans. In order to overcome this,
some conducting material is used between the
liner and the autoclave walls, just as oil is used
in the thermometer-tube. Paraffin w a x has been
used with some success, but has become almost
entirely superseded by solder. The autoclave is
heated slightly above the melting point of the
solder and the liner placed in position. Solder is
melted and poured round the lmer, which has
previously been filled with boiling water. W h e n
a satisfactory packing of s o l d e r h a s b e e n obtained,
the water i n t h e liner is c o o l e d b y means of a coil.
The question of the heating of autoclaves will be
considered more fully in subsequent chapters, but
it is i n t e r e s t i n g to note here that where liners are
used, t h e oil-bath for Keating t h e a u t o c l a v e becomes
almost a necessity, otherwise the local superheating
of t h e a u t o c l a v e w a l l s c a u s e s t h e s o l d e r t o m e l t and
the Imer to rise a n d j a m against the inside of the
cover.
With regard to manometers, the one which finds
almost u n i v e r s a l u s e is t h e s t e e l - t u b e t y p e . Some
are m a d e with bronze tubes, but these possess no
advantages and are inadmissible in operations in
which ammonia is evolved. In certain reactions
substances are sublimed or steam-distilled into the
manometer and cause a choke in the steel tube
itself or in t h e p i p e l e a d i n g t o t h e m a n o m e t e r . This
Introductory 23
p i p e is m a d e wide and often looped to form a trap

for such material, b u t in b a d c a s e s t h e r e is n o cure,
a n d the chemist has to be content with the tempera-
ture control. This naturally introduces an element
of d a n g e r , s i n c e o n e is w o r k i n g i n t h e d a r k a s t o the
internal pressure, and if there is a n y possibility
of r e a c t i o n s s e t t i n g i n w h i c h w o u l d c a u s e abnormal
pressure some safeguard m u s t be taken. The use
of a safety valve of t h e ordinary type would be of
little value, as this would probably choke exactly
as does the manometer. T h e only possible working
a r r a n g e m e n t w o u l d b e t h e fitting of a w i d e exhaust
pipe closed b y a cap which would blow off at the
safety limit. The operating of the device would
probably m e a n s o m e l o s s of m a t e r i a l , b u t it would,
at any rate, give some feeling of security. Con-
tingencies of t h i s description are fortunately rare.
L A B O R A T O R Y A U T O C L A V E S -
C O N S T R U C T I O N
C H A P T E R II
LABORATORY AUTOCLAVES—CONSTRUCTION
T H E laboratory autoclave, as the n a m e implies,

is a p i e c e of a p p a r a t u s d e s i g n e d f o r t h e c a r r y i n g out
of reactions under pressure on a small scale.
Although, of course, there is v e r y little difference
in size between the largest laboratory autoclaves
and the smallest semi-large-scale plant, for con-
venience of classification it is best to regard the
laboratory autoclave as designed for experimental
work rather than manufacture on even a very small
scale.
Manufacturers of laboratory autoclaves put on

the market a very large range of apparatus in
order to meet all requirements, but, as it would
be impossible in a work of t h i s size t o describe in
detail every kind, there are certain ones which m a y
be taken as characteristic types. These find very
general use in all classes of chemical work, and
serve to show the fundamental principles of
laboratory autoclave construction.
The following pieces of apparatus will therefore

be considered as illustrating very representative
examples:
(1) Small non-agitator autoclaves.

(2) Small agitator autoclaves.
(3) Large agitator autoclaves.
(4) Medium sized non-agitator autoclaves
specially d e s i g n e d for uniform oil-bath heating.
(5) Autoclaves for very high pressures and
temperatures.
(6) A u t o c l a v e s designed for special purposes.

27
Type No. 1.—The small non-agitator autoclave

is p r o b a b l y the most common type of all a n d the
one which finds most general use. I t is a cylindri-
cal steel vessel, cast in one piece a n d fitted with a
cover, which is s c r e w e d down on to the flange of
the body by means of nuts and bolts. Fig. 1
shows the general construction. I t will b e observed
that the bottom is hemispherical in order to
increase the strength. The diagram is a sectional
one. hi which the part (a) represents a raised ring
of steel on the underside of the cover. This fits
i n t o t h e s u n k g r o o v e (6) i n t h e t o p of t h e autoclave,
at the bottom of which sunk groove is a ring of
lead or copper. Hence the result of the pressure
exerted when the large nuts (c) a r e screwed down
w i l l b e t o p r e s s t h e r i n g (a) into the comparatively
soft metal of the washer, be it copper or lead.
B y this means a perfect joint is m a d e capable of
w i t h s t a n d i n g a n y pressures u p to t h e limits for the
particular autoclave. The thermometer pipe (d)
is s c r e w e d through the cover of the autoclave by
m e a n s of a s p a n n e r w o r k i n g o n t h e t o p of t h e pipe,
w h i c h is m a d e hi the form of a hexagonal nut (g).
This is d o n e by the manufacturers and, except in
rare cases, need never be interfered with. The
e a s o
pip (/)» l screwed through the cover, represents
the outlet to the pressure "gauge or manometer.
It is sometimes simply a straight steel pipe of
internal diameter i inch to § inch, or it m a y be
looped in a complete circle, the latter idea being
supposed t o r e n d e r c h o k i n g less likely.
This type of autoclave is made in a range of
FIG. I . — S e c t i o n of a X o n - a s r i t a t o r
30 Autoclaves and High Pressure Worh
sizes, but the most common is about 600 c.c,

which allows a charge of half a litre comfortably.
They are suitable for pressures up to 500 atmo-
spheres and temperatures of 500° C , but these
l i m i t s a r e w e l l o u t s i d e t h e o r d i n a r y r a n g e of organic
chemical work. It must be remembered, too,
that special manometers suitable for these high
pressures must be employed if s u c h c o n d i t i o n s are
to be carried out.
Generally spjeaking, the ordinary limits of

chemical reactions carried out in these autoclaves
would be up to 300° 0. a n d 60 atmospheres, and a
gauge capable of standing 100 atmospheres with
perfect safety would accordingly be employed.
Most gauges have a red line marking the safety
limit, and as the manufacturers allow a very
l i b e r a l m a r g i n of s a f e t y , t h e r e is n o r i s k if pressures
are kept within these limits.
The number of cylindrical nuts (c) e m p l o y e d in
an autoclave of the size described is g e n e r a l l y six
or eight.
This type of a u t o c l a v e can be heated, either by

direct flame, b y a heated oil- or solder-bath, or
electrically, although the latter method is not
usual. W h e n direct flame is employed it is
important to use a proper form of iron tripod or
metal case, the autoclave resting on a ring wliich
supports the edge of the flange {g). The bottom
of t h e a u t o c l a v e m u s t b e w e l l a b o v e t h e g a s r i n g or
w h a t e v e r t y p e of b u r n e r is u s e d , s o t h a t i t is really
heated in an air-bath, which somewhat reduced
the chances of b u r n i n g a t t h e b o t t o m and sides.
F I G . 2 . - . A r r r i v i v ^ r ^ n 4 - of G e a r e d A g i t a t o r o n C o v e r
o f >'••«;); . V . ' : • ! : : • • ' L a b o r a t o r y A u t o c l a v e .
31
If an oil-bath is used it should be a properly

constructed cylindrically shaped one, in which the
a u t o c l a v e is s u p p o r t e d o n i t s flanged edge, and with
s o m e a r r a n g e m e n t w h e r e b y i t c a n b e l i f t e d o u t of the
oil a n d allowed to drain over the bath.
For oil-bath work, however, the most satis-

factory design is t h a t to be described later under
type No. 4.
Type No. 2.—This class m a y be said to embrace

l a b o r a t o r y agitator autoclaves u p t o 1 litre capacity,
the most general sizes being COO c.c. and 1 litre.
The general construction of the body is exactly
similar to the small non-agitator type, and a
satisfactory joint is m a d e between the cover and
the body-flange by means of the raised circular
ridge working in a groove against a lead or copper
washer, exactly as described previously.
Pig. 2 shows the arrangement of t h e top of the

cover.
The general superstructure to bear the agitator
shaft is s h o w n by (a), w h i c h is s o p l a c e d that the
shaft (b) passes through the centre of the cover.
The shaft terminates at the bottom in the agitator
blade, which is o f t e n of t h e anchor type, although
m a n y other designs are in use for special require-
ments. T h e shaft passes through the top of the
cover into a heavy piece of metal (c), which is
either cast as part of the cover, or screws into it.
T h i s p i e c e of m e t a l is t o r e c e i v e t h e s t u f f i n g - b o x (d),
w h i c h is p a c k e d w i t h a s b e s t o s , c o p p e r , l e a d or some
such suitable material. A liberal size of stuffing-
box should be allowed, a n d it should be possible
Laboratory Autoclaves—Construction 33
to tighten u p after heating has commenced b y

screwing it further down. After passing through
the stuffing-box, the shaft is k e y e d on to the cog-
wheel, which is operated b y the worm-drive (e).
T h i s d r i v i n g s h a f t is l u b r i c a t e d b y v a s e l i n e c u p 3 (/)
at either end, a n d power is a p p l i e d by means of a
pulley (g) driven b y round leather belting from
shafting or a small electric motor. The arrange-
m e n t of the thermometer tube (h) and manometer
(i) requires no explanation.
I n m a n y of the first-class models all rotatory

parts are fitted with ball bearings, while two other
points of great structural importance are, (i), the
agitator should almost scrape t h e sides a n d bottom
of the autoclave, and (ii) the thermometer-tube
should be as long as possible,
These autoclaves can be heated b y direct flame,

in which case a properly constructed sheet-steel
surround with furnace-door is necessary, the heat
being supplied by a large gas-ring or Fletcher
burner, A more uniform heating is, however,
obtained if an oil-bath is used. To reduce the
possibility of local over-heating to a minimum,
some models have an arrangement whereby the
oil itself is agitated b y means of a plunger driven
b y a separate pulley off the same shafting which
Operates the stirrer.
Type No. 3.—The large-size agitator autoclave

designed for laboratory work can be obtained in a
great variety of sizes, but the most useful is that
which will comfortably take a charge of 2 litres.
This size not only enables a chemist to make a
reasonable quantity of material for subsequent

research work, but enables him also to try out a
recipe on such a scale as to give him some idea
as t o h o w t h e process will g o on t h e large scale.
The general construction of this type of auto-

c l a v e is so s i m i l a r t o t h e s m a l l e r o n e d e s c r i b e d under
T y p e N o 2 t h a t a d e t a i l e d d e s c r i p t i o n is u n n e c e s s a r y ,
Pig. 3 being self-explanatory. I t will b e seen that
t h e r e is n o f u n d a m e n t a l difference from the smaller
models in so far as the arrangements for agita-
tion are concerned. These larger autoclaves are
generally fitted with some form of v a l v e f o r releas-
ing the pressure, the arrangement shown in the
diagram being usual and, on the whole, efficient.
I t will b e seen t h a t a c o m m o n pipe serves as the

outlet to this valve and to the pressure gauge.
The advantage of having this valve fixed is two-
fold. N o t only does it form a means of releasing
pressure should anything abnormal occur, but it
can be used in certain classes of experiment for
blowing off steam at the end of the reaction,
t h e r e b y a c c e l e r a t i n g t h e r a t e of cooling. Although
one might expect these valves to block up, in
£3ractice t h e y k e e p wonderfully clear, n o r are they
a s o u r c e o f l e a k a g e if r e a s o n a b l e a t t e n t i o n is given
to them.
The diagram shows an autoclave standing in a

furnace for "direct-fire" heating, generally b y
means of g a s r i n g s . They can, however, be heated
b y electricity or in an oil-bath.
The modern practice of good firms is t o supply
the gas furnaces lined with fire-bricks, with a brick
Manometer
Lubricator Lubricator
Large cogwheel
kêyed on to shaft
Valve outlet
Stuffing box
Cover of
autoclave
Thermometer
"pipe
Agitator
Furnace
case
Opening for
'gas heater
FIG. 3.—Large Agitator Laboratory Autoclave.

35
baffle under the flue fitted to the back of the

furnace. The gas burner is such' t h a t no direct
flames impinge on the bottom or sides of the
autoclave. This type of autoclave is really an
almost perfect model of a works high-pressure
agitator pan, and is c a p a b l e of s t a n d i n g tempera-
tures up to 300° C , and pressures of 200 to 300
atmospheres.
Type No. 4.—For certain reactions, it m a y be
necessary to keep the whole of the autoclave and
cover at a uniform temperature, and under these
conditions the reaction will proceed quite satis-
factorily without agitation.
It is for such cases that the special oil-bath
autoclave about to be described is d e s i g n e d . The
capacity of the autoclaves varies from 500 c.c. to
2 or 3 litres, b u t the 1 litre size is t h e m o s t useful.
I n g e n e r a l c o n s t r u c t i o n i t is s i m i l a r t o t h e standard
non-agitator autoclaves, except that it is not
usually built quite so substantially, being designed
m o r e f o r t h e l i m i t of 2 0 0 a t m o s p h e r e s p r e s s u r e and
temperatures u p t o 300° C. The method of fitting
the cover and the arrangement of m a n o m e t e r and
thermometer-tube present no modification. The
chief p o i n t of i n t e r e s t t o o b s e r v e is, t h a t the auto-
clave rests on a number of l u g s (a) cast or riveted
to the sides of t h e oil-bath. This latter is of such
a size that the autoclave can be completely
immersed in oil or other heating m e d i u m to a
depth of 1 inch above the cover. The plates (b)
are of steel and are arranged to swivel in order
that the autoclave flange can be m a d e to rest on
FIG. 4.—Xon-Agitator Laboratory Autoclave for
C o m p l e t e Oil I m m e r s i o n ,
37
38 Atitoclaves and High Pressure Work
them when it is desired to stop the experiment,

and withdraw from the bath. T h i s is particularly
convenient, as it not only enables most of the
surplus oil to drain back into the bath, but also
forms a u s e f u l m e t h o d of s u p p o r t w h e n u n d o i n g the
large round nuts preparatory to removing the
cover. T h e heating of the oil-bath is best per-
formed b y means of a l a r g e r i n g burner.
Tupe No. 5.—It has been shown that the limits

of pressure and temperature possible with the
types of ax>paratus previously described are very
high, in fact higher than is usually required hi
research work on synthetic dyestuffs, or general
organic chemistry. It is sometimes necessary,
however, to carry out reactions under pressures
higher even t h a n 500 atmospheres a n d temperatures
above 500° G.
For these cases, special apparatus must be

employed which m a y be regarded as autoclaves,
although they are really m o r e in the nature of
electric furnaces, especially where very high
temperatures are required. N o general principles
can be laid d o w n for t h i s t y p e of v e s s e l . It must
vary greatly according to the kind of work for
which i t is designed.
One example is a steel vessel of about 3 litres

capacity, fitted with adjustable electrodes at the
top a n d bottom. T h e heating medium is a
graphite rod or tube with nickel water-jacketed
holders. T h e whole s t e e l v e s s e l is itself immersed
hi a water-jacket of cast iron or steel. A valve
passes through this water-jacket from the inner
steel vessel to the air. Sometimes this valve is

fitted with a quartz; window so that it is possible
t o v i e w t h e i n t e r i o r of t h e s t e e l v e s s e l w h e n working
at high pressures and -temperatures.
It is p o s s i b l e to obtain internal temperatures of

1500° C. w i t h this type of autoclave and pressures
u p t o 1 0 0 0 a t m o s p h e r e s , a l t h o u g h i t is n o t safe t o go
a b o v e 5 0 0 a t m o s p h e r e s if t h e q u a r t z w i n d o w i s fitted.
If v e r y high pressures b u t t e m p e r a t u r e s n o t above

5 0 0 ° C. a r e r e q u i r e d , i t is p o s s i b l e t o u s e apparatus
of more orthodox design in which the heating
medium is a gas furnace. The points of interest
to note in considering this type of apparatus are
(1) that only a very good-quality high-speed tool

steel is u s e d in the manufacture of the autoclave,
(2) the walls of the autoclave are very thick, (3)
the height of the autoclave is very m u c h greater
in proportion to its diameter than with ordinary
models. This means that for a n y given capacity
t h e d i a m e t e r of t h e r i n g u s e d t o m a k e a , j o i n t between
the cover and the body is m u c h less, thereby
r e d u c i n g t h e p o s s i b i l i t y of l e a k a g e . In other words,
the apparatus approaches more to the dimensions
of a steel tube. Again, all the bolts which screw
the cover to the body a r e of h e a v i e r design, and a
c o p p e r o r e v e n a soft steel r i n g is u s e d t o m a k e the
joint.
These autoclaves are non-agitator and can be

m a d e capable of withstanding pressures up to
1000 atmospheres.
T h e h e i g h t of t h e b o d y is from six to ten times

the internal diameter.
Type No. 6.—In addition to those autoclaves
specially designed for very high temperatures and
pressures, there are numerous models which are
normal in so far as their pressure and temperature
limits are concerned, but which depart from the
standard types in other respects. For example,
FIG. O.—Anchor Design F i o . 6.-—Propeller for Stirring

Agitator. . Thin Mixtures.
t h e r e is t h e q u e s t i o n of a g i t a t i o n . B y far the most
common type of agitator used in laboratory auto-
claves is the anchor design, which gives efficient
stirring for all o r d i n a r y p u r p o s e s . A great advan-
t a g e of t h i s t y p e of a g i t a t o r is t h a t i t c a n be m a d e
to sweep within ^ inch, or less, of the sides, thus
preventing the accumulation of solid crusts and
consequent burning of the same. Again, the

thermometer pipe can be m a d e to slope within the

space between the shaft a n d wings of the anchor,
thus getting very near to the bottom of the p a n
(Fig. 5). The disadvantage of the anchor type of
agitator is that, with thick pastes, the inside
portions are only imperfectly stirred. For really
17b valve
Discharge
'pipe
Fra. 7 . — A g i t a t o r for R e a c t i o n requiring

little Stirring.
e f f i c i e n t s t i r r i n g of t h i n m i x t u r e s , s a y a n oil a n d a n
aqueous l a y e r , t h e r e is n o t h i n g b e t t e r than a good
propeller (Fig. 6). This causes up and d o w n
agitation as well as the usual circular whirlpool
kind, but it is n o t very efficient with thick pastes.
Fig. 7 shows a n agitator a r r a n g e m e n t for a reaction
i n w h i c h v e r y little s t i r r i n g is n e c e s s a r y , b u t where
9*
i t m a y b e r e q u i r e d t o b l o w off s a m p l e s of t h e batch
from time to time during the c o u r s e of t h e experi-
ment. A f u r t h e r a d v a n t a g e of t h i s t y p e of agitator
is that very small batches can be made, as the
thermometer pipe comes almost to the bottom of
the vessels.
F I G . 8.—Gate A g i t a t o r for Stiff Pastes.
Ci
F o r t h e a g i t a t i o n of stiff p a s t e s a f u r t h e r gate "
is s o m e t i m e s fitted to the anchor type (Fig. 8), or
a double agitator autoclave is used. This latter
is a n excellent device for high-speed agitation of
any sort, and is perhaps the best of all systems
where very vigorous agitation is e s s e n t i a l and the
pressures are low. As will b e seen in F i g . 93 both
a g i t a t o r s a r e d r i v e n off t h e s a m e p u l l e y i n opposite
Laboratory Airfodaves—Construction 4 3
directions, t h e t o p b e v e l c o g (x) operating one, a n d

the b o t t o m (y) the other.
A n o t h e r type of a u t o c l a v e worthy of m e n t i o n is
that with which i t is p o s s i b l e to introduce, or t o
Outer agitator Inner agitator driven

driven <ff? inner off outer shaft from
shaft from "Reared wheel y
geared wheei oc
FIG. 9.—Double Agitator Type of Stirring.

