c







 
By - 05/25/2006
in



To separate the binary mixture by simple distillation using fractionating column

 
    



is a j
 

in which compounds with different boiling points
can be separated by controlled heating. Vapors from a sufficiently heated sample can
be recondensed and collected, purer than the initial mixture.The liquid which has not
vaporized is called the 
  , and the liquid which is collected in the receiver is called
the 

 .
Since not all chemicals distill the same way, there are several distillation techniques can
be preferred depending on the nature of constituents to be purified or to be separated.
These include
 



 



 


 

 

 .
A
 

  ! is for purifying liquids of one component (separating
nonvolatile liquid impurity or to purify a liquid from solid contaminants), multiple liquids
where the differences in boiling points is very large (a low boiling liquid from a high
boiling liquid)(b.p difference around 50 -70°C). Simple distillations are not effective in
removing multiple solvents from one another with a high degre e of success.
In 

 

 "! a fractionating column is inserted between the
distillation flask and the distillation head. The fractionating column provides a large
surface area in which the mixture can be continuously vaporized and condensed.
The principle of a fractionating column is that, as the vapours ascend the column from
the boiling mixture below, the high boiling components are condensed and returned to
the flask, the ascending column of vapour being thus steadily ³scrubbed´ by the
descending column of liquid condensate. The ascending column of the vapour becomes
therefore steadily richer in the lowest boiling component, and the descending column of
condensate steadily richer in the highest boiling component.
Figure 1 represents the typical curve for simple and fractional distillation. In an ideal
fractional distillation, two distinct fractions are obtained. The first corresponds to the
component with the lower boiling point and the second to the high -boiling point
component. What characterizes a good fractional distillation is the sudden increase in
temperature between both fractions, or in other words, a very small volume distilled at
temperatures other than the boiling points of the pure liquids. In simple distillation, a
much more gradual increase in temperature is observed, reflecting the impure nature of
the distillate
c #$%
 

 

 

%
 

 is used for separating mixtures of chemicals such as oils, resins,
hydrocarbons, etc. which are insoluble in water and may decompose at their B.P.
&
 

 is used for separating liquids boiling above 200ƕC
c



'



The set-up for fractional distillation is shown in Figure 3. It consists of a round -bottomed
distillation flask where the liquid is placed, a fractionalting column, a distillation head that
connects the distillation flask to the condenser; and a distillation adaptor that connects
the condenser to the receiving flask. The condenser is a tube surrounded by a water
jacket to cool and condense vapors. The distillation head holds a thermometer to allow
the temperature of the vapors to be monitored during the distillation.

c  % 


 (
   )

Assemble the apparatus as shown in Figure 3, use graduated cylinder to collect the
distillate. Place the liquid (25 mL of cyclohexane (b.p.80.7°C) and 25 mL of
toluene(b.p.111°C) or 25 mL of benzene (b.p.80°C)or 25 mL of of toluene) to be distilled
into the distillation flaskPla ce a boiling chip in the distillation flask to ensure smooth
bubbling and prevent bumping of the liquid up into the distillation head. Heat the liquids
and distil slowly, so that the total distillation occupies about 1 hour and 30 minutes. As
the liquid boils, vapors rise into fractionating column and to the distillation head and
condensed liquid will be seen dripping from the thermometer bulb. Eventually the vapors
enter the side arm of the distillation head and continue into the condenser. Once in the
condenser the vapors are cooled due to the water circulating in the outer jacket; the
vapors condense back to a liquid that runs down the condenser and is collected in the
receiving flask. Increase the heating rate near the midpoint of the distillation otherw ise
the head temperature will drop.
Take temperature readings at the first drop and at each 2 ml increment. Continue until
you have distilled 48 ml(collect the fractions having boiling points (a) 80 ²85°, (b) 85-
107° (c) 107-111°, these fractions should hav e the volumes about 23, 2, 23 mL
respectively). Construct a table in your notebook as given below, to record the
temperature at the distillation "head" as a function of volume distilled.
Volume distilled (mL) 2 4 6 8 10 12 14 16 18
20
Temperature without column

Temperature with column

Make a plot of Temperature (ºC) Vs. volume of distillate Co llected (ml) and determine
the b.p of each of these solvents.
Õ


ÿ. t i i l l t t t i ,
t f t ili i t ill l l t t . i lit t .
.N i till fl t l i i t t f
t t t l fl t i .
.U l ili t t t i ,t ti i f li i t t
l t ft fl i i l i till ti i
f ti l i till ti .A ili t i ll i f l l.
*+,

-  


 




At l

t t t i   f   ti
t
j
t  ff t  f Õ
  . . . t i .  B t  t 
 j it    ? If      l t il t t   ti  i   i t i  t i ,  l   t  it
    i  f l !A" G #DS? I i  t   i iliti! $  t fl  l 't  t t  i 
t 
    l t  ? A  i  f %% f  it   i  t & t     i i  ? A
 
it , ' ti i  iliti t  t ' i  t i  t   t   f tt   t t   (
  
 f l t i    t t  t  i  t i     l   l li   i ?
            