The g l a n d s z should be packed so as to stop leakage
not only between the outer shaft a n d t h e outside,
b u t also b e t w e e n t h e t w o shafts themselves, otherwise
t h e c o n t e n t s of t h e a u t o c l a v e will b e d r i v e n u p a n d l e a k
into t h e gland. T h i s t y p e of p a n i s o n l y s u i t a b l e f o r
low p r e s s u r e .
extract, a gas while working at high pressures.

The autoclaves are generally of about 500 c.c.
capacity, of special steel a n d capable of with-
standing pressures of 500 atmospheres and

temperatures u p to 500° C.
They are supplied with manometer, thermometer-
tube and two valves, connected to inlet a n d outlet
pipes respectively. The inlet pipe passes down to
the bottom of the autoclave and the outlet to the
top.
There a r e , of course, m a n y other types of auto-

clave, and makers of scientific apparatus are
generally quite willing to discuss the requirements
of their clients and to design for special needs.
For example, the author would mention in this
connection the firm of C h a s . W . Cook and Son, of
Ashhy-de-la-Zouch, whose autoclaves he has used
with complete satisfaction for m a n y years. Some
of t h e t y p e s d e s c r i b e d i n t h i s c h a p t e r a r e illustrative
of t h e i r s t a n d a r d models.
L A B O R A T O R Y A U T O C L A V E S - U S E
CHAPTER III
LAB0KAT0KY AUTOCLAVES—USE
W H I L S T there are a great variety of chemical

reactions which are best carried out in autoclaves,
or for w h i c h a u t o c l a v e s a r e , if n o t essential, at a n y
rate desirable, three m a y be taken as illustrative
of high pressure work. It should, however, be
explained that the term " h i g h pressure " means
pressure above the normal atmospheric pressure,
and not necessarily great pressure as measured hi
lbs. per s q u a r e inch.
The three chemical reactions to be considered

are :
(1) The substitution of a h y d r o x y - g r o u p for

a sulphonic acid group.
(2) T h e s u b s t i t u t i o n of a n a m i n o - g r o u p f o r a
hydroxy-group or a halogen group.
(3) The introduction of one or more alkyl
groups into an amino-group.
The particular types of apparatus most suitable

for t h e s e r e a c t i o n s differ very greatly one from the
o t h e r , a n d i t is b e c a u s e of t h i s t h a t t h e s e examples
have been selected.
(1) The first is t h e well-known caustic fusion or
" m e l t " p r o c e s s , w h i c h is of s u c h g r e a t importance
in the manufacture of intermediates for azo-
dyestuffs. Generally speaking, the process consists
in melting a certain calculated quantity of caustic
soda or potash, either in the autoclave itself, or
in s o m e o t h e r suitable vessel for transference to the
autoclave. The melted alkali is then raised to a
47
certain temperature, which naturally varies with

the particular process, a n d the sulphonic acid, say
of the naphthalene series, or its sodium salt is
charged in. This substance m a y be in t h e form of
a dried powder or a stiff paste; in a n y case, it
probably contains a large proportion of inorganic
salts such as sodium chloride or sulphate. W h e n
all h a s been added, the resultant mixture is a stiff
paste, and will probably be a stiff paste even at
the temperature of the reaction; moreover, the
inorganic salts will be out of solution. These
points should be considered hi the choice of the
autoclave, for to carry out such a reaction in a
non-agitator autoclave heated b y direct flame
would certainly cause local burning a n d uneven
mixing of the charge. Possibly some parts would
be melted to dihydroxy-derivatives, if t h e starting
material contained more than one sulphonic acid
group, whereas there would be unchanged sulphonic
a c i d i n t h e c e n t r e of t h e autoclave.
B y t h i s i t is n o t m e a n t t h a t it Avould b e impossible
to carry out such operations in non-agitator direct-
fired laboratory autoclaves, but rather that such a
piece of apparatus would not be desirable, much
less ideal.
Since most of the caustic fusion recipes given

in such works as Cam's " Manufacture of Inter-
mediate Products for Dyes " for working in auto-
claves recommend the use of caustic soda of from
2 5 % to 5 0 % strength, and temperatures below
2 0 0 ° C.? it f o l l o w s that the pressures generated will
Laboratory Autoclaves—Use 49
not be very high. For this type of reaction the

pressures rarely exceed 10 a t m o s p h e r e s , so there is
absolutely no reason w h y agitator autoclaves
should not be used.
As the paste is fairly stiff, the type of the

agitator most likely to do its work thoroughly
is the anchor design, supplemented perhaps by
; ,?
an inside " gate (Figs. 5 and 8). The speed of
agitation need not be h i g h — i n fact to attempt high
speed would be to risk b e n d i n g the agitator blades,
so, all t h i n g s considered, a n anchor agitator auto-
clave of capacity, say, A to 1 litre, driven by a
worm gear, and heated hi a n oil-bath, would be the
m o s t s u i t a b l e for a p i e c e of r e s e a r c h w o r k involving
caustic fusions.
Before c o n s i d e r i n g d e t a i l s of c l o s i n g u p , heating,
a n d opening laboratory autoclaves which are
m u c h the same whatever the nature of t h e opera-
tion performed in t h e m , let u s briefly t o u c h on the
special requirements of chemical reactions (2) and
(3).
(2) The operation of substituting an amino-

g r o u p for a hydroxy- or a halogen-group is known
as amidation. The usual p r o c e d u r e is to h e a t the
hydroxy- or halogen-derivative with ammonia,
either aqueous or alcoholic, w i t h or w i t h o u t sodium
bisulphite, at temperatures sufficient to give a
p r e s s u r e o f 6 to 1 0 a t m o s p h e r e s . Typical examples
of t h e s e r e a c t i o n s c a n b e s e e n i n a n y organic text-
book, the following being fairly representative of
t h i s c l a s s of w o r k :
(a) the preparation of

N H 2 CI
S 0 3a H - ( > S 0d 3 H
from \ .
N 0 2 N 0 2
(b) the preparation of
/ X
/ \ l N H 2 . / V > O H
^ from
(c) the preparation of

S 0 3 H SO3H
2
I from
H e r e , t h e n , w e h a v e a final mixture after charg-

ing, w h i c h is m u c h t h i n n e r t h a n t h e c a u s t i c fusions,
and which w h e n on temperature m a y c o n s i s t of an
oil a n d an aqueous solution [example (6)]. If this
operation were carried out in a non-agitator
autoclave, poor and inconsistent yields would,
without doubt, be o b t a i n e d , and even if t h e agita-
tion were of t h e slow whirlpool t y p e recommended
for caustic fusions, it w o u l d hardly b e sufficient to
c o p e w i t h t h e n e e d s of t h e case.
T h e pressures, again, are not high, although
a m m o n i a is one of the most " searching " of all
gases, a n d m a n y a gland which is perfectly tight
to steam shows a leak to ammonia. Still, t h a t can
be dealt with, a n d t h e pressure will be a diminishing
one as the amidation proceeds, Undoubtedly the
type of a g i t a t o r most suitable for the whipping up
of a n oil a n d water is t h e propeller, although the
twin agitator shown in Pig, 9 would probably be

satisfactory if the glands did not leak. A worm-
d r i v e is n o t n e c e s s a r y , n o r altogether desirable, for
bevel cogs would give a greater speed of agitation
without having to run the pulley too fast. Since
t h e a g i t a t i o n w i l l k e e p t h e c o n t e n t s of t h e autoclave
in constant movement, it would be quite possible
to work satisfactorily with direct heating, the
advantage being, of course, speed of heating up.
There is n o t h i n g to be said against oil-bath work,
however, if p r o p e r l y carried out, and i t is perhaps
easier to keep strictly to temperature conditions
w h e n a n o i l - b a t h is u s e d . O n a c c o u n t of t h e action
of a m m o n i a o n c o p p e r i t is e s s e n t i a l t h a t t h i s metal
be not used, either for packing rings, washers or
in the gauge. A lead ring for the cover, asbestos
packing for the gland and steel-tube gauges are
a satisfactory c o m b i n a t i o n for amidations.
(3) Examples of this type of reactions are as

follows :
N H - C H 3 N < x S *
(a) The preparation of | | or j ]
from aniline.
(6) The preparation of ethyl a-naphthyl-
amine from a-naphthylamine.
Further examples could be quoted in large

numbers, as these reactions are simply typical
cc
methylations " or " ethylations."
T h e m o s t c o m m o n m e t h o d s of i n t r o d u c i n g m e t h y l -
or ethyl-groups into a n amino-group are treatment
of the a m m o - b o d y either with methyl or ethyl

alcohol a n d a mineral acid, or w i t h the methyl or
ethyl esters of mineral acids, such as methyl
sulphate or ethyl chloride.
Although m a n y methylations and ethylations

can be carried out under ordinary pressure, there
are a great m a n y commercial recipes in constant
use in the chemical industry which involve the use
of autoclaves.
I n working recipes involving the use of dilute

mineral acid the autoclave must naturally be pro-
vided with a liner, and all steel p a r t s protected in
order to avoid corrosion of the autoclave and the
development of enormous pressures b y reason of
the hydrogen evolved. If sulphuric acid is used,
it is p o s s i b l e t o e m p l o y l e a d a s a p r o t e c t i v e material,
but in most cases an enamelled cast-iron liner is
more satisfactory. The mixture of the amino-
compound (or its sulphate or hydrochloride),
mineral acid a n d alcohol often forms a homogeneous
whole. Accordingly this type of operation can
often be carried out in a non-agitator autoclave
just as easily and completely as in an agitator
one, which is a great advantage, considering the
difficulty in * securing adequate protection of
the* steel autoclave from the searching acid
vapours.
Sometimes methylations or ethylations are

carried out b y heating a mixture of the amine,
methyl or ethyl chloride a n d milk of lime, the
function of the latter being to absorb the acid
formed in the reaction. I n this case, a n agitator
autoclave would be used, but it would not be

necessary to employ the enamel liner.
In order to. follow exactly the procedure most

l i k e l y t o e n s u r e t h e s u c c e s s f u l w o r k i n g of laboratory
autoclaves, let us take a typical case—say of the
caustic fusion of a sulphonic acid or amino-
sulphonic acid of the naphthalene series to the
corresponding hydroxy-compound—and go over
carefully every step taken.
The autoclave chosen for the work will be an

agitator one of from 600 to 1000 c.c. capacity,
the type of agitator being a simple anchor, or
an anchor reinforced with an inside gate. The
autoclave will be worm-driven and heated in an
oil-bath.
The size of the batch will be regulated so that

the complete charge before sealing up occupies
three-quarters to four-fifths the total capacity of
the autoclaves. This is v e r y important as, owing
t o t h e e x p a n s i o n of l i q u i d s o n h e a t i n g , if t h e charge
be too great, enormous pressures will b e generated
when the high temperature is reached.
T h e a u t h o r h a s k n o w n of c a s e s i n w h i c h t h e screw
t h r e a d s of t h e m a n o m e t e r and even the cover bolts
have been stripped owing to the neglect of this
precaution. In carrying out a series of experi-
ments it is important to keep the sizes of the
batches approximately constant, for the golden
rule in research work is to alter one factor, and
one factor only, at a time. In spite of m u c h that
h a s b e e n w r i t t e n t o t h e c o n t r a r y , it is q u i t e possible
to carry out caustic fusions in a steel autoclave
54 Autoclaves and S i g h Pressure Work
without t h e u s e of a l i n e r , p a r t i c u l a r l y if t h e fusion
of t h e rock caustic with the necessary quantity of
w a t e r is d o n e in a c a s t - i r o n vessel, a n d , w h e n melted,
transferred to the autoclave. If the liner is
properly fitted with solder into the b o d y of the
autoclave there can, of course, be no possible
objection t o t h e u s e of it.
Let us suppose, then, that the calculated

quantity of caustic soda a n d water has been fused
together a n d transferred to the autoclave, a n d the
sulphonic acid or its sodium salt is weighed out
ready for charging. As the resultant mixture will
p r o b a b l y b e f a i r l y stiff, i t w i l l p e r h a p s b e advisable
to h a v e t h e a u t o c l a v e in its oil-bath a n d s o m e heat
applied in order to end up with a mixture at 70° C.
or higher. Naturally no hard-and-fast rule can be
laid d o w n o n this point, for so m u c h d e p e n d s o n the
particular recipe, but the final temperature before
sealing up should be as low a s is c o m p a t i b l e with
proper mixing of t h e charge.
W h e n all t h e sulphonic acid has been a d d e d , the

mixture will be a thick cream, and the operation
of closing the autoclave is n o w begun. This is a
very important stage and one which m a y easily be
carried out incorrectly by inexperienced hands.
In the first place, it is important to see t h a t the
sunk ring in the body flange of the autoclaves,
on to which the raised rim on the cover presses, is
in perfect condition and quite clean. This ring
is generally m a d e of lead for most laboratory
purposes, although for very high pressures copper
is b e t t e r . T h e c o v e r is p l a c e d over the r o u n d bolts
Laboratory Autoclaves—Use o5
on to the body flange and shaken about to ensure

that it is " s i t t i n g " nicely. Then the large round
nuts are threaded down until they just begm to
grip. U p to this stage nothing b u t the fingers has
: i
been necessary, but n o w two stout t o m m y bars ''
should be used. One of t h e s e is s l i p p e d alongside
the round nuts and the other threaded through the
circular hole in one nut. Pressure is n o w exerted
so as to tighten u p that one n u t b y half a revolution.
The bars are withdrawn and the nut immediately
opposite to the one first tightened is n e x t turned.
In this way all t h e n u t s a r e in t u r n screwed down,
always going from any nut to the one immediately
opposite to it. W h e n all the nuts have been so
treated twice, the procedure is c h a n g e d , and the
nuts are screwed down one after the other, passing
round and round the cover until it is impossible
to screw a n y nut down a n y further. I t is a b s o l u t e l y
unnecessary to use a h a m m e r to tighten up a
laboratory autoclave, and such a procedure only
risks stripping the thread of the screws. The
autoclave is n o w h e a t e d u p , t h e a g i t a t o r b e i n g run
at a steady continuous speed. Unless there is
some special reason to the contrary, it is a s well
to heat u p to the correct temperature as quickly as
possible, which m a y take any time from one to
six hours.
The raising of a n autoclave to temperature and

the subsequent maintaining of it a t that tempera-
t u r e is b y n o m e a n s a n e a s y o p e r a t i o n , b u t o n e that
requires considerable experience. Still, it is possi-
ble to give some hints as to h o w to set about the
task without claiming that the method described is

the only practicable one.
I n the present case let us suppose t h a t t h e desired
internal temperature of t h e b a t c h is 1 8 0 ° C , which
is a fairly representative figure for this class of
chemical action. The temperature of t h e oil-bath
containing the autoclave would be raised steadily
to this figure, which might take from one to two
hours. As there is always a " lag " or difference
in t e m p e r a t u r e between the oil-bath and the inside
of the autoclave, even when both are perfectly
constant and s t e a d y , t h e r e is n o r i s k r u n in raising
the oil-bath straight away to the desired tempera-
ture. A t this point the inside temperature of the
batch will be perhaps 120° C , as shown b y the
thermometer placed in the thermometer-tube
which has previously been partially filled with oil.
A n a t t e m p t is n o w m a d e t o s t e a d y t h e temperature
of t h e o i l - b a t h b y a d j u s t m e n t of t h e g a s o r electric
heating appliances, the object being to slow off
the rate of h e a t i n g of t h e oil-bath and to bring its
temperature to about 10° to 20° C. above the
desired internal temperature of t h e c h a r g e . While
this is being done, the temperature of the charge
in t h e a u t o c l a v e rises steadily, a n d finally comes to a
figure about 10° to 40° C. below that of the oil-
b a t h a t w h i c h it is c o n s t a n t . T h e difference between
the two temperatures when both are steady is the
:c
lag," a n d depends on the capacity and the design
of t h e a p p a r a t u s . W h e r e t h e l o s s of h e a t b y radia-
tion from oil-bath and autoclave top is low, the
" l a g " i s s m a l l , a n d vice versa. Let us suppose we
Laboratory Autoclaves,—Use 57
have reached a position of steadiness a n d equili-

brium., the oil-bath being 195° C and the ther-
m o m e t e r in the autoclave tube showing 175° C ,
i.e., 5° too low. W e n o w slightly increase the heat
on the bath a n d wait till i t comes up and remains
steady at 200° C. W h e n this has occurred it is
probable that there has been no change in t h e
autoclave thermometer reading, but we m u s t be
patient, for t h e heat takes some time to pass from
the bath and raise the temperature of the large
mass of a u t o c l a v e a n d charge. Only when we are
sure that the full effect of our heating of the oil-
b a t h .has b e e n reflected in t h e t h e r m o m e t e r reading
of the autoclave should w e consider a further
i n c r e a s e o r d e c r e a s e i n h e a t o n t h e b a t h if required.
It is essential that a chemist should be m o s t

systematic a n d patient if h e is t o a c q u i r e a n y skill
in regulating autoclaves, particularly those heated
in oil-baths.
Once the autoclave has been got " on tempera-

ture " the maintenance of i t a t t h a t d e g r e e of heat-
is a simple matter provided one remembers that
one m u s t never m a k e s u d d e n a n d drastic alterations
in the heating a n d m u s t always w a i t for t h e effect
of a n y c h a n g e t o s h o w o n t h e a u t o c l a v e thermometer
before making further adjustments. It is sur-
prising h o w little an alteration in gas supply to
the burner is n e e d e d hi order to cause a rise or fall
of 5 ° o n t h e a u t o c l a v e thermometer.
It is advisable to keep a r e c o r d of the progress

of the experiment in the form of a chart, the
following being a typical example.
T e m p , of T e m p , of
oil-bath. charge. Pressure.
A s s o o n a s t h e t i m e for t h e h e a t i n g of t h e charge
at full temperature is over the heat is turned off
and t h e a u t o c l a v e is a l l o w e d to cool. The practice
of c o o l i n g v e r y q u i c k l y i n w a t e r is n o t t o b e recom-
m e n d e d except in cases of emergency, as it is
liable to cause strains m t h e s t e e l of t h e autoclave.
In addition, it is a procedure which it would be
hnpossi ble to imitate on a large scale. It is,
however, quite reasonable to lift the autoclave
from its "bath and allow it t o cool in t h e a i r of the
laboratory. T h e chart should be filled up during
cooling, a n d this m a y yield valuable evidence in
some experiments.
As regards opening the autoclave, this is an

operation of some danger unless done correctly,
especially if t h r o u g h the evolution of a gas during
the reaction there is a residual pressure shown on
the gauge even when the autoclave is quite cold.
Nevertheless if c a r r i e d out properly accidents need
Ci
never occur. The first step is t o insert t h e t o m m y
bars " which were used for tightening up, one
between the big round nuts to steady the autoclave
on its stand, and the other through one particular
nut. Reference to the diagrams will show these
nuts to h a v e circular holes in t h e m a n d the " t o m m y
bars " are m a d e just to fit these holes tightly.
A l t h o u g h it was possible to tighten up an autoclave
cover without the u s e of a h a m m e r , it is generally
necessary to hit the t o m m y bar smartly with a

2 lb. h a m m e r in order to loosen the nut. T h e
m o m e n t the nut is l o o s e n e d ever so slightly i t is left
a n d the operation carried out on the adjacent nut.
I n this manner all t h e n u t s are loosened, b u t unless
there is a huge residual pressure—say 20 atmo-
spheres—the c o v e r will b e so e m b e d d e d in t h e lead
ring that there will b e no apparent diminution in
the pressure on the gauge. W h e n all the nuts
have been loosened they are unscrewed slightly—
say half a revolution—and the edge of a well-
sharpened cold chisel is p l a c e d b e t w e e n the flange
of t h e c o v e r a n d t h a t of t h e a u t o c l a v e . On driving
this h o m e with a few smart blows the cover is
eased in the lead ring and the gas causing the
r e s i d u a l p r e s s u r e , if a n y , e s c a p e s h a r m l e s s l y without
splashing the charge over the operator. E v e n if
' t h e r e is n o residual pressure shown, this procedure
should b e always adopted, a s o f t e n t h e r e is a slight
puff of gas when the cover is eased which would
m e a n t h e p r o b a b l e l o s s o f s o m e o f t h e c h a r g e if the
cover should be taken off carelessly. Once the
operator h a s a s s u r e d h i m s e l f t h a t t h e c o v e r is eased
a n d that a n y pressure in the autoclave has been
relieved, then the large nuts are quickly unscrewed
a n d t h e c o v e r is e n t i r e l y lifted off.
The author has opened autoclaves showing from

300 to 400 lb. per sq. inch residual pressure with
perfect safety b y adopting the method just
described.
T o s u m up, it should be observed that there
are certain golden rules governing the successful
use of laboratory autoclaves^ and although skilled

and experienced chemists m a y depart from these
and still o b t a i n satisfactory results, that does not
alter the fact that b y so doing they are taking a
risk which m a y lead to unreliable a n d untrust-
worthy work.
T h e s e rules c a n be s t a t e d briefly as follows :
(1) E m p l o y an agitator autoclave wherever

possible, a n d always where the starting mixture
or final r e a c t i o n p r o d u c t is n o t homogeneous.
(2) E m p l o y an oil-bath as the heating medium

wherever possible, and always where a solid is
likely to separate out during the course of the
reaction.
(3) K e e p accurate records of t h e temperature of

the oil-bath, temperature of the mixture and
pressure. These observations should be charted
every half-hour.
(4) Try to regulate the size of the batches to
occupy 7 0 % to 8 0 % of the capacity of the auto-
clave w h e n fully charged before heating up.
(5) R e m e m b e r that time spent in correctly

tightening u p the bolts which hold the cover to
the body of the autoclave so as to ensure an even
p r e s s u r e o n t h e r i n g is w e l l spent.
(6) Get the mixture to the proper reaction
temperature as quickly as possible without taking
risk of burning. It is safer to force an agitator
autoclave t h a n a non-agitator. In special cases it
m a y be necessary to heat u p slowly in order to cause
a r e a c t i o n t o t a k e p l a c e o v e r a r a n g e of temperature
to avoid getting too high pressures.
(7) Never tighten up a n y nuts and bolts except

those on the stuffing-boxes w h e n the contents of
the autoclave are under pressure.
(8) Never depart from the correct method of

opening an autoclave as previously elaborated.
It is perfectly safe to open an autoclave with
residual pressure inside if t h e proper procedure is
adopted, but the careless opening of one con-
taining caustic soda m a y cause the operator to
lose his sight.
S E M I - L A R G E - S C A L E P L A N T
C H A P T E R I V
SEMI-LARGE-SCALE PLANT
T H E R E is some difficulty hi correctly defining

semi-large-scale plant, as there is bound to be a
gradual transition from the very large laboratory
autoclave to the real large-scale plant. I t is hardly
enough to fix limits in definite capacities, nor is
ifc altogether correct to describe " laboratory"
autoclaves as those used for experimental work
(C
and plant " as those used for production.
There are some fine chemicals the market

requirements of w h i c h are so small that they can
be, and are, actually manufactured b y the trade
in laboratory apparatus, while on the other hand
it is often the custom to p u t batches through in
semi-large-scale plant simply as experiments in
order to determine without great cost how a new
process will go under works conditions. Perhaps
t h e best classification and the one which shows the
real distinction between laboratory apparatus and
s m a l l - s c a l e p l a n t is t o r e g a r d l a b o r a t o r y apparatus
as that which can be m o v e d about from place to
place, which is capable of being emptied of its
charge by hand and whose capacity does not
greatly exceed 4 or 5 gallons.
Semi-large-scale plant is, then, apparatus

installed permanently in brickwork in a shed
which is w o r k e d by workmen under the direction
of a chemist, and whose function is e i t h e r to test
o u t new processes on a small scale or t o manufacture
s m a l l b a t c h e s of m a t e r i a l r e q u i r e d i n o n l y moderate
quantities.
3 ^
The capacity of semi-large-scale autoclaves is

from 5 to 50 gallons, whereas a small-size works pan
will b e a b o u t 2 0 0 gallons.
As was found to be the case with laboratory-
apparatus, so there are a great variety of semi-
large-scale pans, m a d e to meet all s o r t s of require-
ments. There are four examples, however, which
will be considered in detail as being interesting
and representative types ;
(1) A moderately high pressure non-agitator
autoclave.
(2) A ' moderately high pressure agitator
autoclave.
(3) A very high pressure agitator autoclave.
(4) Steam-jacket autoclaves.
Type No. 1.—The non-agitator autoclave is

becoming used less a n d less of l a t e y e a r s owing to
the great improvement in the design of agitator
pans, particularly with regard to the construction
of t h e g l a n d of t h e agitator shaft. Still, for some
purposes, a gas-heated non-agitator p a n is all that
is required. The pan about to be described is
classified a s a m o d e r a t e l y h i g h p r e s s u r e one, a n d in
this connection a few words of explanation are
necessary. W e have seen that with laboratory
apparatus it is q u i t e c o m m o n to have autoclaves,
a g i t a t o r o r o t h e r w i s e , w h i c h a r e c a p a b l e of standing
pressures up to 200 atmospheres. These high
pressures are seldom required in chemical research
w o r k , still t h e c o n s t r u c t i o n of t h e a p p a r a t u s is such
that they could easily stand them. Naturally,
Semi-large-scale Plant 67
when one is dealing with large pans, the possible

sources of leakage are much greater, and hence it
b e c o m e s m o r e difficult to get really full-size works
autoclaves to s t a n d pressiu'es which are considered
low in laboratory apparatus. Semi-large-scale
plant is i n t e r m e d i a t e i n t h i s respect.
A glance at the table given on p. IS illustrates

this point, and we m a y summarise the matter as
follows ;
Ordinary laboratory autoclaves agitator type

will s t a n d pressures up to 300 atmospheres, while
the non-agitator ones can go to 500 atmospheres.
Really " high p r e s s u r e '' laboratory apparatus
can be made to stand 500 to 1000 atmospheres
pressure.
Semi-large-scale plant for moderately high pres-
sures will s t a n d w o r k i n g pressures in t h e region of
50 atmospheres whether agitator or non-agitator
type.
Very high pressure semi-large-scale plant which
is u s u a l l y of t h e a g i t a t o r t y p e will w o r k u p t o 200
atmospheres.
I n t h e l a r g e - s c a l e w o r k s c l a s s of p a n of capacities
200 gallons upwards, non-agitator pans will work
u p t o 1 0 0 a t m o s p h e r e s , a l t h o u g h t h i s t y p e of plant
has m a n y disadvantages.
The high pressure works pan of 400 gallons
capacity or more, fitted with stuffing-box agitator,
has a working p r e s s u r e of 40 to 50 atmospheres,
while t h e larger size low p r e s s u r e agitator autoclave
w o r k s best u p t o 10 or 15 atmospheres.
To return to our Type No. 1 non-agitator

autoclave. T h i s is d e s c r i b e d a s a m o d e r a t e l y high
pressure semi-large-scale pan, and is therefore
u s u a l l y of c a p a c i t i e s of 2 5 t o 5 0 g a l l o n s a n d working
p r e s s u r e s of 4 0 atmospheres.
K g . 10 gives a general idea of the type and

suitable setting of these autoclaves. As the
construction of t h e p a n is s o s i m i l a r t o t h e agitator
ones w h i c h will b e s h o w n later in section drawing,
it w a s thought that a g e n e r a l v i e w of t h e arrange-
ment of t h i s p a n w o u l d b e m o r e interesting.
The autoclave is m a c h i n e d from solid mild steel

forgings and fitted with pressure gauge, safety
valve, and thermometer pipe. I t is set in brick-
work and heated by gas burners, which are the most
satisfactory and usual means of heating semi-
large-scale plant. In addition to the regulation
of t h e g a s p r e s s u r e o n t h e b u r n e r s , s o m e regulation
of t e m p e r a t u r e is effected b y m e a n s of t h e damper
controlled b y chain and wheel as illustrated in the
diagram.
Type No. 2.—The moderately high pressure

agitator autoclave about to b e d e s c r i b e d is a very
useful and efficient piece of plant, and represents
the latest m o d e r n practice in autoclave construction.
Fig. 1 1 s h o w s a s e c t i o n of t h i s p a n a n d serves to
i l l u s t r a t e t h e o u t s t a n d i n g f e a t u r e s of t h e same.
T h e autoclave is m a d e of cast steel and is

immersed in an oil-bath for uniform heating. As
with most semi-large-scale plant, gas firing takes
t h e p l a c e of t h e o r d i n a r y f u r n a c e . The capacity of
this t y p e of p a n ranges from 20 to 50 gallons and
the best working pressures are u p to 40 atmospheres,
Safety Valve
' ',"' :\i)Pressure

Gauge
t- • > ; ! ; i m
Gas
Heater
FIG. 1 0 . — G e n e r a l a r r a n g e m e n t a n d s e t t i n g of m o d e r -
ately High Pressure Non-agitator Autoclave.
G9
although it would be quite safe to work up to 50

atmospheres.
T h e c o v e r is fitted to the flange of t h e b o d y b y a
c o p p e r g a s k e t in a full register joint, c o n t a c t being
m a d e good b y means of h e x a g o n a l n u t s and bolts.
The agitator is of the anchor type and passes
through a water-cooled stuffing-box packed with
black-leaded asbestos or lead rings.
Power is applied to the p a n b y means of a flat

belt passing over a " fast a n d loose " pulley, which
renders it possible to stop the agitation at a
m o m e n t ' s notice b y sliding the belt on to the loose
pulley. A good speed agitation is secured b y
m e a n s of b e v e l cogs.
Other p o i n t s of i n t e r e s t are the use of a liner to

protect the autoclave body, the space between the
liner and autoclave walls being filled with solder,
and the fitting of the safety collar. It has been
found that w h e n working at pressures over 20
atmospheres or even at lower pressures in large-
size a u t o c l a v e s , t h e r e is a t e n d e n c y for t h e agitator
to be forced upwards. This not only causes grind-
ing a n d wear on the bevel cogs, but also tends
to cause leakage through the stuffing-box. The
safety collar fixed to the shaft just below the inside
of t h e c o v e r t a k e s t h i s s t r a i n a n d s o e n s u r e s smooth
running. A l t h o u g h n o s a f e t y v a l v e is s h o w n i n the
d i a g r a m , i t is u s u a l t o fit o n e , b u t t h e q u e s t i o n as to
t h e m o s t suitable k i n d will b e d e a l t w i t h u n d e r the
section devoted to large-scale plant, as this is a
problem of m u c h greater concern to the users of
large-scale plant.
\Mk copper qashet
xnat
tarn
Oil Jacket
•joafl
< 5 6 < p 6 , 6
Gas burners
F I G . 1 1 . — H i g h P r e s s u r e G a s F i r e Aufcoclavo Section.
71
Type No. 3.—There are now on the market ;

n u m b e r of s m a l l s e m i - l a r g e - s c a l e a u t o c l a v e s capabl
of s t a n d i n g r e a l l y h i g h p r e s s u r e s a n d of t h e agitato
type. The pressures referred to are up to 20(
atmospheres and the most convenient capacity I
g a l l o n s , a l t h o u g h i t is p o s s i b l e t o o b t a i n l a r g e r sizes
N a t u r a l l y w h e n e n o r m o u s p r e s s u r e s of this descrip-
tion h a v e t o b e resisted, all p a r t s of t h e p l a n t must
be s o m e w h a t massive, and although the section in
Fig. 12 is not intended to be strictly to scale, it
serves to s h o w how liberal must be the allowance
of metal in autoclaves of this type. To anyone
familiar with autoclaves, the diagram itself will
show most of t h e points of i n t e r e s t i n this model,
but a very brief survey will not, perhaps, be out
of place.
The body of the autoclave (a)9 which is c a s t in

one piece, rests on an iron platform (?/) supported
on brickwork or a specially constructed furnace
casing hidicated b y (x). Such small pans arc
usually directly heated by gas, precautions being
t a k e n t o a v o i d t h e p l a y o f t h e b u r n e r f l a m e s on the
b o t t o m o r s i d e s of t h e a u t o c l a v e . Oil-bath heating
as shown for the lower pressure type in Fig. 11
would, however, be perfectly satisfactory and in
m a n y ways superior to the most perfect system of
direct-firing with baffle plates. T h e cover of the
a u t o c l a v e (6) i s of i n t e r e s t , a s t h e s h a p e of t h e inside
is s u c h a s t o avoid sharp angles, a very necessary
thing for semi-large-scale plant, which has to
withstand very high pressures. The cover is
fastened down on to the body b y means of the
Furnace
door
F x c i . 1 2 . — S o c t i c f n of H i g h P r e s s u r e A g i t a t o r
Autoclave—Semi-large-scale Plant.
3* 73
heavy round nuts (d), a perfect joint being m a d e

w i t h a full register j o i n t a n d copper gasket (c).
T h e inside fittings of t h e a u t o c l a v e are as usual,

viz. a thermometer pipe (e) and agitator (/), the
s h a p e of t h e l a t t e r b e i n g p e c u l i a r so as t o enable a
d i s c h a r g e p i p e (g) t o c o m e t o t h e b o t t o m of t h e pan.
The discharge pipe leads to a heavy valve (h) and
finally to the outlet (i), it being sometimes the
custom to h a v e a further valve fitted which acts as
a n inlet for charging or as a blow-off at the end of
the reaction.
T h e agitator shaft is fitted with a safety collar

(h) as described previously, this b e i n g all t h e more
necessary to take strain off t h e bevel cogs at such
very high pressures.
T h e stuffing-box (j) is n o t usually water-cooled
in the 5 gallon sizes, b u t for a n y t h i n g m u c h larger
it w o u l d b e b e t t e r so. The usual arrangements for
driving the agitator are shown (jt l,m>), the addi-
tion of the fast and loose pulleys (n) being a very
necessary safety precaution in semi-large-scale plant.
Although small in size a n d somewhat inefficient

in agitation, this type of autoclave has numerous
advantages and will b e f o u n d c a p a b l e of v e r y faith-
ful service for experimental work and small-scale
manufacture where high pressures are unavoidable.
Type No. 4. Steam-jacket Autoclaves.—Although

t h e r e a r e a g r e a t v a r i e t y of s p e c i a l d e s i g n s of semi-
large-scale autoclaves, too, n u m e r o u s to mention in
detail, no section on this subject w o u l d be complete
without a few words on steam-jacket pans.
As the n a m e implies, these are autoclaves in

Semi-large-scale Plant 75
which steam is u s e d a s t h e h e a t i n g m e d i u m , some-

times direct from the boiler a t high or low pressures
a n d sometimes superheated where higher tem-
peratures are required.
FIG. 13.—Horizontal Staam-jacket Autoclave.
A brief d e s c r i p t i o n of t w o t y p e s of steam-heated
autoclave will n o w follow:
(a) Horizontal type—large capacity.
(b) Vertical t y p e — s m a l l capacity for higher

pressures,
(a) A typical horizontal steam-jacket autoclave

is shown in Fig. 13. Although m a d e in smaller
sizes, t h e m o s t useful is t h e 5 0 - g a l l o n - c a p a c i t y pan,
which has a working pressure of 30 to 40 atmo-
spheres. T h e autoclave itself is m a d e from solid
steel forgings and is fitted with manhole and lid3
pressure gauge, inlet a n d discharge pipes, together
with the necessary valves. T h e steam-jacket
takes the form of a mild steel t u b e fitted into the

autoclave covers at either end. I t is p r o v i d e d with
its own gauge and safety valve, the latter being
of the ordinary steam-boiler type, and inlet and
exhaust pipes for the steam supply. I n order to
p r e v e n t l o s s of h e a t b y r a d i a t i o n i t is u s u a l t o have
t h e s t e a m - j a c k e t w e l l l a g g e d w i t h a t h i c k c o v e r i n g of
suitable non-conducting material, such as some of
the asbestos composition pastes sold for s t e a m pipes.
The agitator shaft runs horizontally through the

autoclave from one cover to the other and is fitted
with blades at intervals along its entire length.
It passes through stuffing-boxes at either end, and
is s u p p o r t e d also at each e n d b y external bearings.
P o w e r is s u p p l i e d b y m e a n s of a flat belt operating
fast a n d loose pulleys.
The measurement of temperatures in this type

of autoclave presents some difficulty, as a single
thermometer pipe would hardly give a truly repre-
sentative reading. The best modern p r a c t i c e is to
use pyrometers which can be arranged to slide
inside the hollow agitator shaft from cither end,
thus rendering it possible to obtain accurate
temperature measurement at any point.
(b) The vertical steam-jacket autoclave shown

in F i g . 1 4 is a r a t h e r m o r e h e a v i l y b u i l t t y p e of pan
for pressures up to 60 or 70 atmospheres. The
general construction of the autoclave is so similar
to designs previously described t h a t no explanation
of the diagram in t h a t respect is necessary. The
capacity of this autoclave generally ranges from
5 to 20 gallons. The points of i n t e r e s t are those
Outlet steam pipe
jrhairrlft i m
Run off tap