N  t l t  i t ti i   i t i  t i .*
 "               
 i  t i l t   t l t  i
  
it  f  t   
   t   i till ti . "   itill li' i  ill  &t  t  it      i
 l  t )tl   *, fi  , t       t t  i  t  fi  l   t.

N
 I    t  '  t i i  : i it  f f   t t           t  t &t  t f
 t i ? + ll ! $ it i   . A  '  ll   l  l . P    t l t    
t  i   t &t  i l. I  f t,  t i   il  t t i   il l f    t i l t  i
 till j t   t l t  ,   it i  i l  i    t i i i  . ,   t il l t .

÷
-. . . . 3 34 t- 2. 5 ill 2- t . 23 6l. 7- 0 t- 4 1.3t. 3 43 t 3 187.
N t : /01 2 / t l

V
„
 -„  „ „
 „

 V
If
9: ;'<= t> ?= @ > @9 A B= CiDt E9 l> F: E> t: E9 A l>DD=D , : E if 9: ; B><= > F>A ?G E: ;@H i @ C:: @D Bi @=
H H
IE: ;A ti: @, t B= @ 9: ; ?@:J > t Bi @G : E tJ: > F: ;t iDtill> ti: @. K=> t D: C=t Bi @G ;I t: F: ili @G , t B= @
A: ll=A t t B= <> I: ED F9 A: @ = @D i @G t B= C i @t: > @:t B= E A: @t> i @= E. St=> C HiDtill> ti: @ iD t B= D> C=
H
H M H H
IEi @A i I> l > @ ;D=D t B= D> C= =L ;i IC= @t. B= : @l9 iff= E= @A= iD t B> t 9: ; iDtill D: C= t Bi @G i @ t B=
IE=D= @A= :f J> t= E. St=> C D= E<=D t: <:l> tiliN= A= Et> i @ A B= CiA>lD, D ;A B t B> t t B=9 A:O F: il Jit B t B=
J>t= E > @H A> @ F= A: ll=A t=H > l: @G J it B tB= Dt=> C J B= @ it A: @H= @D=D .

M D D > A > 9 D= : =P >A G > H H

Bi i I Eti ;l El ; f ;l f E t E ti @ Il @t C>tt= E, J B= E= t B= Dt=> C D= E<=D : ;Fl= ;t9,
H H H
FE=> ?i @G : I= @ A=ll J> llD > @ E= l=>D i @G <: l> til= : ilD li ?= @= I= t>l>A t: @= . A Dt> @ > E > II> E> t ;D t B> t
9: ; J: ;lH ;D= i @ > A B= CiDt E9 l> F iD D B:J @ i @ t B= fi EDt IiA t ;E= F=l:J. Qf A: ;ED= , J= 'll F= H:i @G t BiD
> t B: C= J it B: ;t >AA=DD t: f> @A9 DA i= @A= G>HG= tD.

H H H
R: E t BiD A> t @i I =Pt E>A ti: @, I'<= A: @Dt E;A t= > C;A B D i CIlifi= > II> E> t ;D D B:J @ i @ t B= D=A: @
A = M = A> > H J> = G:=D = : : : > G : J > A >A= H: : M = H D
Ii t ;E . B t @i I @ t E i @ t B F t C f Fi I t, it B ;I Il @ t I. B li i
H H H
E=>ll9 t B= ?=9 A: CI: @= @t B= E= ; F9 Di CIl9 t ;E@i @G t B= li :f t B= I: t ;ID i = :J @, t B= <> I: ED Jill
A: @H= @D= > @H H Ei I H:J @ f E: C t B= A= @t= E, A:ll=A ti @G i @ t B= A ;I F=l:J. B9 filli @G t B= t: I : f t B= liH
Jit B iA= J> t= E, t B= <> I: ED > E= A: @H= @D=H <= E9 =ffiA i= @tl9.

V
 O


  
  







 




   
  

O
 



 
 

  
 
O


  

 




ÿ  ½
 O

   V
 Π
O

   V




 

 O
   

 
  

    
 

O    
   

 
 
 


 
        


 
 
     

    „


 





ÿ  Œ

V ÿ
V

V 
  !

   
 
  "#$%& 


 

'"(  V
 Õ
 

 V
  

 

)#%& 
 

O

  


  
 V
 Œ

V
V½  V
 !

 
 
"#$%&
"  V
 Õ
 

 V
  

   
   
 )#%& 
  
 
  O

  





 V
  Œ

V 
V   V 
   !

  *
  
 


  
  
 
)#%& 
  
" V
  Œ

V 
V
 V 
   
   
 
 
 
   
| „
     
|





  „ 
    
 
 
 O

 
 
 
 


'+ 
*
 



  

 
 



( V




 

 
 
     

    "#$$$$"%& 
,
 
    
    
   
 
 
*
     
  
 -

 
    


    

  ,
 



VV

Œ
 

 

Vacuum distillation in the petroleum industry has not up to the present received the
attention it deserves. Plants for the distillation of lubricating oils are often operated under
vacuum, but this is seldom sufficiently high to give the best results, in many cases,
indeed, being so low as to have little marked effect on the distillation. The advantages of
distilling under vacuum are: -The fractions are distilled off at relatively lower
temperatures, cracking or decomposition being thus largely avoided. The distillates
obtained are of better colour and of higher flash -point; the residues are also of better
quality, as they have not been cracked and so contain little or no free carbon. From wax
base oils, for example, a better yield, not .only of the heavier lubricating oils but also of
the higher grade waxes, may be obtained. ood distillates suitable for concentrating to
cylinder oils may thus be obtained. The difference in character between wax and asphalt
oils, as far as yield of lubricating oils is concerned, largely disappears under high
vacuum distillation.1 Vacuum distillation plants are naturally more costly as regards
capital outlay and operating wages. This is, however, counterbalanced by the fact that
the products obtained are of better quality and require less subsequent chemical
treatment. The system finds application, in the petroleum industry, chiefly for the
manufacture of lubricating oils ; but there is no reason why it should not be applied to
other operations as well, the treatment of which lies outside the scope of this work.

Vacuum distillation may be applied either to periodic or continuous distillation. The

simpler forms of plant consist of a still of the ordinary type, structurally strengthened to
withstand the external pressure, with dephlegmators, coolers, and receiving boxes, all
under vacuum. The system is connected to the top of a barometric condenser and
exhausted to the required vacuum by an air pump. Many forms of plant, differing in detail
but similar in principle, have been devised, e.g. that of Henderson, designed as far back
as 1883 (Eng. Pat. 5401 of 1883 and 17332 of 1889), those of Lennard (Eng. Pat. 944 of
1892) (applied in the coal -tar industry), of Zaloziecki, Palmer, Wanklyn and Cooper (Eng.
Pat. 4097 of 1893) and others, all of which operate at relatively low vacuums. Fig. 150
illustrates the main features of a simple vacuum pla nt.

1 L. Singer, Petroleum, Berlin, 10, 605. 352

The still is of the ordinary type, internally strengthened to withstand t he external

pressure. It is fitted with perforated pipes in the usual way, as the distillation is invariably
conducted with the aid of steam.

The vapour pipe, which is always of large diameter, is connected to several domes on
the still. It leads to dephle gmators, or atmospheric condensers, where the heavier
fractions are condensed. The first air -cooled condenser often takes the form of a number
of large diameter horizontal pipes. The condensate from these air coolers flows through
a cooler into a receiving tank connected to the air pump. The receiving tanks are in
duplicate, so that that which receives the distillate can always be kept under vacuum,
while the other is being pumped out. Several air -cooled condensers may be employed,
and also water-cooled condensers, the condensates from which run off through coolers
to receiving tanks under vacuum. The vapours containing the lightest fractions and the
steam are finally condensed in a spray condenser, elevated and connected with a water
pipe terminating in a w ater seal below, of such a height that it functions as a barometer
tube, the vacuum in this barometric condenser being maintained by an air pump.
An apparatus designed for working at high vacuum is that of Steinschneider ( .S. Pat.
981953 of 1911). One of the chief objections to the previously described schemes is that
the receivers for the distillates are under vacuum, an inconvenient arrangement, as they
are not under complete observation and control. Further, if evacuation takes place via
the distillate receiver, the lighter vapours are retained in contact with the distillates,
whereas they should be removed as quickly as possible. This could be avoided by
placing each receiver tank at the bottom of an oil barometer, but this would necessitate
either building the plant very high, or else much excavating, both of which are
expensive. Steinschneider avoids t hese difficulties in the following way (Fig. 151). The
distillate vapours pass from the still s through dephlegmators or air condensers d to the
cooler c and on to the elevated barometric condenser b. The distillates condensed in the
dephlegmators d flow a way through the coolers e to the receivers r, which may be fitted
with floats for regulating the level of the liquid contained in them.
 i . ÿ
. Si l i till ti l t.