^ a for water
i^g-^:
Gas' heaters
FIG. 14.—Vertical Steam-jacket Autoclave—Section.
77
connected with the steam-jacket. This is of mild

steel, a n d is fitted with safety valve, steam gauge
a n d the necessary pipes for connecting to the
steam mains. In addition, the steam-jacket m a y
be heated b y gas burners in order to superheat the
steam 5 b y which means temperatures up to 300° C.
can be conveniently reached.
If so desired, the inlet valve could be closed and

the steam-jacket used as a boiler to generate its
o w n steam.
I n concluding this c h a p t e r i t is n o t intended to

devote a n y space to the details of working semi-
large-scale plant. Although there are without
doubt several points of d i f f e r e n c e , generally speak-
ing the conditions approximate to those of large-
scale manufacture, which will be considered at some
length in subsequent chapters.
I n those models which have not permanent

blow-over pipes fitted such as in Fig. 12, it is usual
t o e m p t y t h e p a n b y m e a n s of a s p e c i a l p i p e , which
is i n s e r t e d through the charging hole or through a
hole m the manhole lid after the batch is cooled
d o w n a n d the pressure relieved. On passing
compressed air into the p a n the contents are blown
over into a n y suitable vessel for the next stage of
manufacture or experiment. A l t h o u g h it has been
impossible to show the compressed air inlet in the
diagrams, most semi-large-scale autoclaves except
t h e v e r y smallest sizes h a v e s u c h a fitting, as lifting
the cover a n d bailing out t h e contents b y means of
buckets would be a very clumsy a n d tedious
o p e r a t i o n to perform for e a c h batch.
T H E C O N S T R U C T I O N A N D U S E
O F W O R K S A U T O C L A V E S
C H A P T E R V
THE CONSTRUCTION AND USE OF WORKS
AUTOCLAVES
Introduction.—Up to now we have been con-

sidering apparatus essentially designed either
simply for experimental work or for very inter-
mittent manufacture possibly of an experimental
nature. W h e n dealing with the subject of works
plant, we must remember that t h i s is i n t e n d e d for
regular routine production and that therefore
s e v e r a l f a c t o r s w h i c h u p t o n o w h a v e b e e n of small
importance become vital. Foremost amongst
these factors is reliability, b y which one means
that a satisfactory design of works autoclave is
o n e t h a t is c a p a b l e of w i t h s t a n d i n g r e a s o n a b l e wear
and tear for long periods w i t h o u t constantly need-
ing attention at the hands of the maintenance
engineer. W h e n considering t h e different types of
works autoclaves and comparing t h e m with those
of the semi-large-scale or laboratory sections, it
m a y seem that some repetition has occurred, for
all autoclaves must necessarily be fundamentally
similar, but the conditions of w o r k s p r a c t i c e a r e so
different t h a t i t is d e s i r a b l e t o t r e a t t h i s b r a n c h of
t h e s u b j e c t a s a s e p a r a t e c h a p t e r r e g a r d l e s s of what
has gone before.
Although works autoclaves m a y be said to range
in size from 25 gallons to 2500 gallons, the lower
limits are better regarded as semi-large-scale plant,
while t h e higher are so exceptional as to be outside
the scope of this book. For general purposes,
works autoclaves m a y be taken as ranging in size
81
from 200 gallons to 1000 gallons, the larger sizes

b e i n g t h o s e f o r l o w p r e s s u r e s , a n d vice versa.
I t was stated in t h e previous chapter that owing

to the improvement in the manufacture of agitator
autoclaves, the use of the non-agitator type was
becoming less common, and this is t r u e of works
plant also. For this reason it is n o t intended to
take a n y particular design of the works non-agi-
tator autoclave into consideration, b u t as in m a n y
old-established works these pans are still doing
good service a few general observations on their
use will suffice.
T h e non-agitator autoclave is often a small-

sized p a n m a d e of v e r y thick steel, a n d is u s e d for
w h a t m u s t be regarded as very high pressure from
a works point of view. I n some cases the walls
of the p a n are 4 or 5 inches thick and when
properly sealed will stand pressures of 100 atmo-
spheres; indeed the whole problem of getting
works pans to stand pressures resolves itself into
the problem of getting packed joints to remain
good. T h e non-agitator autoclaves have small
manholes for charging—far too small to allow a
m a n to pass t h r o u g h — a n d the joint of the cover
on to the body, o n c e m a d e , is n e v e r b r o k e n u n t i l it
is necessary to have the p a n cleaned out and
examined. T h i s j o i n t is p a c k e d either with a lead
ring or thick black-leaded asbestos rope, and
although the full or half register gasket as in
Fig. 11 (Chapter IV) might be employed with
advantage, in old pans it is not usual. The nuts.
Construction of Works Autoclaves 83
a n d bolts employed to exert the necessary pressure

between cover and body are very strong and as
numerous as possible. Really satisfactory joints
have been m a d e by using rings 1 inch to 2 inches
wide and | i n c h t o |- i n c h t h i c k , t h e m a t e r i a l being
l e a d , c o p p e r , o r b l a c k - l e a d e d a s b e s t o s , a n d i t is good
to bear in m m d that the method of t i g h t e n i n g up
and fitting the ring is just as important as the
material used. The joint between the manhole lid
a n d t h e m a n h o l e i n t h e p a n c o v e r is a n o t h e r source
of weakness, but here again a flat black-leaded
asbestos ring gives a good joint, although it is
a d v i s a b l e t o u s e a fresh ring for each batch.
Non-agitator autoclaves should always be oil-
bath-heated unless the contents are an absolutely
homogeneous mixture of mobile liquids or a thin
aqueous solution. The author once had occasion
to investigate v a r i a b l e y i e l d s of a c a u s t i c f u s i o n of
a naphthalene sulphonic acid and found that the
operation was being carried out in a direct-fired
non-agitator autoclave. No* wonder the yields
were variable ! W h e n working with these auto-
claves, it is very necessary to have adequate
arrangements for relieving pressures should they
get too high. It has been stated that the ordinary
s a f e t y v a l v e is n o t v e r y reliable for a u t o c l a v e work,
b u t , as will b e s h o w n later, t h e r e are devices which
seldom fail, In the event of internal decomposi-
tions, if the cover and manhole joints had been
m a d e correctly, it is probable that the contents
w o u l d attain a n enormous pressure before anything
happened, W i t h no safety device and no friendly
agitator gland to protest by leaking and the pressure

gauge blocked up, the first i n t i m a t i o n of anything
wrong would be the " blowing " o f t h e r i n g off the
m a n h o l e l i d a n d s u b s e q u e n t e j e c t i o n of t h e contents
of t h e p a n a l l o v e r t h e shed.
Apart from the fact that non-agitator pans are

more likely to collect a deposit on the inside and
therefore should be cleaned out more frequently,
the routine of periodic testing a n d examination is
the same as with agitator pans. It is n o t always
necessary to remove the cover a n d put m e n inside
the pans for removal of deposits, although this is
the last resort. If, however, the works chemist
will c u l t i v a t e t h e h a b i t of b o i l i n g o u t h i s p a n s with
water whenever an opportunity presents itself,
he will be surprised to find how m u c h dirt and
insoluble matter can be dislodged. The cost in
firing is very little, and it m a y m e a n that the
autoclave will continue its routine work for half
as long again before h a v i n g to be dismantled for a
complete scraping and examination.
T H E L A R G E - S I Z E L O W P R E S S U R E W O R K S
A U T O C L A V E
I t is i n t e n d e d to devote some considerable space

to the description of the construction of the low
pressure works autoclave, as for all-round work
t h e r e is n o d o u b t t h a t t h i s , t y p e of p a n is t h e most
useful t h e w o r k s chemist h a s a t his disposal. First
of all, w i t h o u t c o n f i n i n g o u r s e l v e s t o s p e c i f i c limits,
let us decide a reasonable range of capacities and
pressures within which to fix the definition of this
autoclave. On the works, working with large

pans, low pressures m a y be said to range from 5 to
15 atmospheres, a n d although with careful attention
t o t h e p a c k i n g of j o i n t s i t m i g h t b e p o s s i b l e t o work
u p t o 2 0 a t m o s p h e r e s i n t h e t y p e of a u t o c l a v e t o be
considered, i t is g e t t i n g f a r too near to the actual
t e s t e d limit to be safe. For regular routine work,
b y far the best results are obtained at pressures of
from 5 to 10 atmospheres, and although these
limits m a y appear close together and on the low
s i d e , i t is s u r p r i s i n g h o w g r e a t a v a r i e t y of reactions
c a n b e c a r r i e d o u t a t t h e s e p r e s s u r e s if t h e research
chemist sets himself to try to devise recipes
accordingly. For example, most of t h e important
hydroxy-derivatives of the naphthalene series,
particularly aminonaphtholsulphonic acids, can be
prepared by recipes which do not involve greater
pressures than 100 lb. per square inch, while
amidations both in the benzene and naphthalene
series seldom give rise to pressures higher than
150 lb. to the square inch, and even that pressure
d i m i n i s h e s s t e a d i l y o w i n g t o a b s o r p t i o n of a m m o n i a
as the reaction proceeds.
It can be taken then, that, although for experi-

mental work we need autoclaves capable of stand-
i n g m a n y h u n d r e d s of a t m o s p h e r e s , t h e b u l k of the
most important products required in mass b y
chemical industry can be m a d e successfully in
comparatively low pressure pans.
As regards capacity and temperature limits,
there is less nfeed for explanation, as undoubtedly
t h e m o s t u s e f u l size of l a r g e Avorks a u t o c l a v e is from
600 to 1 0 0 0 g a l l o n s c a p a c i t y , w h i l e it is s e l d o m that
temperatures higher t h a n 2 5 0 ° G. a r e required.
T h e f r o n t i s p i e c e of t h i s b o ' o k is f r o m a photograph
of a l a r g e size l o w p r e s s u r e works autoclave m a n u -
factured b y Messrs. A d a m s o n a n d Co., Ltd., of
H y d e , Manchester. T h e author has used m a n y of
these pans a n d subjected t h e m to a practical test
of r e l i a b i l i t y b y r e a s o n of m o n t h s of unintermittent
daily working quite out of the ordinary. T h e y
came through the test m o s t creditably a n d can be
confidently q u o t e d a s e x a m p l e s of f i r s t - c l a s s British
workmanship. I n the following descriptions of a
low pressure works autoclave, it is n o t intended to
follow in every detail the A d a m s o n design, b u t the
description a n d diagram m a y be taken as sub-
stantially correct and characteristic of a works
autoclave of t h i s type.
-îg- 15 gives a sectional elevation of the pan,

and is w o r t h y of c a r e f u l study, as it s h o w s m a r k e d
differences in design f r o m the laboratory a n d semi-
large-scale plant previously considered.
I n the first p l a c e , t h e b o d y of t h e p a n , i n s t e a d of
being cast in one piece, c o n s i s t s of a riveted cylin-
drical tube, m a d e from sheet steel, o p e n at the top
to receive t h e cover, a n d a shallow dish for the
b o t t o m w h i c h is r i v e t e d o n t o t h e c y l i n d r i c a l sides.
I t is c l a i m e d b y some authorities t h a t the prejudice
in favour of a riveted joint between the dish and
the sides is without foundation, b u t m o s t works
chemists w h o have h a d experience of b o t h riveted
a n d w e l d e d joints will favour the former.
The depth of t h e c y l i n d r i c a l p a r t of t h e autoclave

Sea r/n£ packing
Metallic packing
?•>*:
•i^
LI
:j
1 . •/..
\ s * " «.'/ t :•j
rf .
£! ,;;
• "clearance
•£•$
-1 iiil
c
2
FIG. 1 5 . — S e c t i o n a l E l e v a t i o n of S t e e l A u t o c l a v e .
87
from the cover flange to the beginning of t h e cl

is f r o m 5 feet 6 inches to 6 feet, w h i l e t h e dej
of t h e dish in the centre is 1 foot. T h e h e i g h t
t h e d o m e d c o v e r is a b o u t 1 0 i n c h e s a n d the interi
d i a m e t e r of t h e a u t o c l a v e 4 f e e t 6 inches.
Such-a p a n has a c a p a c i t y of about 700 galloi

which is a very suitable size for all-round m a r
facturing processes.
The flange o n w h i c h t h e c o v e r r e s t s is e i t h e r of
as part of the cylindrical body or riveted, to
although in autoclaves m a d e of thicker steel
might be bolted into the body, the bolts being,
course, n o t t a p p e d through.
For this type of p a n it is sufficient to u s e stc
of 1 inch thickness both for the sides a n d dis
although the cover would be thicker, say 2 inchc
I t is i n t e r e s t i n g t o n o t e t h a t t h e j o i n t m a d e betwct
the cover a n d the flange is of the " half-register
type, whereas u p to n o w in previous models w e ha"1
always dealt with full register joints. F i g . ]
shows the two kinds of joints on a larger seal
from which it will be seen that the full registi
w o u l d b e s e l e c t e d if v e r y h i g h p r e s s u r e s w e r e to I
withstood. For this type of autoclave t h e hal
register joint, if properly packed, is on t h e w h o
satisfactory. In this connection it is interestin
to note a suggestion which appeared as a contr
bution of M r . P . Bloor i n t h e Engineering World c
M a y 7th, 1921. In this it is s h o w n t h a t th
p r e s s u r e of t h e b o l t s o n t h e h a l f - r e g i s t e r j o i n t tend
to squeeze the packing material out at A (Fig. 1
a) and causes a hinge m o v e m e n t at B to be exerte
b y t h e pressure in the pan. T h e s u g g e s t i o n is that

t h e faces of t h e m e t a l to be joined b y half register
should be at an angle of J5° with the horizontal,
and that a clearance portion 0 ( F i g . 1 6 c) s h o u l d be
(a) Full r e g i s t e r (b) Half register
FIG. 10.—Examples of Joints.
provided. The effect of screwing down will now

cause the faces to find their true level, besides
which the ring can give to the point 0 and fill the
space allowed. Having m a d e such a joint the effect
of p r e s s u r e i n t h e p a n w i l l b e t o cause hinge action
into the ring, thereby m a k i n g t h e joint more secure.
T h e author has never personally tried such a

d e v i c e , b u t i t a p p e a r s w e l l w o r t h y of t r i a l , especially
in autoclaves working u p to 30-40 atmospheres
pressure. T o return to the description of the low
pressure agitator autoclave, it m u s t b e n o t i c e d that
the nuts a n d bolts which secure the half-register
joint between the body a n d the cover of the pan
are of massive construction and placed as closely
t o g e t h e r a s is p o s s i b l e * It has been stated that the
internal diameter of t h e p a n is 4 f e e t 6 inches, and
so, a l l o w i n g 1 i n c h t h i c k n e s s of steel a n d a reasonable
width of flange, the total over-all diameter of the
c o v e r is a b o u t 5 feet 6 i n c h e s . H e n c e , if t h e s e bolts
are placed five or six inches apart that will mean
between thirty and forty altogether, which caii be
taken as a reasonable n u m b e r to secure a good*joint.
The steel superstructure, whose function it is to
support the agitator shaft and driving wheels,
c a n n o t b e c a s t i n o n e p i e c e w i t h t h e c o v e r , a s is t h e
case w i t h s m a l l e r a u t o c l a v e s , b u t is b o l t e d o n t o the
cover as s h o w n in the figure at The
holes into which these bolts go m u s t not be tapped

through the cover, which is one reason w h y a
liberal thickness of metal is allowed in the cover.
In a similar m a n n e r the base of t h e s t u f f i n g - b o x is
bolted o n t o t h e cover, the t a p p e d holes again being
only allowed to penetrate an inch into the metal.
Attention is d r a w n to two points of g r e a t interest
which can be seen both in Fig. 15 a n d the frontis-
piece. These are, first, the height of the stuffing-
b o x , w h i c h is c o n s i d e r a b l e , a n d , s e c o n d l y , t h e liberal
space allowed between the top and sides of the
stuffing-box and the steel superstructure which

bears the agitator shaft. These are essential
f e a t u r e s c h a r a c t e r i s t i c of g o o d d e s i g n i n autoclaves,
for a large stuffing-box, properly packed, means a
fling for chain

to take strain.
Bar r\ s~s
C±3
Tightening
' Nut '
Vertical
Rod
V-/ \J
Plan o f manhole l i d .
(Dotted lines show position
of packing ring.)
Hexagonal Vertical
Nut " H : 3 s Rod
Ring Packing
i-ra- -at B
Rin$±
F r o n t elevation o f manhole lid

(Bars not shown)
FIG. 17.—Cover of A u t o c l a v e M a n h o l e Lid.
tight gland, while liberal space round it ensures

freedom of m o v e m e n t w h e n i t is n e c e s s a r y t o screw
d o w n t h e c o l l a r of t h e s t u f f i n g - b o x w h e n the p a n is
under pressure.
A l t h o u g h it h a s n o t b e e n possible t o s h o w it i n the
diagram, the cover of the autoclave should have a
n u m b e r of o p e n i n g s i n it, of w h i c h t h e following are
necessary for o r d i n a r y w o r k (Fig. 17) :
(1) A large oval opening, k n o w n as the

manhole.
(2) A tapped hole for the thermometer pipe.
(3) A t a p p e d hole for the pipe leading to the
safety valve.
pressure gauge.
(5) A tapped hole for the pipe fitted with a
valve for " blowing off."
compressed air supply.
These will n o w be considered in turn and
commented on.
(1) In such large pans as these a manhole is an
absolute necessity, as t h e lifting of t h e c o v e r is an
operation involving the use of pulley-blocks, and
means putting the autoclave out of commission
for the best part of a week. Once a satisfactory
joint has been obtained between cover and body,
it should only be broken w h e n it begins to leak
t h r o u g h w e a r o r f o r t h e p e r i o d i c o v e r h a u l i n g of the
plant, say once every six m o n t h s or even a year.
The function of the manhole is, therefore, the
c h a r g i n g of t h e m a t e r i a l f o r t h e b a t c h a n d t h e usual
means of access into the p a n for examination.
Naturally the size of the manhole shoixld be as
small as possible, for the larger the hole the more
difficult it will b e t o m a k e a tight joint when it is
closed. I t is u s u a l in 7 0 0 g a l l o n a u t o c l a v e s to have
the m a n h o l e of o v a l s h a p e a n d j u s t l a r g e e n o u g h for
an a v e r a g e m a n to squeeze through. The manhole
is c l o s e d b y a h e a v y l i d of s t e e l a s t h i c k a s t h e rest
of t h e cover. I n t h e m i d d l e is a s t o u t r i n g through
which c h a i n s c a n p a s s w h i c h b e a r t h e w e i g h t of the
lid w h i l e the workmen, are adjusting the packing
ring. T h e m a n h o l e lid is l a r g e r than the oval hole
it is designed to cover, and has, therefore, to be
passed edgewise through the hole into the pan. On
its o u t e r side at the extreme edge is p l a c e d a flat
packing ring about an inch wide, m a d e of black-
leaded asbestos, which fits into a shallow groove
designed for the purpose. T w o stout rods cut
with s c r e w threads are fastened at right angles to
the surface of the lid, and these thread through
stout b a r s which bridge across the manhole itself.
O n screwing down two massive nuts, one on each
rod, t h e manhole lid is pressed upwards firmly
against the inside surface of the manhole, the
asbestos packing ring causing a gas-tight joint to be
made?:. I t will be seen that, provided the joint is
good, t h e effect of p r e s s u r e w i l l b e to push up the
m a n h o l e lid more firmly against the inside of the
cover. This explanation is necessarily rather
involved, but a study of the frontispiece, which
shows clearly the nuts and bars holding the manhole
lid in place, together with Tig. 17, w h i c h s h o w s a
sketch of the manhole lid from different positions,
should help to m a k e this explanation easier to
follow.
(2) T h e t h e r m o m e t e r p i p e is n o t s h o w n i n F i g . 1 5 ,
as it w a s desired to illustrate mainly features of
difference between works and laboratory pans.

The general construction and function of the
thermometer pipe are just the s a m e in these large
autoclaves as in the laboratory ones. It is a
narrow tube, say of 1 inch bore, of thick-walled
steel piping wide e n o u g h to conveniently accommo-
date the works thermometers, a n d is a r r a n g e d to
r e a c h a s n e a r t h e b o t t o m of t h e p a n a s p o s s i b l e . As
t h e r e is g e n e r a l l y p l e n t y of r o o m on the cover top,
the works thermometer pipes pass vertically down-
wards, rather than at a slant, as was so often the
case in laboratory apparatus. There is no parti-
c u l a r v i r t u e i n t h i s e x c e p t t h a t i t is p r o b a b l y easier
to avoid breakage of the thermometer if it comes
out vertically from the pipe. A few words at this
point on works thermometers suitable for auto-
claves m a y not be out of place. T h e works ther-
mometer differs from the usual laboratory one hi
being of g r e a t length—say from 3 feet 0 inches to
7 feet, the size of the bulb, bore of capillary and
quantity of mercury inside being arranged so that
the scale from 0° to 200° or 360° 0. occupies the
top 1 2 i n c h e s o r 18 i n c h e s of t h e instrument.
T h e best w o r k s t h e r m o m e t e r s , especially for high

temperatures, are filled with nitrogen to prevent the
condensation of m e r c u r y vapour in the cool upper
parts. M a n y of these instruments h a v e engraved
scales inside the tube rather than the graduations
s i m p l y e t c h e d o n t h e o u t s i d e of t h e g l a s s . If these
inside scales are reliable a n d rigid this type is the
better, as they are so m u c h easier to read in the
shadows round the pan. Moreover, they never
alter, whereas the other type become attacked by

fumes which destroy the black markings in the
e t c h e d lines. I n t h i s c o n n e c t i o n it is useful t o note
that a n outside scale t h e r m o m e t e r whose markings
h a v e become so faint as to be almost invisible may
be brought back to usefulness by rubbing with a
cloth containing a little finely-powdered copper
oxide, manganese dioxide or charcoal, which fills
up the fine lines a n d makes these and the figures
visible once more. In choosing a works thermo-
meter for a n y particular autoclave attention must
be paid to the length, so as t o h a v e t h e scale just
nicely clear of the top of the thermometer pipe.
Another even more important point is t o s e e that
the amount of i m m e r s i o n is r e a s o n a b l y n e a r t o that
marked on the thermometer as corresponding to
the graduations. With a large autoclave such as
the one we are considering a 6 to 7 feet ther-
mometer will be suitable, and these are generally
graduated for 4 to 5 feet immersion, which will
represent the amount that will be actually
immersed in the hot oil w h e n working with a full-
sized batch. It is h a r d l y necessary to note that
the amount of oil in t h e t h e r m o m e t e r pipe should
be such as to fill it c o n v e n i e n t l y w h e n t h e b a t c h is
on temperature—ordinary machine oil or high
boiling paraffin f o r m a suitable m e d i u m for ensuring
that the thermometer is registering a true and
a c c u r a t e m e a s u r e of t h e t e m p e r a t u r e of t h e batch,
(3 and 4) It was mentioned previously that the

question of providing an adequate safety valve
for autoclaves was not easy of solution. Xever-
t h e l e s s it is e s s e n t i a l t o h a v e some such device, and

although the ordinary steam safety valves are not
very satisfactory for autoclave work, while a cap
at the end of a b l o w - o f f p i p e d e s i g n e d t o r u p t u r e at
a definite pressure limit is somewhat crude, there
are other neater and fairly effective devices in
technical use. As this is more a problem of the
high pressure w o r k s p a n , it will b e considered when
dealing with t h a t p i e c e of p l a n t . Again, although
m a n y autoclaves are merely fitted with straight
pipes of 1 inch bore leading direct to steel-tube
pressure gauges, there are one or two refinements
w o r t h y of n o t e , p a r t i c u l a r l y r e l a t i n g t o h i g h pressure
large-scale w o r k on which a few comments should
be m a d e at the same time.
(5) W h e n one speaks of t h e " blow-off " pipe or

valve in connection with works autoclaves, one
d o e s n o t r e f e r t o t h e e j e c t i o n of t h e c o n t e n t s of the
pan, which operation is m o r e commonly described
as " blowing over the batch." The blow-off pipe
leads from t h e c o v e r t o t h e o u t s i d e of t h e s h e d and
is, t h e r e f o r e , generally sloped upwards at an angle
of 60° with the horizontal, and passes out of the
shed through t h e wall or roof. I t is c o n t r o l l e d by
a g o o d g l a n d v a l v e , for l e a k a g e h e r e is j u s t a s b a d as
anywhere else. The function of t h i s b l o w - o f f pipe
is t w o - f o l d :
(a) to give a means of r e l e a s i n g pressure in

an emergency,
(6) to blow off steam or other vapour and
thereby greatly facilitate the cooling rate of
Construction of Worhs Autoclaves 97
the contents of the p a n at the end of the

operation. Naturally this can only be
employed if the product is not volatile in
steam or the vapour concerned.
It w a s stated t h a t this blow-off pipe w a s led out

through the Avail o r r o o f , but if t h i s w a l l i s n e a r a
road or passage along which m e n are likely to pass
the probability of condensed boiling water, etc.,
being dropped from the pipe m u s t not be forgotten.
In such c a s e s , it is w i s e r t o b r i n g t h e blow-off pipe
down again after leaving the shed and allow it to
eject a n y liquids on to the g r o u n d or into a dram.
(6) The pipe supplying compressed-air service

to the a u t o c l a v e is in m o s t cases a necessity, since
it is usual to evacuate the pans at the end of
the operation by " blowing over." The methods
whereby the contents of the p a n are blown by
means of compressed air to the desired vat will
b e fully considered when dealing with the working
of the plant. In any case, all autoclaves should
have compressed-air service, as this forms a
usual means of ventilation when the necessity for
e x a m i n a t i o n of t h e i n t e r i o r c o m e s along.
The next items of constructional design to be

considered are the agitator and agitator shaft.
The latter can be either a rod or a tube of s t e e l of
approximately 3 | inches or 4 inches diameter>
t h e t u b u l a r shaft being t h e better for m a n y reasons.
Not only does a hollow shaft ensure less risk of
bending u n d e r a h e a v y load, b u t it possesses advan-
t a g e s c o n n e c t e d w i t h t h e w o r k i n g of t h e autoclaves
4
which will be more fully elaborated in due course.

T h e shaft is generally thicker inside the p a n and
narrows in diameter before entering the stuffing-
box at the top end, a n d the setting in which it
rotates at the bottom. After leaving the stuffing-
box the shaft passes through the steel super-
structure a n d is k e y e d or screwed on to the large
bevel cog-wheel which forms part of the gearing
arrangement by means of which the agitator is
driven.
T h e diagrammatical illustration of t h e b e v e l cogs

a n d fast-and-loose pulley for driving off the
shafting is sufficiently clear to need no further
c o m m e n t save that it is usual, a n d desirable, to
have all rotating parts working on ball bearings.
A ball-race will therefore be provided in t h a t part
of the steel superstructure m a r k e d bx a n d b2i
K g 15, in order to ensure smooth easy rotation of
the large bevel cog-wheel.
As has been stated, the agitator shaft terminates

a t i t s l o w e r e n d i n a s e t t i n g o r c u p (C\ G2—Fig. 15).
This is b o l t e d on to the dish, care being taken, as
usual, that the holes are not tapped through a n y
further t h a n is n e c e s s a r y to give a really good, firm
connection. It is essential that the bottom oup >
the stuffing-box, a n d the hole through the upper

part of the steel superstructure be absolutely in
alignment so that the shaft fits tightly yet easily,
and that n o strains are set up w h e n it revolves.
Points like this determine whether an autoclave
is g o i n g t o b e a f a i t h f u l s e r v a n t or a c o n s t a n t source
of worry to the m a n w h o works it, as strains a n d
FIG. 18.—High Pressure Works Pan.
vibrations invariably lead to leakages und<
pressure.
Corning to the question of the shape of th

agitator, there can be no hard-and-fast ride lai
down, b u t the design shown is one that will I
useful for most chemical reactions. It should fc
noted h o w perfectly and closely the agitator ;
m a d e to fit the shape of t h e p a n — \ inch clearanc
only being provided between the blade and th
vertical side of the autoclave body. T h e allelic
agitator shown is s u p p l e m e n t e d somewhat b y th
extra short blades dv d%9 Fig. 15, b u t a still mor
massive inside " gate " might with advantage b
fitted for stiff mixtures, as shown in Fig. 18; th
special shaped pieces of metal A , A (Fig. 15.) ar
not usual, but were employed b y the author for i
special purpose, as will be explained later whei
d e a l i n g w i t h t h e w o r k i n g of t h e s e pans.
As the heating of a u t o c l a v e s is a p r o b l e m whicl

presents little difference whether the p a n is of t h
low pressure works typo (10 atmospheres) or higl
pressure works type (30 to 40 atniosplicres), it i
proposed to deal with, the subject of the setting
of a u t o c l a v e s i n b r i c k w o r k or oil-bath as a chapte:
by itself.
A short description of the higher pressure

autoclave will n o w follow, after which t h e problems
of h e a t i n g a n d w o r k i n g t h e p a n s w i l l b e considered
T H E H I G H P R E S S U R E W O R K S
A U T O C L A V E
C H A P T E R VI
THE HIGH PRESSURE WORKS AUTOCLAVE
W H E X considering this piece of plant it is

recommeiifled that the student refer hack to one
or two earlier chapters of the hook. In the first
place he should refresh his memory as to the
meaning of h i g h pressure when used in connection
with works plant together with the probable size
of s u c h autoclaves.
Secondly 3 t h e r e a r e t w o t y p e s of a u t o c l a v e either
of which possesses some characteristics of t h e pan
about to be described, namely, the high pressure
s e m i - l a r g e - s c a l e a u t o c l a v e s h o w n in Fig. 11 a n d the
large low pressure works pan which has been dealt
w i t h so fully in the preceding chapter.
This recapitulation is n e c e s s a r y a s . o w i n g t o the

inevitable resemblance between the high pressure
works autoclave and the two examples just cited,
it would be verv monotonous if an absolutely
detailed description of this pan were set down,
w h i l e , o n t h e o t h e r h a n d , t h e r e are sufficient points
of difference to make some comment on this type
essential.
Briefly5 then, we expect a full-sized works auto-
c l a v e t o h a v e a c a p a c i t y of a t l e a s t 3 0 0 g a l l o n s , but
as it has to withstand a higher pressure than the
type shown in Fig. lo it is probable that the
capacity will be less t h a n the 700 gallons quoted
i n t h e d e s c r i p t i o n of t h a t pan.
S u c h is g e n e r a l l y t h e case, a n d 4 0 0 gallons m a y
be taken as a fair size for a high pressure works
autoclave. A s regards pressure, w e h a v e seen that.
103
although i t is e a s y to obtain laboratory apparatus

to withstand m a n y hundreds of a t m o s p h e r e s , even
with semi-large-scale plant of 20 gallons capacity
and upwards a working pressure of 500 lb. to the
square inch is considered high, and so a full-size
works autoclave of 4 0 0 g a l l o n s capacity and work-
ing pressure of 30 to 40 atmospheres m a y be
d e s c r i b e d j u s t l y a s a h i g h p r e s s u r e Avorks pan.
I t is b e s t t o r e g a r d t h e s e m i - l a r g e - s c a l e autoclave
of F i g . 11 a n d t h e l o w pressure w o r k s autoclave of
P i g . 15 a s t h e p r o t o t y p e s of t h e h i g h p r e s s u r e works
pan, a n d so, in order to avoid useless repetition, only
a diagram a n d t h o s e p o i n t s of o u t s t a n d i n g interest
or difference will n o w be given.
L e t u s t h e r e f o r e s t u d y d i a g r a m F i g . 1 8 , w h i c h is a
s e c t i o n a l e l e v a t i o n of a t y p i c a l w o r k s h i g h pressure
pan. In the first place, since the question of heat-
ing w o r k s p a n s , w h e t h e r h i g h or l o w pressure, will be
considered in a subsequent chapter, no method of
firing has been shown. The space A represents
where the coal or gas furnace for direct or oil-bath
heating would be situated. The general construc-
t i o n of t h e a u t o c l a v e is v e r y s i m i l a r t o t h a t shown
in Fig. 15, but it is interesting to note that the
4C
d i s h " or b o t t o m w h i c h is r i v e t e d on to the main
body at (av a2) is less shallow a n d m a y even be
hemispherical in shape in order to better resist
the higher pressures. Again, the overlap between
the " dish " and the autoclave sides is greater, a
double row of rivets being often employed. On
examining the top part of the diagram it is again
to be observed t h a t t h e r e is a g r e a t e r r o u n d n e s s of
The High Pressure Works Autoclave 105
design and less s h a r p euryes or angles. These are

small points, but they make for greater security
a n d tighter joints u n d e r t h e higher pressures.% The
c o v e r of t h e a u t o c l a v e , w h i c h is m o r e dome-shaped
tlian that of Fig. 15, is fastened to the body by
m e a n s o f t h e n u t s a n d b o l t s (bv 62), t h e d o t t e d lines
showing the position of the great flanges of cover
a n d body round which the bolts are placed as
closely together as is consistent with convenient
working. It will be remembered that a half-
register joint [see Fig, 16 (6)] w a s perfectly satis-
f a c t o r y for t h e low pressure pan, b u t where pressures
u p t o 4 0 a t m o s p h e r e s h a v e t o b e r e s i s t e d t h e r e is n o
doubt but that a full r e g i s t e r j o i n t m a d e against a
copper or lead r i n g is n e c e s s a r y . This is another
point of d i f f e r e n c e between Figs. 15 a n d 18. The
flange (Cv C\2) s h o w n i n t h e d i a g r a m i s n o t essential,
but merely a method of s u p p o r t i n g the autoclave
a n d r e n d e r s a c c e s s t o t h e b o l t s (h1? b.z) easy.
It is seen that the agitator shaft is h e l d in the

pocket (d) a s u s u a l a n d p a s s e s u p t o t h e t o p of the
p a n . w h e r e it t e r m i n a t e s in a safety collar similar to
t h e d e s i g n of t h a t i n t h e s e m i - l a r g e s c a l e autoclave
(Fig. 11), The tendency of the agitator shaft to
rise when under pressure is n a t u r a l l y greater in
these large pans when working at 40 atmospheres,
a n d i n t h i s c o n n e c t i o n it is i n t e r e s t i n g t o n o t e that
not o n l y is t h e s a f e t y collar fitted at (e) (Fig. 18),
b u t t h a t t h e a r r a n g e m e n t of t h e g e a r i n g is different
from t h a t of t h e l o w p r e s s u r e p a n . T h e effect of a
slight rising in the shaft of the low pressure pan
would be to grind the two bevel geared wheels
together. Whereas in the high pressure pan, even

if t h e safety collar were not fitted or worked loose,
a lifting of t h e s h a f t w o u l d o n l y r e a c t o n t h e t o p of
the superstructure (B) or would slightly loosen the
contact of t h e b e v e l wheels.
The stuffing-box (/) is of similar design to that

of the low pressure pan, save that it should be
larger a n d could with advantage be water-cooled.
As regards the agitator, this is h a r d l y a feature

of t h e a u t o c l a v e , b u t r a t h e r of t h e t y p e of operation
to be carried out in it ; the one shown in Fig. 18
is a fine a l l - r o u n d s y s t e m , b e i n g a c o m b i n a t i o n of a
close-fitting anchor to scrape the sides and a
" g a t e " to m i x the middle portions of a thick
batch.
N o pipe fittings are shown in the diagram, but

the usual services described for the low pressure
pan should be provided.
T h e r e is a t e n d e n c y i n r e c e n t m o d e l s t o substitute
pyrometers f o r t h e t h e r m o m e t e r a n d p i p e , a n d if of
reliable design this form of temperature measure-
ment has naturally m a n y advantages. For one
thing, a n u m b e r of p y r o m e t e r s c a n b e fitted which
will s h o w if'the a g i t a t i o n is c a u s i n g a t r u l y uniform
m i x i n g of t h e c o n t e n t s , w h i l e , f o r a n o t h e r , automatic
registration of temperature can be effected in the
chemist's office during night shifts which enable
h i m t o k n o w w i t h o u t p o s s i b i l i t y of e r r o r if batches
have been kept to correct temperature for the
s p e c i f i e d i e n g t h of time.
Still, w i t h trustworthy foremen and good ther-
m o m e t e r s t h e r e is v e r y little t o b e s a i d a g a i n s t the
The High Pressure Works Autoclave 107
older method of temperature registration by a

t h e r m o m e t e r in a t h e r m o m e t e r pipe.
W h e n dealing with the low pressure autoclave
it was stated that, although the ordinary type of
Pips to drain or trap
Bolt
m ^
Plate of metal' l*^2qj.p autoclave
tested to burst h^£^^~~~^
at desired pressure
Sectional elevation
Hole for making flange

oint with nut and bolt
Inside of pipe
Sample of hexagonal
bolt head
ê of sheet of metal
lying as a plate over
the pipe between the
flanges
Plan of flange
FIG. 10.—Safety Pressure Device.

>~
safety valve was unsatisfactory owing to the likeli-
hood of it sticking or getting made up with sub-
limed or distilled solid material, there were some
fairly satisfactory safety devices to enable a blow-
off of p r e s s u r e t o o c c u r a t a d e s i r e d l i m i t . Perhaps
the most reliable is t h a t shown in Fig. 10. This
consists in leading a pipe of fairly wide bore,

certainly n o t less t h a n 1 inch, from the cover which
terminates in a flange joint m a d e as usual with nuts
a n d bolts, the pipe continuing a short distance—
say to a drain—after the flange joint. Between
the two flanges of the joint, besides the necessary
washer for withstanding pressure, tliere is a flat
plate of metal wliich is tested to burst at any
desired pressure. T h e result of an excessive
pressure would be the rupturing of t h i s p l a t e a n d a
subsequent escape of t h e steam or gas. Of course
some of t h e batch would probably froth up and be
lost, but that can hardly bo avoided unless a
special trap chamber were provided into which
the pipe would lead instead of into the drain. A
s e c o n d p o i n t of g r e a t e r i n t e r e s t w i t h h i g h t h a n with
l o w p r e s s u r e p a n s is t h e p r o b l e m of t h e manometer,
or pressure gauge, as it is often called. For
ordinary w o r k t h e r e is n o doubt that a good wide
tube looped in a complete circle and leading to a
steel tube pressure gauge is p e r f e c t l y satisfactory,
but there is a device specially designed for those
cases w h e r e distillation or f o a m i n g causes blocking
of the leading pipe or the steel tube of the gauge
and consequent breakdown of t h e o r d i n a r y method
of pressure registration. Fig. 20 shows this
a r r a n g e m e n t in s e c t i o n a l e l e v a t i o n . It needs very
little e x p l a n a t i o n except to point out that the effect
of p r e s s u r e i n t h e p a n will b e to f o r c e s o m e of the
liquid mixture u p the pipe (a), t h e r e b y compressing
t h e a i r i n t h i s p i p e a n d f o r c i n g t h e oil of t h e oil s e a l
round the loop (6). This will compress the air
FIG, 20.—Special Pressure Regis-
tration Device.
g e t p a s t t h e oil seal n o r c a n t h e oil itself b e driven

up into the gauge, as in each ease there is this
e l a s t i c a i r c u s h i o n a c t i n g , s o t o s p e a k , a s Bi b u t t e r .
Fig. 21 contains nothing new, it merely shows
h o w these last two devices can be arranged neatly
in order to use only one hole through the autoclave

cover. T h e safety valve (A) can consist of the
arrangement shown in Fig. 19 or any other type
Oil seal
FIG. 21.—Safety Pressure Device and Special

Manometer Connection.
considered to be suitable for particular require-

ments. It should be noted that there is one
objection to this particular combined fitting of
m a n o m e t e r a n d safety valve, for in the event of
the safety valve blowing, the c o n t e n t s of the auto-
The High Pressure Wtrt< Aufwhw 111
clave will be driven by t h e prc-^nrt- through the

ruptured plate and down t h e p:p* to the drain or
trap, which will present the chemist with the
unpleasant problem of getting a purtlaiiy reacted

and possibly solidified b a t c h kitjk again into the
a u t o c l a v e for t h e c o m p l e t i o n of t h e r e a c t i o n !
T H E H E A T I N G O F W O R K S
A U T O C L A V E S
C H A P T E R V I I
THE. HEATING- OF WORKS AUTOCLAVES
I N discussing the heating of l a b o r a t o r y or semi-

large-scale plant it was seen that there was very
little to be said a g a m s t oil-bath heating and m u c h
to be said in its favour. I n certain cases, it is
true, it was stated that oil-batli working was
unnecessary and that gas firing, for example, with
p r o p e r baffles t o p r e v e n t b u r n i n g w a s all t h a t could
be desired. Still, this was hardly a criticism of
the oil-bath, but merely the expression of opinion
that an alternate method of h e a t i n g would meet a
particular case. The problem of h e a t i n g of works
a u t o c l a v e s is, h o w e v e r , a v e r y different proposition,
for there are factors operating here which do not
come into play with other t h a n real manufacturing
conditions.
I n t h e first p l a c e , t h e t y p e of w o r k d o n e i n works
autoclaves is so different. Instead of a series of
isolated batches carried out on a very small or
moderately large scale mainly, if not solely, for
experimental purposes, we are faced with the
problem of routine manufacture in which i t " is
d e s i r a b l e t o g e t a s m u c h o u t of a n y p l a n t i n a given
time as is possible. Then, again, the heating of
laboratory or even semi-large-scale autoclaves of
the smaller sizes b y means of coal or coke fires is
out of the question, as it would be impossible to
regulate or control such tiny furnaces, whereas
the coal or coke furnace is probably the most
economical and general method of actually firing
works pans.
115
If an oil-bath is e m p l o y e d it m a t t e r s very little