f ti ll t i t i t l l l ,
f ti i it ,i t t i ti ti t. l
t ft l t i t tt t f ti l
t i f.

i t l t i till ti t i t i it t it
i t t i t ft i i t t
.B l i t , it i i l t t f ll f t i
i G t tt l f li i i t i i i t l t t i t
i t i i l t i t i ti .

l t t i l i i till ti t t i tilli
ff f t l til f ti f t l , t t t t i t
i till t ff l t t t i
l i t t i t li t .

i . ÿ ÿ. St i i ' i till ti l t.
I t i ti f i i till ti ti t i
t t f l . Di till ti t i t t i
i t i i l i l i t t f t i f
t l .B t ti l iti ft i i t t
l l li t f ti i t i .S iti i , t
iti , i i l i t t f ti f
l , t lit f t i i l i i i t t
f ti f .E i f ti i , i , ft i f f
t .S t f ti i f t ti
f t l til f ti f t l i till t , i ll f t t l
ft i ff t t ll , t l t i till t
f t l i ff t t i t t . l til
f ti l l f l i i t U it St t
l , i ll t i li . I l f i
l t , ti l t , i il t l ti l i ili i till t
i t, f tl l .D B t B t f P t l ij.
i E . P t. ÿ  f ÿÿ t t l tf t i till ti
tifi ti f l til li i . i i f i
, , li t i t ft i l .

Distillation
From Wikipedia, the free encyclopedia

ë

ë
ë

ë

  





 







 

 


 



 
V
 tiST l iStill ti ÿ 
 ti iU
tillt till  tili it
t tu  li  ti li  tut itill tii l   uu 
iltÿ tilliÿÿ  ttlÿ
titlÿ ti tl tÿ  ti il 

tÿ tii   ! ti-
ui   ul i ltiÿ li 
t "#$ 

  i t  ti ixtu
iitil tilitii 
ili 
liquiixtu itill tii uit ti! i l  ti! t i l
 ti 

i ll!itill ti  u
 li ti %tiut  tuilit
 tiiiuu t t!  ti  ti & tiitillt
iuiti!u  lt  t 
iiitillt  titt'
t
lx !it !   'iuti lu itill titluti 

ui ittituitill
 it i  lltt i
itill tii iut!i llitill ti ll!     
 Œ



V
V

ÿV
V
iV  V V V
ºVV V V
Y º ÿV
V V
Y º iV  V V
Y º ºV
V
V
6V

VV V
Y 6 ÿV V V
Y 6 iV
 V V
Y 6 ºVV V
Y 6 6VV V
Y 6
V
VV V
Y 6 V

V 
V V
Y 6 V!

V V

V 
V V
Y
ÿV
"#VV 
V$
V
 V

V  V
Y
iV%

 $#V V
V
V V
V& VV V
#V
Y  ÿV&V
#V
mV
V
åV' V
ÿV


V
#V
ÿÿV()
V"V


istory

Distillation apparatV s of ZosimV s, from Marcelin erthelot, Œ
 

 
 

(3 vol., Paris,
1887 W1888).

The first clear evidence of distillation comes from Greek alchemists working in AleX andria in the first
centYry AD[2]. Distilled water has been known since at least ca. 200 AD, when AleXander of
Aphrodisias described the process.[3] Arabs learned the process from the Egyptians and Y sed it
eXtensively in their alchemical eX periments.

The first clear evidence from the distillation of alcohol comes from the School of Salerno in the 12th
centYry.[2][4] Fractional distillation was developed by Tadeo Alderotti in the 13th centYry.[5]

In 1500, German alchemist ieronymY s raY nschweig pYblished 






(The ook
of the Art of Distillation)[6] the first book solely dedicated to the sY bject of distillation, followed in
1512 by a mY ch eXpanded version. In 1651, John French pYblished The Art of Distillation the first
major English compendiY m of practice, thoYgh it has been claimed[7] that mY ch of it derives from
raY nschweig's work. This inclY des diagrams with people in them showing the indY strial rather than
bench scale of the operation.

A retort.
Distillation

Old Ukrainian vodka still

As alchemy evolved into the science of chemistry, vessels called retorts became Zsed for distillations.
oth alembics and retorts are forms ofglassware with long necks pointing to the side at a downward
angle which acted as air[ cooled condensers to condense the distillate and let it drip downward for
collection. Later, copper alembics were invented. Riveted joints were often kept tight by Z sing varioZs
mi\tZres, for instance a doZ gh made of rye floZ r.[8] These alembics often featZred a cooling system
aroZ nd the beak, Zsing cold water for instance, which made the condensation of alcohol more
efficient. These were called pot stills. Today, the retorts and pot stills have been largely sZpplanted by
more efficient distillation methods in most indZstrial processes. owever, the pot still is still widely
Zsed for the elaboration of some fine alcohols sZ ch as cognac, Scotch whisky,te]Zila and
some vodkas. Pot stills made of varioZs materials (wood, clay, stainless steel) are also Z sed
by bootleggers in varioZs coZ ntries. Small pot stills are also sold for the domestic prodZ ction[9] of
flower water or essential oils.

Early forms of distillation were batch processes Zsing one vaporization and one condensation. PZ rity
was improved by fZ rther distillation of the condensate. Greater volZ mes were processed by simply
repeating the distillation. hemists were reported to carry oZ t as many as 500 to 600 distillations in
order to obtain a pZre compoZnd[10].

In the early 19th centZ ry the basics of modern techni]Z es inclZ ding pre[ heating and reflZ\ were
developed, particZlarly by the French[10], then in 1830 a ritish Patent was issZ ed to Aeneas
offey for a whiskey distillation colZ mn[11], which worked continZ oZ sly and may be regarded as
thearchetype of modern petrochemical Znits. In 1877, Ernest Solvay was granted a U.S. Patent for a
t lu i itill ti"#($ t  u
qut  ltti
til iit 

&itt i l ii   iili ttt#)ttu!itii
 tt ii ltul
 li li tluiutit l(*t
tuititutlt u ti tu tM
-
ilt t+qu ti   il
ilitulut  l ll
itutiul tiitill tilu 

li tiitill ti

 li tiitill ti u l
iiiu u l
 t l!iuti l
itill ti!itill ti
u ii l
litill t! i 
l ttt ititilitttit titi 
 !
titill tiitu  tuuii tit
uttt  lll tilt
u ti lttitill t 

 ii
tl
 t litill ti iuti litill tiit tl
 t
 litill tiit
t-i! iuti litill titu
tiuul %
titill ti!tititu ti l!t titilli 
u titill t  ui titill ti %
titill ti! tilli  
uliit 
tixtu!iit  tititt tii
lltquti lltl tiltll til!itt
tt ii l t-
l til ti tt till t
   t t 

%tiuuitill ti!tu ti l! ! itill t t t t t

iti
 ulllii tu ti l i  ti
t  
liquiitt iulti 
tttlt  ti 

% li itill til

ili it liquiitt tu tit utliquiqu lt
uitliqui!
li 
u

ltitut
i u 
i l it l

ili it!t utliquiqu lt 
it tiu 

%ti itit ti liquiixtu t  iu! t
il tt

ili iti tt iu t  tillllt
  tl ul i!!tui i li^ t % li^ l
itill ti ti ll 
R ult _l   lt,l !  ut t -liqui
quili
i   tt i 

R ult,l  ut t tti
uttttt l utixtui
tititt tixtu it uu!uitl  ti l
uqu ll tiultili
 uu %t  
another component's vapor press`re, or if the volatility of a component is dependent on its percentage
in the mia t` re, the law will fail.

Dalton's law states that the total vapor press`re is the s` m of the vapor press`res of each individ` al
component in the miat` re. When a m`ltib component lic` id is heated, the vapor press`re of each
component will rise, th`s ca`sing the total vapor press` re to rise. When the total vapor press` re
reaches the press` re s`rro`nding the lic`id, boiling occ` rs and lic`id t` rns to gas thro` gho`t the b` lk
of the lic`id. Note that a miat` re with a given composition has one boiling point at a given press` re,
when the components are m`t`ally sol` ble.

An implication of one boiling point is that lighter components never cleanly "boil first". At boiling
point, all volatile components boil, b`t for a component, its percentage in the vapor is the same as its
percentage of the total vapor press` re. Lighter components have a higher partial press` re and th`s are
concentrated in the vapor, b`t heavier volatile components also have a (smaller) partial press` re and
necessarily evaporate also, albeit being less concentrated in the vapor. Indeed, batch distillation and
fractionation s` cceed by varying the composition of the miat` re. In batch distillation, the batch
evaporates, which changes its composition; in fractionation, lic`id higher in the fractionation col` mn
contains more lights and boils at lower temperat`res.