-whether it is h e a t e d b y fire or b y gas burner, for,
after all, it is the hot oil which really heats the
autoclave. So to systematise this subject as m u c h
as possible we will consider the following three
methods of heating in turn, pointing out the
advantages or disadvantages of each and drawing
conclusions therefrom:
(1) Heating b y oil-bath.
(2) Heating b y direct heat from coal or

coke fire.
(3) Heating b y direct heat from gas burner.
(1) As the n a m e implies, this means that the

autoclave is partially immersed in a bath of oil
generally to within 6 inches of t h e cover flange so
t h a t t h e l e v e l of t h e oil is a little a b o v e t h e l e v e l of
the charge. T h e type of oil chosen depends on
the temperatures required, b u t a good thick black
oil of coal tar or petroleum residuum origin is
generally employed. T h e oil m u s t possess certain
characteristics. It m u s t h a v e as high a flash-
point as possible—certainly well above t h e tempera-
t u r e t o w h i c h i t is r e q u i r e d t o b e h e a t e d i n o r d e r to
give the desired inside temperature to the charge.
In this connection it m u s t be remembered that
there m a y be a " lag " or difference in temperature
between oil-bath and charge due to losses by
r a d i a t i o n of as m u c h as 40° C , so t h a t if a n inside
temperature of 180° 0. is required the oil should
certainly not " flash " below 250° 0. This presents,
however, very little difficulty, since satisfactory
The Heating of Works Autoclaves 117
oils can be obtained which do not flash till well

above the zone of m o s t autoclave work. Another
important property of an oil-bath oil is that it
must be not easily " cracked/' i.e., decomposed
when maintained at these high temperatures for
long periods. It must resist oxidation and its
viscosity and general physical properties m u s t
be unchanged after m a n y rises and falls in
temperature.
Of course, one cannot expect perfection and no

oil can be used indefinitely, but as the emptying
and refilling of an oil-bath is a m e s s y and tedious
business, this operation should not be necessary
more than two or three times a year.
As regards the heating of the oil-bath there is

little to require explanation. Whether heated b y
g a s b u r n e r s o r fire, i t s h o u l d b e d o n e i n s u c h a w a y
a s t o a v o i d b u r n i n g t h e oil a t t h e b o t t o m and sides
of t h e bath. After all, oil is a n organic substance
and must not be treated too roughly as regards
heating. The chemist who never forces his baths,
but nurses them carefully to the desired tempera-
ture, reaps the benefit in having much longer runs
between dismantling and m u c h less labour in
cleaning up baths and autoclaves before restocking.
T h e o n e g r e a t v i r t u e of o i l - b a t h h e a t i n g i n which
r e s p e c t i t is s u p e r i o r t o a l l o t h e r f o r m s i s , of course,
that the charge receives uniformity of h e a t i n g and
that the possibility of local burning is reduced
to a m i n i m u m , if n o t e n t i r e l y obviated. With the
thickest mixtures, given reasonable agitation under
this s y s t e m of heating, the autoclave charge is at
a uniform temperature throughout even during

heating up a n d cooling down. A further advantage
is t h a t the u s e of a n oil-bath will p r o b a b l y prolong
the life of an autoclave, although whether the
capital value thus gained compensates for the other
costs associated with oil-bath work is a debatable
question. H a v i n g stated these points, one has
practically exhausted the list of advantages of
oil-bath heating over the best forms of direct
firing. There are, too, some disadvantages con-
nected with the use of oil-baths for large-scale
work which do not operate in laboratory or semi-
large-scale.
The greatest of these drawbacks is the very

considerable length of time inevitably taken in
raising an autoclave to a desired temperature b y
means of an oil-bath, as compared with direct
firing, a n d the corresponding length of time taken
by the charge in cooling when the containing
vessel is oil-j a c k e t e d . It m a y not always be
possible to e m p t y an autoclave immediately the
reaction is over—perhaps the temperature and
pressure are too high—which will necessitate the
cooling d o w n of t h e c h a r g e b y , s a y , 5 0 ° C.
W i t h a direct fired p a n this would take, perhaps,

three hours, b u t treble this time with an autoclave
s t a n d i n g i n a b a t h of h e a t e d oil. This disadvantage
operates in t w o ways, and is more serious than
appears at first sight. I n the first place, it restricts
the output of the plant so t h a t a p a n capable of
making, say, five b a t c h e s a w e e k if d i r e c t fired, can
only turn out three if oil-bath heated. I n the
The Heating of Work? Autoclaves 110
second place, this greater period of time taken in

h e a t i n g u p a n d c o o l i n g clown is a s e r i o u s departure
from t h e c o n d i t i o n s of a n y r e c i p e w h i c h w a s in the
first place worked out in a laboratory where the
t i m e s of h e a t i n g a n d c o o l i n g w e r e v e r v s h o r t . The
u s e of o i l - b a t h s m e a n s often considerable modified-
tions in recipe times and frequently means that
recipes involving only short times can hardly be
successfully imitated at all. As plant is nearly
always used for routine production, the first
objection is a serious one, which m a y mean that
much greater capital must be sunk in plant for a
given monthly output when oil-hath heating is
u s e d i n s t e a d of d i r e c t firing.
W i t h o u t wishing to lay down any hard and fast

r u l e i t is p e r h a p s fair t o s t a t e t h e e a s e t h u s :
Where large output to the limit of a plant's
capacity is n o t essential a n d where the substances
involved are damaged if heated to temperatures
o u t s i d e r i g i d l i m i t s , a n d w h e r e t h e r e c i p e is capable
of m u c h latitude as regards the length of heating.
then oil-bath heating is clearly indicated, it is
again desirable in works where plant depreciation
m u s t b e r e d u c e d t o its lowest possible state regard-
l e s s of loss of output.
In most c a s e s of r o u t i n e m a n u f a c t u r e , however,
it is p r o b a b l e that the best forms of direct firing
if carried out under experienced guidance possess
advantages over the oil-bath m e t h o d which exceed
their drawbacks.
(2) I t is n o t proposed to complicate the subject

by g o i n g i n t o d e t a i l s of t h e r e l a t i v e advantages of
coal or coke firing o v e r gas firing in direct he&ted

pans. Generally speaking, so m u c h depends on the
facilities available, b u t i t is a f a i r l y s a f e generalisa-
t i o n t o s a y t h a t of l a t e y e a r s g a s - h e a t i n g appliances
have improved so wonderfully that they are
encroaching into fields at one time held entirely
by K i n g Coal. Still3 most chemists or engineers
faced with the problem of heating an autoclave
will h a v e t o e m p l o y t h e coal or c o k e fire.
At first glance the joroblem m i g h t seem to consist

of nothing more complicated than the building of
a brickwork support for the autoclave and the
provision of a fire-box beneath it. If that were
done, however, there would be, it is to be feared,
m a n y charred batches in that autoclave and the
log-book would show strangely variable yields from
day to clay !
P u t as a general statement the problem of cor-
rectly and safely firing a n autoclave by direct heat
is s o l v e d b y the provision of t h e f o l l o w i n g :
(1) A brickwork support for the autoclave,

the top of which forms the staging which is
on a level with the cover a n d manhole.
(2) A fire-box, w e l l in f r o n t of t h e autoclave,

with a firebrick arched roof leading to the
space under a n d round the autoclave.
Ci
(3) Suitable baffles " whose function is to
block out too fierce heat rays and flames and
to direct the hot gases into a definite p a t h so
that the whole of the autoclave is uniformly
5
heated in a " hot air bath.'
(4) Fire-box door and dampers so that the
heating can be regulated to a wonderful
d e g r e e of accuracy.
Cover flange
Brickwork indicsted thus fHi;
F I G . 2 2 . — A r r a n g e m e n t f o r D i r e c t F i r i n g of a n Autoclave.
A very general arrangement for direct firing of

an autoclave is s h o w n in Figs. 223 23 and 24. It
has been necessary to give these tliree sectional
views in order to show all essential parts of the
setting, and a s t u d y of t h e s e diagrams in detail is
recommended. T h e y represent, as h a s been stated,

a general arrangement a n d one that works fairly
satisfactorily for the firing of an autoclave con-
taining a mobile mixture which is well agitated.
T h e m e t h o d of circulating the hot gases a n d con-
^ . Q'-Q\ _->j
F I G . 2 3 . — A r r a n g e m e n t f o r D i r e c t F i r i n g of a n Autoclave,
sequent h e a t i n g of t h e s i d e s of t h e p a n i s g o o d , a n d
although this setting possesses one grave defect,
this can be obviated b y an addition rather than b y
complete reconstruction so t h a t the design deserves
description as it stands, especially as it is a n
arrangement in very c o m m o n use. I n order to
The Heating of WorJes Autoclaves 123
fully understand the design let us consider Figs.

22 and 23 together. The former is a sectional
side elevation and the latter a sectional p l a n as
seen from above.
The autoclave rests on a two-course brickwork
F I G . 2 4 . — A r r a n g e m e n t f o r D i r e c t F i r i n g of a n Autoclave.
w a l l w h i c h s t a r t s a t o n e s i d e of t h e fire-bos tunnel
(X, Fig. 23) a n d passes r o u n d to t h e other side (Y)
as a n u n b r o k e n circle s a v e for a g a p a b o u t 18 inches
a c r o s s (Z). T h i s wall is a b o u t 3 feet high. S o m e
further support could be given b y allowing the
flange of the autoclave to rest in p l a c e s on brick-

work supports at the top, but that r n i g h t m a k e it
difficult t o g e t a t t h e c o v e r b o l t s a n d is u n n e c e s s a r y
even with large pans. Turning to K g . 2 2 , we see
that the fire-box (A), which will be a b o u t 2 feet
in length, 18 inches across and a little more in
height, terminates in a short wall (B) a n d leads
over this into the circular space b e n e a t h the
pan (C). The heat and flames from t h e fire pass
over the wall (B) into the space u n d e r n e a t h the
pan, and from thence through the gap (Z/, K g . 23)
into the outer circular space (if) (Fig. 2 3 ) , This
space is a l s o marked (M) for the sake of clearness
in Fig. 22. The hot gases circulate all r o u n d the
s i d e s of t h e p a n , f o r t h e only outlet to t l i e flue lies
o v e r a b a f f l e w a l l (N) ( F i g . 23), which is a l s o about
3 feet in height and serves to prevent t o o rapid
suction into the flue and consequent c o o l i n g of the
side of the pan near (Y). Having therefore h a d
free access u n d e r and round the p a n the l i o t gasses
are allowed to escape into a flue 9 i n c h e s square
through a small hole and pass down t h i s before
being finally led into a suitable chimney. Pig. 24
shows the front sectional elevation, and a s t u d y of
the three diagrams taken together with t h e above
explanation should m a k e this rather intricate
matter clear.
Without being too specific it has been t h o u g h t

advisable to indicate the relative sizes of various
parts of this setting b y giving a few d i m e n s i o n s
both in the text and in the diagrams, a n d these
can be taken as roughly suitable-for a large works
autoclave of seven or eight hundred gallons
Such a setting could be used for heating oil-

baths if it was decided to place the autoclave in
one. although it would hardly be necessary to
baffle t h e g a s e s q u i t e so t h o r o u g h l y in t h a t case.
It has been stated that this arrangement pos-
FIG. 25.—Showing ** B a i r l e " " b e t w e e n Fire-box ami

Autoclave.
sesses o n e g r a v e defect, a n d doubtless t h e discerning

reader will h a v e detected it. Of course i t is that
the flames will b e d r a w n by the draught right into
the open space beneath the pan and will impinge
on the bottom, thereby causing burning of the
c h a r g e a n d d e t e r i o r a t i o n of t h e p l a n t . The author
h a s a c t u a l l y s e e n t h e b o t t o m of a n a u t o c l a v e bright
red hot through too rapid firing hi such a setting.
This defect, enormous as it seems, c a n be overcome

b y a very simple device. This consists in building
up the wall (J3) (Fig. 22) until it reaches the roof
of t h e arch beyond the fire-box, not, of course, as
a complete wall, which would cut off a l l h e a t from
5
t h e p a n , b u t a s a baffle of " p i g e o n - h o l e s / This is
shown in Figs. 25 and 20, which are side sectional
elevations and front elevation respectively. The
FIG. 26.—Showing " Baffle " b e t w e e n Fire-box and

Autoclave.
effect of t h e e r e c t i o n of t h i s baffle is r e m a r k a b l e , as
with a good draught it does not d a m p d o w n the
fire, but entirely prevents the actual flames entering
the space beneath the autoclave, which is to all
intents a n d purposes heated b y a hot air-bath.
Such a modified setting, properly a n d skilfully
worked, is an almost ideal method of firing pans
m t e n d e d for h a r d routine use, a n d one w h i c h allows
the m a x i m u m output to be obtained from the plant.
Once the autoclave lias been raised to the desired
temperature it is surprising h o w small a fire will
keep it steady, a skilled w o r k m a n being able to
regulate the temperature of the charge to within
a degree or two by a combination of intelligent
Flanges of autoclave
Dampen
Body of autoclave
Airspace Air space

Gas burners
4
Regulator
F I G . 2 7 . — S e c t i o n a l E l e v a t i o n of a S e t t i n g t o a Gas-
heated Autoclave.
stoking and adjustment of the flue damper and

furnace door,
(3) I n conclusion, a few words m u s t be said about
gas-heated autoclaves. E v e n large pans of four
or five hundred gallons capacity can now be
heated b y gas. I t is usual to have the burners
some little distance underneath the pan, heating
up being started by a small flame in order to avoid

burning. Gas heating can be regulated so finely
that the same elaborate system of baffles is not
required as is the case with coal fires, the simple
expedient of running a baffle plate three-quarters
of the circumference of the autoclave to force the
heated air to encircle the body of the pan being
sufficient. Although m u c h of the regulation is
d o n e b y m e a n s of t h e g a s s u p p l y t a p s , i t is advisable
to have a clamper in the flue as well, and this
enables one to keep the whole of the space round
the autoclave full of h o t gases, which slowly circu-
late against the baffle and over it a l o n g the upper
part of t h e p a n to the flue.
Fig. 27 shows a simple setting to a gas-heated

autoclave in s e c t i o n a l elevation.
T H E W O R K I N G O F L A R G E - S C A L E
A U T O C L A V E S
C H A P T E R V I I I
THE WORKING OF LARGE-SCALE AUTOCLAVES
W H E N considering the use of laboratory auto-

claves a few typical examples of reactions best
carried out in such apparatus were given. It is
not, therefore, proposed to go into.the chemical
side of working plant, as this must necessarily
be similar to that already considered, but rather
to pay attention to those details of plant usage
in which large and even semi-large-scale work
differs f r o m t h e p r o c e d u r e of t h e laboratory.
A chemist who knows perfectly h o w to carry out

a certain operation at his bench will meet with
all m a n n e r of technical troubles when faced with
the problem of manufacturing from that same
specification on a large scale, so that it is the
object of t h i s c h a p t e r to anticipate to some extent
these troubles and to show h o w they can be m e t
and overcome.
The best method of so doing is t o imagine our-

selves in charge of an autoclave engaged in the
manufacture of any of those important hydrqxy-
or amino-hydroxy-derivatives of n a p h t h a l e n e which
are prepared b y the fusion of a sulphonic acid
with caustic soda. Such an o p e r a t i o n will probably
be carried out in the large low pressure agitator
pan previously described, o r , if t h e t e m p e r a t u r e of
fusion were very high and the concentration of
caustic soda low, w h e r e b y great pressures w o u l d be
generated, in the rather smaller autoclave working
up to 30 atmospheres. B y far the most likely
pressures would, however, be in the region of
131
7 or 8 atmospheres, so that the low pressure pan

could be employed.
Before coming to the actual mechanical side of
the subject a few words on the question of batch
control tests would not be out of,place. In order
to get the best results from his plant the works
chemist should keep a very complete record of all
conditions in his log-book. The size of the batch
should be the largest that the plant will safely
take, remembering that no autoclave should be
filled to more than 8 0 % of its total capacity in
order to allow for expansion of t h e l i q u i d contents
under heating.
In the laboratory the chemist has probably used

a pure dry powdered sulphonic acid to melt,
whereas in the works he m a y be delivered a paste
containing not only water, but possibly also free
mineral acid. In his calculation for the amount
of caustic to give the required concentration he
must, therefore, make allowance for the following :
(1) Caustic used in neutralising the free

mineral acid (if any).
(2) Caustic used in neutralising any acid
g r o u p s i n t h e m o l e c u l e of t h e s t a r t i n g material.
(3) T h e water formed by any such neutralisa-
tions.
(4) T h e water actually present in the paste
of t h e s t a r t i n g material.
Having m a d e any such allowances that the

particular case m a y render' necessary, he finally
The Working of Large-scale Autoclaves 133
arrives at a figure for t h e caustic t o be used a n d the

extra w a t e r to be added.
E v e n if t h e p r o c e s s i s a very steady regular one,

a good control c h e m i s t will a r r a n g e to t a k e samples
a t c o n v e n i e n t stages for w o r k i n g u p in t h e laboratory
in order to get some approximation of yields.
B y this means if any stage of the process is not
working properly—if the plant is leaking in any
^vvay—that defective stage will be s h o w n u p b y the
figures of the control tests a n d can be put right
before a n y great financial loss h a s occurred. When-
ever i t is possible t o k e e p individual batches separate
this s h o u l d be done, and the log-book should always
s h o w t h e y i e l d s of e a c h b a t c h t h r o u g h o u t t h e week,
m o n t h , or year. The author once had occasion to
investigate a mysterious loss of yield in a process
which u p to that time h a d worked perfectly
satisfactorily. Such a system of y i e l d estimations
b y samples taken at each stage in the process
s h o w e d the leakage to occur between a certain
vat a n d filter-press, and it w a s found that a small
hole h a d developed in the storage boiler sunk in
t h e g r o u n d i n t o w h i c h t h e s u s p e n s i o n of t h e material
w a s r u n before blowing it b y compressed air through
the filter-press. The effect of the compressed air
was t o blow a certain a m o u n t through this hole
into t h e ground at each operation of filtration.
This example shows h o w necessary routine tests
are in order to discover defects before great loss
has occurred.
T o return to the manufacture of our hydroxy-
d e r i v a t i v e , l e t u s s u p p o s e t h a t t h e s i z e of t h e batch
has been fixed a n d al] c a l c u l a t i o n s h a v e b e e n made.