The idealized model is acc` rate in the case of chemically similar lic`ids, s` ch as benzene and tol` ene.
In other cases, severe deviations from Rao` lt's law and Dalton's law are observed, most famo`sly in
the miat` re of ethanol and water. These compo` nds, when heated together, form an azeotrope, which
is a composition with a boiling point higher or lower than the boiling point of each separate lic`id.
Virt`ally all lic`ids, when mia ed and heated, will display azeotropic behavio`r. Altho` gh there
are comp`tational methods that can be `sed to estimate the behavior of a mia t`re of arbitrary
components, the only way to obtain acc` rate vaporblic` id ec`ilibri` m data is by meas` rement.

It is not possible to  p`rify a miat` re of components by distillation, as this wo`ld rec`ire
each component in the miat` re to have a zero partial press`re. If `ltra bp` re prod` cts are the goal, then
f`rther chemical separation m`st be applied. When a binary miat` re is evaporated and the other
component, e.g. a salt, has zero partial press` re for practical p`rposes, the process is simpler and is
called evaporation in engineering.

2


 
w

 



 
A batch still showing the separation of A and .

eating an ideal midte re of two volatile se bstances A and  (with A having the higher volatility, or
lower boiling point) in a batch distillation setep (se ch as in an apparate s depicted in the opening
fige re) e ntil the mid tere is boiling reselts in a vapor above the life id which contains a mid tere of A
and . The ratio between A and  in the vapor will be different from the ratio in the lifeid the ratio
in the life id will be determined by how the original mid tere was prepared, while the ratio in the vapor
will be enriched in the more volatile compoe nd, A (de e to Raoelt's Law, see above). The vapor goes
throe gh the condenser and is removed from the system. This in tern means that the ratio of
compoe nds in the remaining life id is now different from the initial ratio (i.e. more enriched in  than
the starting lifeid).

The rese lt is that the ratio in the lifeid midtere is changing, becoming richer in component . This
caeses the boiling point of the mid te re to rise, which in tern reselts in a rise in the temperatere in the
vapor, which reselts in a changing ratio of A  in the gas phase (as distillation contine es, there is an
increasing proportion of  in the gas phase). This rese lts in a slowly changing ratio A  in the
distillate.

If the difference in vapor pressere between the two components A and  is large (generally ed pressed
as the difference in boiling points), the midtere in the beginning of the distillation is highly enriched
in component A, and when component A has distilled off, the boiling life id is enriched in component
.

Œ


 



ontine oes distillation is an ongoing distillation in which a lifeid mid tere is contine oesly (withoe t
interre ption) fed into the process and separated fractions are removed contine oe sly as oetpe t streams
as time passes dering the operation. ontine oe s distillation prode ces at least two oe tpe t fractions,
incle ding at least one volatile distillate fraction, which has boiled and been separately capte red as a
vapor condensed to a lifeid. There is always a bottoms (or reside e) fraction, which is the least volatile
reside e that has not been separately captered as a condensed vapor.

ontine oes distillation differs from batch distillation in the respect that concentrations shoe ld not
change over time. ontine oe s distillation can be re n at a steady state for an arbitrary amoe nt of time.
For any soe rce material of specific composition, the main variables that affect the pe rity of prode cts
in contine oe s distillation are the refled ratio and the ne mber of theoretical efe ilibrie m stages
(practically, the ne mber of trays or the height of packing). Refled is a flow from the condenser back
to the cole mn, which generates a recycle that allows a better separation with a given ne mber of trays.
Efe ilibrie m stages are ideal steps where compositions achieve vaporg life id efeilibrie m, repeating the
separation process and allowing better separation given a refled ratio. A cole mn with a high refled
ratio may have fewer stages, bet it refled es a large amoe nt of life id, giving a wide cole mn with a
l  lu l! luit llux tiut  l  u
t !tu
quii  t lllu 

‰ 
t
t tiuuitill ti 
i
 i u  ti ti lu
ttitill til  lui  ti
ii  l  u   t
   ttitt t ilit i tquili
iu l  i
l 
lu it llu
t,t ,,i,i llt i i!

ili liquiixtu! llitti -liquiquili
iu 

 i
tl
 t- l iuti l- l ti ti lu!
utt
iil t  -x ll
 t- l ti ti luii i ii
ilu 

†
i
† i uxluuu lll
 t ll
†  lu it l 
 !t li!ti llit ti l
† ii 
itill tit 
V
 t litill ti
V
 t litill ti  ltxluilu 
titill ti iui
itill ti!tit  „
!it t iiu j iit
u ti li t! Êiit t uil
ttliquit t!
 Êiitt tuiiliqui! llt  !illt  l
l
 t ltiquitill tixit litill tit 