The first p r o b l e m is, t h e r e f o r e , t o w e i g h o u t so much
caustic s o d a a n d t o m e l t it w i t h t h e r e q u i r e d amount
of w a t e r . T h e caustic soda m a y be in the form of
rock, delivered in thin sheet-iron drums, or in
the form of powder or flake. If it is r o c k caustic
then the d r u m s m u s t be split open by sledge
h a m m e r a n d t h e solid m a s s broken"up to l u m p s not
bigger t h a n small loaves of bread. The powder
or flake caustic can naturally be charged into the
water just as it is.
Caustic soda is a d a n g e r o u s substance to handle,

a n d it is the d u t y of the chemist to see that his
m e n are educated to this danger and protected
adequately, even if, i n t h e i r i g n o r a n c e , they object
to the precautions. I n a n y operation involving
the throwing about of caustic b y shovel or the
breaking of rock caustic by hammer, comfortably
fitting goggles should be worn b y the m e n con-
cerned. Strange as it m a y seem a t first thought,
w o r k m e n often prefer to use rock caustic, although
it involves the huge labour of breaking up, to the
powder or flake form, the reason being that the
s h o v e l l i n g of p o w d e r e d caustic causes so m u c h dust
to get into the air, which leads to intolerable
itching of the eyes, nose a n d skin. Perhaps the
best form of all is a g o o d dry flake which does not
contain m u c h dust.
If n o liner is u s e d in t h e autoclave it is essential

that the operation of melting the caustic with the
requisite water be carried out in a separate pan,
not in t h e autoclave. T h e f u s i o n of lumps of rock
caustic or even any form of caustic with a small

quantity of water should never he earrid out in a
steel vessel, a s it a t t a c k s t h a t material much more
readily than it does cast iron. If the sulphonic
acid paste contains much water, then the con-
c e n t r a t i o n of c a u s t i c i n t h e e x t r a w a t e r w i t h which
it is f u s e d p r i o r t o c h a r g i n g the paste will he very
high—perhaps 7 0 % — a n d such a hot fusion will
play havoc with a riveted steel autoclave. If this
o p e r a t i o n is, h o w e v e r , d o n e in a cast-iron p a n and
the fusion blown over into the autoclave immediately
prior to the charging of t h e paste, then very little
harm is d o n e . The blowing o v e r of s u c h a fusion
does not sound a nice job, but if r e a s o n a b l e care
is t a k e n i n m a k i n g j o i n t s , a n d m e n a r e i n s t r u c t e d to
" s t a n d c l e a r " w h e n t h e a c t u a l b l o w i n g is started,
no harm need result.
In order to save time a small fire should he
started m the furnace of t h e a u t o c l a v e before the
fused caustic is b l o w n into it, as by so doing the
brickwork is heated up and the pan itself made
just reasonably warm. A little experience will
soon show how much to heat the autoclave, the
o b j e c t being to p r e v e n t t h e s u d d e n chilling causing
the fused caustic to solidify on coming into the
pan.
As soon as the caustic is hi the autoclave the
agitator is set in motion and charging of the
sulphonic acid is commenced. This operation is
carried out as rapidly as possible, care being taken
t o r e g u l a t e t h e r a t e of c h a r g i n g a n d t h e firing up so
as to h a v e a steadily rising t e m p e r a t u r e throughout.
If the sulphonic acid is in the form of a paste

containing free mineral acid, or if it contains a
n u m b e r of free sulphonic acid groups, then the
heat of neutralisation is considerable and helps
to compensate for the cooling effect of t h e m a s s of
material added.
Naturally it is impossible to fix details too

specifically, but for most operations of t h i s nature
Ct
a large batch of t h r e e or four p o u n d molecules "
could be charged in from four to six hours, and the
temperature at the end should be from 120° to
130° C Care m u s t be taken in charging some
pastes to avoid adding in such sized lumps or so
rapidly as to prevent the rotation of the agitator.
This is k n o w n b y the w o r k m e n as " scotching the
5
pan/ a n d the problem of persuading the agitator
to start again in a badly " scotched " p a n is n o t as
humorous as the n a m e given to the disorder.
It sometimes means hours of p a t i e n t l e v e r a g e with
a long bar shaped to a blade like a cold chisel, witli
which the bevel cogs are turned little b y little.
W h e n the agitator has thus been turned back, say,
half a revolution, the belt is slipped gently on to
the fast or driving pulley a n d b y vigorous slapping
on of the belt one endeavours to persuade the
agitator to run round through the obstruction and
so start r o t a t i n g s m o o t h l y once more.
Some rough treatment m a y be needed to cure a

3
bad " scotch/ but too m u c h vigour m a y lead to
stripped teeth on the gear wheels, or bent and
broken agitator blades.
There never was an operation to which the motto

" more haste, less speed," was better applicable

than that of chargmg an autoclave with lumps of
heavy hydraulically pressed cakes of sulphonic
acids, but once again it is wonderful to observe
the degree of skill which can be acquired b y a
really experienced workman.
As soon as the batch is c h a r g e d no time should

bo lost in sealing up. This involves the fitting of
the m a n h o l e lid, for it has been through the man-
h o l e , of c o u V s e , t h a t t h e charge has been added.
The m a n h o l e lid in l a r g e p a n s is a fairly massive

article weighing a hundredweight or so, and the
o p e r a t i o n of fitting it r e q u i r e s j u s t a little " knack."
It is usual first to fit the wide flat blackleaded
asbestos ring in its special groove on the top side
of the lid, and then, by means of chains looped
t h r o u g h t h e ring in t h e lid (see F i g . 17) a n d stayed
over any convenient piping, to lower the lid until
it hangs just over the manhole itself. One m a n
will now take the strain on the chains, while his
mate, by turning the heavy lid e d g e w a y s a n d side-
w a y s , will slip it t h r o u g h t h e hole. Once inside the
p a n i t is a d j u s t e d to the correct position and then
guided upwards u n t i l t h e a s b e s t o s r i n g is felt t o be
pressing evenly against the rim designed for the
purpose. All this time the weight is b e i n g borne
b y t h e c h a i n s , b u t n o w o n e c a n s l i p o n e of t h e bars
through the rods of the lid and spin the great
hexagonal n u t down to take the strain. The chains
are r e m o v e d , t h e second b a r a n d n u t fitted a n d the
process of tightening up is proceeded with. The
nuts are usually screwed up with box keys or
5*
spanners, tightening b y means of a long lever bar

being preferable to h a m m e r i n g up. T h e ther-
mometer is now, and only nowi placed in its oil
pipe to avoid previous risk of breakage a n d all is
ready to fire u p to temperature. I t is a g o o d plan
to educate the m e n to m a k e a practice of clearing
away all r u b b i s h — o l d casks, papers, etc.—and to
sweep the cover of t h e p a n a n d t h e staging before
firing up, as a neat, tidy staging helps to suggest
that atmosphere of a c c u r a c y which is s o necessary
in autoclave work.
A chart should always be provided on which entries

showing time, temperature ( b o t h of t h e c h a r g e and
oil-bath if t h e latter is employed), pressure, and
general observations should be m a d e every half-
hour. A p a r t from the m e n required for charging,
one skilled h a n d can look after a n u m b e r of auto-
claves as they are coming u p to temperature,
especially if h e has a stoker to fire u p under his
direction. This skilled h a n d will attend to the
charts a n d watch ceaselessly for leaks developing
in glands, manhole lid joints, cover joints or taps.
H e will also see that the oil c u p s o n the bearings
are working properly, for no one w h o knows h o w
to get the best out of machinery will allow it to
squeak or groan complainingly without investi-
gating the cause and, if possible, supplying the
remedy.
The time that it is n e c e s s a r y for t h e b a t c h to be

kept on temperature and, for that matter 9 the
temperature itself, depends on t h e particular
reaction which is b e i n g carried out. I n the case
of caustic fusions of naphthalene sulphonic acids

we can, however, take from two to twelve hours as
a reasonable range. A t the end of the specified
t i m e it will b e t h e object of t h e chemist to get the
temperature lowered as quickly as possible. There
are t w o m a i n reasons for this. I n the first place it
is not generally advisable to keep the reacting
bodies " on temperature " or near t h a t temperature
any longer than necessary, as the recipe has been
worked out carefully to fix the time at which the
best yields or purest products are obtained. Pos-
sibly longer time after a reasonable latitude will
cause over-melting or the substitution of a second
hyclroxy-group for a sulphonic acid one, or, per-
h a p s , it m a y c a u s e d a r k e n i n g of t h e p r o d u c t . One
should remember that a laboratory working is
always carried out in a shorter time than a works
one of the same recipe, so in order to keep as
faithfully as he can to laboratory recipe conditions
a works chemist must avoid unnecessary loss of
time. T h e second reason for speed in lowering the
temperature of t h e b a t c h is a n economic one. As
will b e s e e n , i t is u s u a l t o e m p t y the autoclave by
blowing over the contents through a pipe fitted
in a light manhole lid w h i c h is s u b s t i t u t e d for the
heavy one. This means that the pan must be
opened, a n d in order to do so all p r e s s u r e m u s t be
released. E v e n in t h o s e p a n s fitted with permanent
blow-over pipes it is not desirable to blow over
strong caustic fusions at very high temperatures
and pressures, so that some cooling and release of
pressure will be necessary in any case before the
pan can be evacuated. T h a t was w h y this reason
was described as a n economic one, for a n autoclave
represents capital, and t h e l o n g e r i t is o c c u p i e d on
o n e b a t c h t h e less will b e t h e m o n t h l y output from
that capital.
The usual procedure with caustic fusions and
m a n y other autoclave operations is to draw the
fire o n c o m p l e t i o n of t h e r e a c t i o n t i m e a n d t o open
fully t h e fire-box door and flue, while the blow-off
v a l v e is cautiously released too. N a t u r a l l y if the
p r o d u c t is v o l a t i l e i n s t e a m t h i s l a t t e r c o u r s e cannot
be adopted, but wherever possible it should be
d o n e , f o r t h e r a p i d b o i l i n g off of s o m e of t h e water
has a marked effect on the cooling rate of the
batch.
The degree to which this treatment can be pushed

and the temperature to which the batch is cooled
are factors which only experience in any particular
recipe can fix, but as a general working rule one
can say that caustic fusions can be safely and
conveniently blown over at 120° C , and that a n y
p a n s h o u l d b e o p e n e d a s s o o n a s t h e r e is n o residual
pressure. The blow-off pipe does away with a n y
trouble caused by residual pressure due to gases
formed by decomposition, but to avoid the possi-
bility of accidents the following procedure should
be adopted in opening a large works autoclave.
A s soon as t h e blow-off pipe ceases t o s h o w emission
of gas or steam and the needle of the gauge is
at zero (which is best seen b y striking the gauge
a s m a r t b l o w w i t h t h e p a l m of t h e h a n d , when the
needle should " click " against the pin near the
zero mark), then the hexagonal nuts on the rods

of t h e m a n h o l e lid s h o u l d b e l o o s e n e d with a long-
h a n d l e d s p a n n e r — s a y a No. 6 or 7 adjustable. The
heavy lid will probably remain stuck against the
asbestos ring, b u t a smart tap with a long bar will
cause it t o ease, and once steam is s e e n escaping
the chains can be fixed and the lid removed by
exactly the reverse process to that described in
fitting it.
A very common method of loosening the man-

hole lid, and one which, although it sounds
dangerous, is probably perfectly safe in practice,
is as follows. A s s o o n as t h e c h a r g e h a n d sees that
only a few pounds per square inch pressure is
shown on the gauge, and while the blowing off
still c o n t i n u e s , h e loosens t h e n u t s of the manhole
lid a considerable amount. This has no effect,
for t h e remaining internal pressure holds u p the lid
against the manhole. The charge hand busies
himself with other jobs, knowing that as soon as
the pressure is r e l e a s e d a characteristic crash will
tell him that the lid h a s " dropped," i.e., has slid
down the rods just as far as he loosened the nuts.
H e then can attend to the removal of t h e lid and
subscquejit operations.
Once the heavy lid has been removed a light

" blowing-over " lid is fitted. I t is e x a c t l y similar
in design a n d general construction to the heavy one,
only m u c h lighter, as it has only a few pounds per
square inch of air pressure to withstand. In the
c e n t r e of t h i s l i d is a r o u n d hole for t h e blow-over
pipe, which fits down to a flange on the pipe, a n
air-tight joint being m a d e with small nuts and

bolts against a flange r i n g of r u b b e r , composition,
or asbestos. The blow-over pipe is shaped to go
to as near the bottom of the pan as possible, and
terminates at the top in a union joint which is
m a d e on to the permanent pipe lines in the shed.
In a well-designed shed the pipe lines will be such
as to give the chemist a considerable variety of
vats into which he can blow his batches, and also
some form of emergency receptacle into which he
can p u t a batch a s a l a s t r e s o r t i n c a s e of complete
breakdown of vats or pipe lines. W h e n one
remembers that the value of a batch m a y be
several hundred pounds, a little thought and
expense in planning for emergencies are not out
of p l a c e . As an example of e m e r g e n c y receptacles
one m a y quote boilers sunk in concrete pits and
floored over. These are not expensive, are out of
the way, and come in very useful as storage tanks
for liquors and as temporary resting-places for
b a t c h e s w a i t i n g t h e i r t u r n if t h e p l a n t is w o r k i n g at
full c a p a c i t y and the inevitable breakdowns occur.
To return to the blowing over of our autoclave

contents. Having fitted the light lid, m a d e good
the blow-over pipe, and connected up to the
permanent piping, then there is a g o l d e n rule that
every chemist or foreman, no matter h o w experi-
enced, should invariably follow. It is this :
Hake sure that only those valves are open which lead
to the desired destination of your batch.
In a complicated t a n g l e of p i p i n g i t is surprising
h o w e a s y it is t o omit to close o n e of m a n y paths.
The author has known of v e r y m a n y cases—some

humorous, some tragic—where batches have been
blown over into the most unlikely places, m u c h to
the surprise of the " b l o w e r " and "receiver,"
t h r o u g h t h e n e g l e c t of a t t e n t i o n t o t h a t g o l d e n r u l e !
Again, t h e n , let it b e r e p e a t e d — f o l l o w your pipe

line from the autoclave to the vat, or to wherever
be the destination of the batch, and see that all
valves are closed save those required to direct
the route. Then all taps on the pan should be
watched, and finally, when everything i s known to
be right, give a warning shout to the men at the
" receiving " end and turn on the compressed air.
There is some romance even in the life of a

w o r k s c h e m i s t if o n e c a r e s t o l o o k f o r i t , a n d perhaps
of all moments the one that gives the greatest
feeling of pride is when one sees one's " first
batch " passing smoothly a n d without hitch in a
great stream full bore through 3 inch pipes,
splashing' triumphantly from the autoclave into
the vat on the staging above.
It has been shown that considerable time must

elapse between the completion of t h e r e a c t i o n and
the b l o w i n g o v e r c a u s e d b y t h e s l o w r a t e of cooling
of the autoclave contents. This is p a r t i c u l a r l y so
in those cases where it is impossible to blow off
steam by reason of t h e v o l a t i l i t y of t h e p r o d u c t in
that vapour, and most particularly so in oil-bath,
heated autoclaves used for such operations. I n
cases like these one m a y have to allow as m u c h as
twelve hours before blowing over can be carried
out. Naturally such a disadvantage calls for
investigation in order to see whether a means of

saving this valuable time can be devised.
The greatest l o s s of t i m e is c a u s e d by having to
wait until all pressure has disappeared in order to
c h a n g e t h e m a n h o l e lids a n d fit t h e blow-over pipe,
a n d it is i n o r d e r t o do away with this part of the
process that autoclaves have been designed with
blow-over pipes fitted permanently. Although
in some cases they m a y work satisfactorily, yet
on the whole this design has not been favourably
received by most chemists. One great objection
is t h a t these fixed bloAv-over p i p e s a r e v e r y apt to
get silted u p with solid m a t t e r and so t o refuse to
work at the desired time, while another drawback
is the additional likelihood of leakage during
heating.
Perhaps the most reliable and neatest w a y of

reducing the time required between completion
of t h e r e a c t i o n and blowing over to a m i n i m u m is
that of utilising the hollow shaft carrying the
agitator blades as t h e blow-over pipe, and, provided
certain precautions are adopted, this is a m e t h o d
that works satisfactorily, say, with nine batches
out of ten, even in those cases whore m u c h solid
insoluble m a t t e r is c a r r i e d i n suspension.
In order to explain this most accurately, let us

consider two cases :
(a) The blowing over of a [3-naphthylamine

batch.
(b) The blowing over of a fairly thick
caustic fusion, containing salt and insoluble
matter in suspension.
(a) The points of interest here are that the

temperature a t t h e e n d of t h e r e a c t i o n will b e , say,
w i t h i n t h e r e g i o n of 140° t o 150° 0 . a n d t h e pressure
about 7 atmospheres. If the mass is c o o l e d down,
when a temperature well above 100° G. is reached
and before the jiressure has gone, the p-naj)hthyl-
amine will separate out in the form of lumps of
solidiiied oil or small balls like marbles. E v e n if
t h e o r d i n a r y b l o w - o v e r p i p e is fitted i t is impossible
to do anything until the batch is reheated u p to
about 120° (I to ensure complete melting of the
naphthylamine.
Suppose, however, we have a hoilow shaft with

h o l e s c u t i n t h e b o t t o m t o a l l o w e n t r a n c e of material
and fitted with a good " gland " tap at the top
a b o v e t h e g e a r i n g w h e e l s , t h e n if a n y s u i t a b l e piping
arrangements be m a d e so t h a t on skipping the
agitator connection can be m a d e b y m e a n s of a
union joint, it would be possible to blow over at
the end of the reaction through the hollow shaft
and gland tap into the pipe lines to the desired
vat. This could ho done either immediately,
using the 7 atmospheres residual pressure as the
blowing force, or, if this seemed too violent or
150° C. too hot, then one could wait a few hours
until the temperature was, say, 130° (J. a n d the
pressure 4 atmospheres.
There are one or two precautions it is wise to

take with (3-naphthyIaminc or a n y similar prepara-
tion. If one starts blowing through cold pipes,
the first lot m a y solidify in t h e gland tap, or even
in the pipe lines themselves on a winter's day,
especially if there is s o m e distance to travel from

autoclave to vat. It is necessary, then, to have
steam supplied so that the whole pipe line can be
steamed out immediately before opening the gland
tap and letting loose the batch. Again, suppose
the gland tap has leaked very slightly during the
twelve, or twenty-four, or even thirty-six hours
required for amidations. The effect will be a
gradual rising of the molten contents of the p a n
until they reach the cool portions of the shaft,
wherein they will soldify, thus rendering it impos-
sible t o blow-over this way. There are two things
which the " old hand " can do to guard against
this besides the obvious one of overhauling the
gland tap before each batch. The first is t o close
t h i s t a p before t h e p a n is c h a r g e d , t h u s imj)risoning
air in t h e entire length of p i p e f r o m the gland tap
t o t h e b o t t o m of t h e h o l l o w s h a f t . Under pressure
this elastic cushion of a i r w i l l o n l y allow the batch
to rise slightly in the hollow shaft, and there is a
chance that even with a small leak on the tap the
b a t c h will n o t h a v e risen u p at the end to the cool
parts of the shaft. The second precaution is to
have a good blow-lamp handy, and to play on the
top part of the shaft and the tap itself with the
flame just before blowing over, so as to melt a n y
of the product that m a y be suspected of having
been forced u p through leakage. This sounds
rather drastic treatment, but, if d o n e s e n s i b l y s o as
to gradually w a r m u p the offending part to a tem-
perature above the melting point of the product,
it is surprising how successful a trick of this
description can be. In the case of (3-naphthyl-

amine, if the temperature is about 145° C. and
p r e s s u r e 1 0 0 l b . p e r s q u a r e i n c h , a n d if t h e procedure
just described be carried out and ice and water
placed in the receiving vat, it is p e r f e c t l y safe to
connect up and blow over immediately the proper
amidation time is completed.
It is c u r i o u s how prejudiced m a n y chemists are

against blowing over in this w a y with a residual
pressure, but there is n o r i s k if r e a s o n a b l e care be
taken, and an immense amount of t i m e and worry
is saved.
(b) In the case of t h e caustic fusion t h e r e is not
the problem of the solidifying oil t o consider, but
w e a r e p r o b a b l y left t o ' d e a l w i t h a b a t c h a t a very
m u c h higher temperature on completion of the
fusion. This will have to be blown to a vat and
m a d e acid, and in this connection it is interesting
to note that a considerable quantity of the acid
necessary for neutralisation can safely be placed
with ice in the vat, provided the batch be blown
over slowly and steadily. It would hardly be
advisable to blow over a caustic fusion at, say,
200° C , so with the hollow shaft arrangement
the procedure on completion of the fusion time
would be to draw the lire, o p e n t h e flue, and start
blowing off s t e a m through the blow-off pipe. The
agitator m u s t be kept going right up to the m o m e n t
of c o n n e c t i n g u p the hollow shaft to the pipe lines,
which operation is d o n e a s s o o n as the temperature
has sunk to a more reasonable figure, say 140° 0.
The pressure m a y not be quite enough to send the
batch over—everything depends on the. con-