$  

%   ! lltt u ii tl lit t t
l t  !titill tillt
u-ititiill

iti lttitit  tt it tu u!  
ut
R ult,l  

 ult!ilitill tiiuu llult  tliqui
ili iti

 tlultu
i(./!"#0$t  tliquiil tilliil +t !
t utt uu lluiitlitt tR ult,l  

 ltuttii ii tti
utitll tilt %ti !t
itill t 
uiitluititu 

Ê   

+  !t
ili itttitixtuill
uiitllt t
R ult,l ut
t iti ti !Ê   ut
ui
to separate the components well by repeated vaporizationh condensation cycles within a packed
fractionating coli mn. This separation, by si ccessive distillations, is also referred to
as ‘ 
 

[14].

As the solition to be pirified is heated, its vapors rise to the fractionating coli mn. As it rises, it cools,
condensing on the condenser walls and the sirfaces of the packing material. ere, the condensate
contini es to be heated by the rising hot vapors; it vaporizes once more. owever, the composition of
the fresh vapors are determined once again by Raoilt's law. Each vaporizationh condensation cycle
(called a  
) will yield a pj rer solj tion of the more volatile component.[15] In reality,
each cycle at a given temperatj re does not occj r at ek actly the same position in the fractionating
colj mn;  
 is thj s a concept rather than an accj rate description.

More theoretical plates lead to better separations. A spinning band distillation system j ses a spinning
band of Teflon or metal to force the rising vapors into close contact with the descending condensate,
increasing the nj mber of theoretical plates.[16]

[edit]




w





 

Like vacll m distillation, 



is a method for distilling compol nds which are heatm
sensitive.[17] This process involves l sing blbbling steam throl gh a heated mintlre of the raw material.
y Raol lt's law, some of the target compol nd will vaporize (in accordance with its partial presslre).
The vapor min tl re is cooled and condensed, lsl ally yielding a layer of oil and a layer of water.

Steam distillation of variols aromatic herbs and flowers can resllt in two prodl cts; an essential oil as
well as a watery herbal distillate. The essential oils are often l sed in perfl mery
and aromatherapywhile the watery distillates have many applications in aromatherapy, food
processing and skin care.
Dimethyl so lfop ide o so ally boils at 189 /. Under a vacoo m, it distills off into the receiver at only 70 /.

q
‘


‘
 




 Stirrer baranti rbo mping grano les  Still pot  Fractionating colo mn
Thermometeroiling point
temperato re Teflon tap 1  old finger  ooling water oo t  ooling water in  Teflon tap 2 Vacoo mgas
inlet  Teflon tap 3  Still receiver

[edit] 



w





 

Some compos nds have very high boiling points. To boil ssch compos nds, it is often better to lower
the presss re at which ss ch compos nds are boiled instead of increasing the temperats re. Once the
presssre is lowered to the vapor presss re of the compos nd (at the given temperatsre), boiling and the
rest of the distillation process can commence. This technits e is referred to as a 


and
it is commonly fou nd in the laboratory in the form of therotary evaporator.

This technivu e is also very usefu l for compou nds which boil beyond their decomposition
temperatu re at atmospheric pressu re and which wou ld therefore be decomposed by any attempt to boil
them u nder atmospheric pressu re.

   ‘


is vacuu m distillation below the pressure of 0.01 torr.[18] 0.01 torr is one order
of magnitu de above high vacuu m, where fluids are in the free molecular flow regime, i.e. the mean
free path of molecules is comparable to the size of the evu ipment. The gaseou s phase no longer ew erts
significant pressure on the su bstance to be evaporated, and consevu ently, rate of evaporation no
longer depends on pressure. That is, because the continuu m assu mptions of fluid dynamics no longer
apply, mass transport is governed by molecx lar dynamics rather than flxid dynamics. Thx s, a short
path between the hot sxrface and the cold sxrface is necessary, typically by sxspending a hot plate
covered with a film of feed neyt to a cold plate with a clear line of sight in between. Molecxlar
distillation is xsed indxstrially for pxrification of oils.