centration of the caustic and the height to which
the batch is to be lifted—but it can be supple-
mented with compressed air if required. The
p r e c a u t i o n of s t e a m i n g t h r o u g h t h e p i p e l i n e s should
never be omitted. I n some cases where m u c h solid
is in suspension it is f o u n d that the holes at the
5
bottom of the hollow shaft become " m a d e up.'
This is a troublesome fault, but can largely be
obviated if c a r e i s taken to ensure that the space
round these h o l e s is w e l l agitated. O n referring
b a c k t o F i g . 1 5 a t t e n t i o n i s c a l l e d t o t h e p l a t e s A, A v
the special function of which is t o keep the inlet

holes of t h e hollow shaft clear. With these extra
fittings and the careful following of t h e h i n t s given
when considering the blowing over of anridations
t h e r e is n o r e a s o n w h v h o l l o w s h a f t blowing should
not be m u c h more common than is t h e case.
R O U T I N E R U N N I N G O F L A R G E -
S C A L E P L A N T
C H A P T E R I X
ROUTINE EUNNING OE LARGE-SCALE PLANT
I N t h e p r e c e d i n g c h a p t e r t h e a c t u a l w o r k i n g of a
large-scale autoclave was elaborated in some detail
with a view to provide hints which might be help-
ful to t h e inexperienced. Thus, a typical autoclave
manufacturing process was taken and considered
step b y step from the charging of the starting
m a t e r i a l t o t h e b l o w i n g o v e r of t h e b a t c h . It was
not considered desirable to go into the details of
the subsequent working u p of t h e batch, for these
come under the heading of g e n e r a l c h e m i c a l works
processes rather than high pressure work. It is
p r o p o s e d n o w t o g o i n t o t h e q u e s t i o n of t h e working
of autoclaves from a rather broader viewpoint
to -
than heretofore. B y this one means the manage-

m e n t of high pressure plant rather than the mere
r u n n i n g of o n e i s o l a t e d a u t o c l a v e f o r o n e particular
batch, and although this is n a t u r a l l y a subject on
which i t is difficult to generalise, there are, never-
theless, certain rules the elaboration of w h i c h m a y
prove helpful.
Let us first consider the case taken in the last
chapter—namely, that of a chemist in charge of
one autoclave who is r e q u i r e d to turn out a maxi-
m u m output of a hyclroxy-derivative obtained by
the fusion with caustic soda of a sulphonic acid.
Such substances are very common in chemical
industry, particularly the intermediates for dye-
stulfs of the naphthalene series. Output from
JJ
p l a n t is a l m o s t a s important as the " yield of a
process. The former represents so much more
151
money coming from capital invested, while " b l u e

latter is, of course, the term used to indicate t l ^ e
production from a b a t c h calculated as a p e r c e n t a g e
of t h a t theoretically possible. It is n o t too m u c h
t o s a y t h a t m o r e skill is r e q u i r e d i n a w o r k s c h e m i s t
to squeeze the greatest possible output per w e e k
from his plant without injury to it than to o b t a i n .
good yields from t h e p r o c e s s h e is working.
In the case of the chemist with one a u t o c l a v e ,

much will depend on whether he has r e a s o n a b l e
shift facilities for w o r k i n g t h e p l a n t all t h r o u g h t f c i e
twenty-four hours of each day, but it is g e n e r a l l y
desirable to m a k e the following arrangements.
There will be a large shift working during t h e
hours that the chemist is himself present at t l x e
factory and during which all t h e essential parts o f
the process should be done. The remainder of t t t e
time, say sixteen hours, will be divided into t w o
shifts, each of which has the services of just a, &
m a n y m e n as are needed to keep the process g o i n g .
With experienced men, a charge hand and two g o o d
labourers should be able to attend to three a u t o -
claves d u r i n g t h e d a y shift, while t w o m e n on e a c l i .
of the night shifts will be sufficient. T h e o b j e o t
which should be aimed a t is o n e b a t c h p e r t w e n t y -
four h o u r s f r o m t h e p a n — S a t u r d a y m o r n i n g c o m i n g
in very useful for cleaning up, boiling out t h e
autoclave, and a general winding u p of t h e w e e k ' s
work. This will, of c o u r s e , b e p o s s i b l e o n l y if t h e
process requires a short time " o n t e m p e r a t u r e / '
for it is o b v i o u s that if t h e batch has to be m a i n -
tained at a certain temperature and pressure for.,
Routine Running of Large-scale Plant 153
s a y , t w e l v e h o u r s , t h e w h o l e of t h e o t h e r operations
could not be squeezed into the remaining twelve
hours of the day. Again, with oil-bath heating,
the ideal " one batch per pan per day " is hardly
practicable, but with good management, good
workmen and a short-time fusion it is possible if
a direct-fired p a n is used-
Let us, therefore, consider a typical time-table.
O n arriving a t the works at, say, 9 a.m., the chemist
will find the previous day's batch in the pan, the
fire d r a w n , a n d t h e p r e s s u r e b l o w i n g off. The morn-
ing will be spent in getting r e a d y the material for
the day's batch, breaking caustic, and weighing out
q u a n t i t i e s of t h e s u l p h o n i c a c i d , w h i c h w i l l probably
be in the form of m o i s t c a k e s o r d r i e d powder.
All this m a t e r i a l will b e g o t o n to t h e stage, and

if i t i s t h e c u s t o m t o m e l t t h e c a u s t i c i n a separate
pan, this can be charged and the melting started.
The m e n concerned with the working up of the
previous day's batch will have all in readiness
for the time when it is to be blown over. This
will p r o b a b l y bo about noon, the operation taking
place preferably through the hollow shaft b y means
of 40 or 50 lb. per square inch residual pressure.
As soon as the old batch is out of the pan, the
water and caustic for the new one are charged,
or the melted c a u s t i c is b l o w n in, as t h e case m a y
be, and a fire started under the pan. Charging
of t h e s u l p h o n i c a c i d is n o w b e g u n , w h i c h operation
m a y h a v e to b e done carefully to avoid " scotching "
of the agitator, and this will certainly take the
remainder of the day. The fire is s o maintained
that the temperature is rising all t h e time, ending

at 125° C. by from 4 to 7 p.m. The manhole-lid
is now fixed, and the heating u p to the desired
temperature started. This must not be done too
quickly; but, without forcing the firing, the batch
should be on temperature between midnight and
3 a.m. If the time of heating on temperature is
up to four hours we m a y expect the fire to be
drawn not later than 6 or 7 a.m., which brings us
round the cycle to another day's routine.
This means very hard work all r o u n d and allows

no latitude for the inevitable breakdowns, but it
serves to show what can be got out of a p a n if
m a x i m u m production is essential. A m u c h more
comfortable arrangement would be to have two
pans working on alternate days, in which case the
programme would be as follows :—
Starting with two e m p t y pans.
Monday.—Charge caustic in No. 1 p a n and

get this melted as quickly as possible. Charge
material hi the afternoon and have the p a n
sealed b y 5 p.m. H e a t u p and get " on
temperature " by M o n d a y night. Also charge
caustic in N o . 2 p a n on M o n d a y night a n d have
this slowly melted during the night.
Tuesday.—Blow over batch from No. 1 p a n

when ready, and re-charge this p a n with
caustic for slow melting on Tuesday night.
Make batch in N o . 2 p a n during the day, as
the caustic would be ready melted the first
thing in the morning.
Wednesday,—Blow over the batch from

No. 2 pan and recharge with caustic for
melting on Wednesday night. Make batch in
No. 1 pan.
Thursday.—The same as Tuesday.

Friday.—The same as Wednesday.
This plan, of course, only means one batch per

alternate day per pan, but it has the advantage
of givmg much more time for the processes, while
i t is q u i t e p o s s i b l e t o k e e p t o t h i s p r o g r a m m e even
if t h e t i m e of heating on temperature is a s l o n g as
twelve hours. Since we started with empty pans,
M o n d a y w a s r a t h e r a r u s h e d d a y , b u t e v e n if N o . 1
p a n w a s n o t sealed until late a t n i g h t it w o u l d not
matter, as that pan was not required for actual
manufacture a g a i n till Wednesday.
This should serve to show h o w autoclaves could

be worked, but, of course, each chemist must be
prepared to plan his programme to suit his own
special needs. M a y b e in some cases a modification
of t h e above schemes could be employed, in which
three batches were made in two pans in two days,
but this would not be so good, as the times for
definite operations would change from day to day.
The best programmes, and those which suit the
workmen most, are those in which each m a n can
h a v e his own definite job to carry out each d a y at
roughly the same time.
W h e n dealing with the routine running of larger

numbers of autoclaves, say six or ten, so much
a g a i n d e p e n d s o n t h e p r o c e s s e s t h a t it is difficult to
lay down any general principles likely to be of
help. A t the same time there are certain rules

w h i c h h a v e r e c e i v e d t h e s a n c t i o n of e x p e r i e n c e and
which it will be, therefore, advisable for a chemist
to follow in most cases. I n the first place, it is
often a good plan to group the pans in pairs and
so arrange the work that batches are m a d e in
Nos. 1, 3 , 5 , p a n s on o n e d a y a n d in N o s . 2, 4, a n d
6 on the day following. Again, although the pipe
fitting o f t h e s h e d w i l l b e s u c h a s t o f a l l in with this
system of groups, it should, even at the risk of
becoming intricate^ be such that the chemist in
charge can blow, not only from any autoclave to
any vat, but also from one autoclave to another.
The works chemist should always remember that
breakdowns seldom occur at convenient times, but,
generally speaking, machinery most often gives
under full load. It is o n l y natural that it should
be so, and the really good works chemist is the
one w h o h a s provided, n o t only for s m o o t h running,
b u t also for e v e r y conceivable disaster. The author
remembers a case in which a bad leak developed
in the riveting of the dish of a large autoclave
to the body just as the batch was coming u p to
temperature a n d pressure. The mixture was being
f o r c e d o u t of t h e p a n a n d d r o p p i n g i n t o t h e furnace.
It was a large a n d valuable batch, b u t in less than
ten minutes a few union joints h a d been made, a
few taps opened and shut, and the batch was blown
by means of its own pressure through the hollow
agitator shaft into an adjacent autoclave, the total
loss b e i n g less t h a n 2 % . This was an instance of
foresight a n d good management.
This brings us to another point—whenever

working with a large n u m b e r of pans it is always
wise to " carry a spare." This does not m e a n that
o n e p a n m u s t r e m a i n i d l e f o r m o s t of t h e t i m e o n the
oif chance of an accident occurring, but simply
that the whole plant is not being worked to the
a b s o l u t e l i m i t of i t s p r o d u c t i v e c a p a c i t y . All sorts
of s e t - b a c k s are liable t o occur, and even the best
of t i m e - t a b l e s c a n n o t b e r i g i d l y followed. If there
is some latitude allowed there will be a balance
a b o u t the whole installation which will b e reflected
j n t h e r e g u l a r i t y of t h e m o n t h l y p r o d u c t i o n returns.
Perhaps a batch m a y be started in N o . 2 pan, but
owing to a blockage in the pipes it cannot be
cleared ready for the correct time. If t h e r e is no
spare autoclave, then either a batch must be
3
" dropped/ i.e., n o t m a d e on that day, or it will
be started late, which will m e a n disorganisation
and hurry, bringing as its inevitable result a
mysterious drop in yield. There is n o doubt that
the regularity of production and yield from an
installation which. " carries a spare " more than
compensates for the capital which on the face of
it is standing idle for some part of the week-
While dealing with the question of spare parts of
an autoclave plant, it should be noted that the
remarks made are particularly applicable to the
wooden vats into which the charge from the pan
is s o often blown. The l i f e of these vats is never
very long where corrosive liquids are employed,
and as they are comparatively inexpensive a
reasonable excess over actual requirements should
be provided if r e g u l a r i t y of production is desired.

H e r e again the chemist should r e m e m b e r -that a vat
will often develop a bad leak w h e n empty, which
will b e c o m e apparent just as his batch has blown
over, and, therefore, arrangements should be m a d e
for passing the contents from one vat to another.
This can be done either b y some form of ejector
worked b y steam or b y having an arrangement
whereby a n y vat can be emptied into a storage
boiler a n d the batch blown u p again into a n y
other vat.
T h e output of a large n u m b e r of autoclaves

depends on a great n u m b e r of factors, not the
least of which is the general design of the shed.
M u c h time can be s a v e d if t h e staging built round
the autoclaves is of liberal size to accommodate
the materials for the batches, a n d is adequately
served with hoists to enable both m e n a n d material
to reach the pans b y the most direct routes. Again,
there should be plenty of space round the pans,
so t h a t all v a l v e s — s a f e t y , blow-off a n d blow-over—
are easy of access. A m a n crouching in a corner
at the b a c k of an autoclave on a narrow stage
against a wall would be caught ill a veritable
death-trap if t h e ring of t h e manhole-lid blew out
under pressure.
In conclusion, mention m u s t be m a d e of the

r o u t i n e t e s t i n g of a u t o c l a v e s in order to ensure the
safety of the m e n employed in working them.
T h i s is a very important part of a works chemist's
duties, for neglect of his pans not only causes
rapid deterioration, but thereby incurs the possi-
b i l i t y of e x p l o s i o n , w h i c h m i g h t entail the destruc-

t i o n of a n e n t i r e s h e d a n d l o s s of life.
As has been stated previously, a wise chemist
will always take any opportunity that arises of
boiling out his p a n s with water or weak soda ash
solution in order to prevent the formation of
c r u s t s of b u r n t matter on the sides a n d bottom.
Some regular plan should be adopted for the

cleaning out and examination of a u t o c l a v e s , a n d a
record of the result of these examinations entered
in the log book. This examination of a n informal
nature can be undertaken by the m e n working the
plant; in fact, a charge hand w h o is k e e n on his
job and fond of his pans will welcome it. The
m o m e n t anything o u t of t h e o r d i n a r y — a n indenta-
tion or signs of s p l i t t i n g i n t h e r i v e t i n g o f t h e dish
to the body of the pan—is observed, then the
plant should be handed over to the engineers for
skilled investigation.
Whenever any m a n is about to enter a pan

through the manhole there are certain rules which
should be carefully followed :—
(1) T h e p a n m u s t h a v e been boiled out until

absolutely free from dangerous chemicals.
(2) The pan must be reasonably cool,
(3) The compressed air m u s t have been

blown through the pan for some time, and it
m u s t b e p r o v e d t h a t t h e air inside will support
combustion, i.e., of a c a n d l e flame.
(4) The belt operating the stirring gear must
have been cut off.
This last is of extreme importance. It is not

enough to slip the belt on to the loose pulley, or
to stop the motor driving the shafting. Someone
m a y c o m e along ignorant of there being a m a n
inside the p a n and thoughtlessly start the agitator.
I t is far better to insist on the lacing of the belt
being cut before a m a n is a l l o w e d i n s i d e a n agitator
pan. A n o t h e r g o o d p l a n is t o insist o n m e n engaged
o n w o r k i n g inside a u t o c l a v e s , w h e t h e r for examina-
tion" or actual repairing, always being in pairs.
After all, n o matter h o w one tries to m a k e it safe
a n d easy, working in an autoclave is b o u n d to be
a cramped, hot, a n d trying job. E v e n a strong
m a n m a y suddenly become faint, so that as a
reasonable precaution he should have a m a t e
s t a n d i n g b y i n c a s e of need.
E v e r y few months, whether there appears to be

anything wrong with the p a n or not, it should be
tested a n d examined b y the maintenance engineers.
T h e testing for pressure will consist of subjecting
the p a n just as it stands, with all valves, gauge,
a n d agitator, to hydraulic pressure. This is done
b y p u m p i n g water into the pan through any suit-
able opening—say a v a l v e provided for t h e purpose
on the pipe to the blow-off or pressure gauge—
until a definite desired pressure is indicated on the
gauge. Often the p u m p used will have its own
gauge, so that this constitutes a test for the
pressure gauge as well as for the autoclave itself.
This- o p e r a t i o n is p e r f e c t l y s a f e , f o r if t h e manhole-
lid ring-or any other part gives before the desired
p r e s s u r e is r e a c h e d it o n l y m e a n s a t w o r s t a shower-
bath for the operator and some amusement for

the onlookers.
As regards the pressure to which pans should be

subjected in this test, there is some difference of
opinion. The author firmly believes that an
autoclave should be hydraulically tested up to the
full figure given b y its m a k e r s , but only worked to
half that pressure. Thus if a pan is supposed to
stand 300 lb. to the square inch it should always be
tested up to that limit b y this hydraulic method,
b u t no process evolving a gas pressure a b o v e 150 lb.
to the square inch should be worked in it. After
all, h y d r a u l i c t e s t i n g cold is n o t n e a r l y so searching
as the pressure from steam or ammonia or ethyl
chloride vapour at a high temperature, and the
s y s t e m of w o r k i n g a t h a l f t h e t e s t e d p r e s s u r e allows
a reasonable margin of safety.
I n a d d i t i o n t o t h e t e s t i n g of a u t o c l a v e s instituted
b y the works chemist, most pans are periodically
e x a m i n e d b y b o i l e r i n s p e c t o r s o r , if i n s u r e d , b y the
offi.cj.als of t h e company with w h o m the policy has
been taken out.

Autoclaves and High Pressure Work

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A U T O C L A V E S A N D

Second Scries Price 6s. net each.

Richard Clay & Sons, Ltd., Printers, Bungay y Suffolk

T H E aim of t h i s little book is d e s i g n e d to meet

The scope of the book is fully dealt with in

THE CONSTRUCTION AND USE OF W O R K S AUTO-

THE HIGH PRESSURE WORKS AUTOCLAVE . 103

THE HEATING OF WORKS AUTOCLAVES . . 1 1 5

THE WORKING OP LARGE-SCALE AUTOCLAVES . 131

3. Large agitator laboratory autoclave 35

R E G A R D E D in a general way, an autoclave is a

I n order to render this work of the greatest

I t is, therefore, because of this outlook that

very little knowledge of autoclave working is

N e x t some space will be devoted to apparatus

(1) The high pressure agitator autoclave, and

(2) The low pressure agitator autoclave of

Separate chapters will b e given to each of these

The next section will he devoted to the diffi-

I n conclusion, a chapter will be given to the

Autoclaves can be made of cast iron, steel,

Autoclaves are made over a very large range

regards capacity, temperature of heating, and

Showing the General 'Limits of Various Types of

Laboratory non-agitator 300 to 1000

Laboratory agitator 1000 to 300

Large-scale autoclave, 20O t o 400 300Q C. 100

Large-scale autoclave, 700 200° C. 10

Large-scale autoclave, 400 300° C. 40

A u t o c l a v e s are generally cylindrical in shape,

M a n y different materials are used for packing

generally tapped with screw threads for particular

It was at one time the custom to provide two

Again, it was common at one time to fix one or

v e r y necessary that the stuffing-box be of ample

I t should be observed that these are the only

B e f o r e concluding these general remarks, some

liner and the autoclave walls the transference of

p i p e is m a d e wide and often looped to form a trap

T H E laboratory autoclave, as the n a m e implies,

Manufacturers of laboratory autoclaves put on

The following pieces of apparatus will therefore

(1) Small non-agitator autoclaves.

(6) A u t o c l a v e s designed for special purposes.

Type No. 1.—The small non-agitator autoclave

sizes, but the most common is about 600 c.c,

Generally spjeaking, the ordinary limits of

This type of a u t o c l a v e can be heated, either by

If an oil-bath is used it should be a properly

For oil-bath work, however, the most satis-

Type No. 2.—This class m a y be said to embrace

Pig. 2 shows the arrangement of t h e top of the

to tighten u p after heating has commenced b y

I n m a n y of the first-class models all rotatory

These autoclaves can be heated b y direct flame,

Type No. 3.—The large-size agitator autoclave

reasonable quantity of material for subsequent

The general construction of this type of auto-

I t will b e seen t h a t a c o m m o n pipe serves as the

The diagram shows an autoclave standing in a

FIG. 3.—Large Agitator Laboratory Autoclave.

baffle under the flue fitted to the back of the

them when it is desired to stop the experiment,

Tupe No. 5.—It has been shown that the limits