[edit]‘

a a 




Some compox nds have high boiling points as well as being air sensitive. A simple vacxx m distillation
system as ey emplified above can be xsed, whereby the vacxx m is replaced with an inert gas after the
distillation is complete. owever, this is a less satisfactory system if one desires to collect fractions
x nder a redx ced pressxre. To do this a "pig" adaptor can be added to the end of the condenser, or for
better resxlts or for very air sensitive compoxnds a Perkin triangle apparatxs can be xsed.

The Perkin triangle, has means via a series of glass or Teflon taps to allows fractions to be isolated
from the rest of the still, withoxt the main body of the distillation being removed from either the
vacxx m or heat soxrce, and thxs can remain in a state of reflxy . To do this, the sample is first isolated
from the vacxx m by means of the taps, the vacxx m over the sample is then replaced with an inert gas
(sx ch as nitrogen or argon) and can then be stoppered and removed. A fresh collection vessel can then
be added to the system, evacx ated and linked back into the distillation system via the taps to collect a
second fraction, and so on, x ntil all fractions have been collected.

[edit] ‘






Short path vaczz m distillation apparatz s with vertical condenser (cold finger), to minimize the distillation
path;  Still pot with stirrer baranti {bz mping granz les  old finger { bent to direct condensate  ooling water
oz t
 cooling water in  Vaczz mgas inlet  Distillate flaskdistillate.

 ‘




is a distillation techni|x e that involves the distillate travelling a short distance,
often only a few centimeters, and is normally done at redx ced pressxre.[19] A classic ey ample wox ld
be a distillation involving the distillate travelling from one glass bx lb to another, withoxt the need for
a condenser separating the two chambers. This techni|x e is often xsed for compox nds which are
x nstable at high temperatxres or to px rify small amox nts of compox nd. The advantage is that the
 ti t tu 
i
ll tuut t
ili itt
liqui tt  u! titill tl tt l tit 
i 

t tut tlittluilttit   tu 1u li i
t titill ti   tuitt iultil 
tlltitill t ti 

"it$
 

†  tiitill tiilui t til ttill %ti!
tutiuu lli ii tll-
ili t it t t 
tuti
t t t!iti i}  t tiixtu itiqui x l
 tiuu  
t;  t ilultit  t ti
litt ti  ti l! lu 
†   tii tt  tiixtuliqui
 ti l i~ titu 
-u
  
† -xt tiitill tiii itill tiit ii
l!i 
ili !
l til-l tilt!tlt!t t 2titttt
itixtu 
† +l   ti ti l  tiit ti l i2 tit tu  tu t
liquit u  utiiu
 i tu  tttli  lt
tttli i iitiltuit ti!
i qui ltt 
itill tiitlquili
iut  
† itill tiiitill tiiiixtuiittu t
ii
l 

uit  ti  l
 ll"itill ti" 

† %t   ti  uuitill ti   tuiut
ullt 
 l i llt uui  t
  t i t 
 u 
† % u l t titill ti   tuiti llu  lli
i tiit 
i  uutitilli 
ili 30**/u    tuit i
itut
itillil ! ii tiiiutit! 
 t ti t l  uui ll  t
ui  i  uuu 

tu 

† itill titutiitill ti!itt !ittulitill ti!
ut t

i l ti liiiliu
t   ti it
ui t  l til ti!t ii i -
ili liqui ut
li! llt tutiitill tit it littit
 -
   
† +2itill tii   l utuii tiui 2i it   ti %t
ittulitill ti!
ut t lli2 titutittliqu! t
uutqui lttitill ti iiuitutii

 iiti t l u tt!til %ti lut
u lj  4liitill ti!2itill tit tiu  t
t i t 
"it$
2tiitill ti
w
€ 
 ‚ƒ  j


„



%t ti
ttttluti ttiuiquttluti! t
t ili lixtu!R ult,l tl uit ti ulti 
t t-
ili  i
  iit uui  !
il t i l
t tuit     
t  2t!tlutit it itit
 ti t !t t  tit  tuit! itill tit
t  ti +x l!tl ll  t  2t). 56 t78 #/ 

%t 2titiuiitluu!txittiqut
 t
2tt i uitill t ittiqu   Ê   
tiqu iti
"jui "t 2tiiti
 i   iti l
tt t  2t!
 i tu t
i ll
i lli quti tiuit +x l!tuit l
).6! 
i  t i tu t iu 
 t 
 tttlu
l t
itilu
l tt lli2 ti Mlul i tutiu ll 

%ii
lliqui!u  t tlu! il 2t l!t 2t

t  l
ili  2t
 ut
ili itt 2tilt t

ili ititut t tu itit 2ti il
itt utut!itutuR ult,l   2t
i il
i itill tit-u
ui  liqui-liqui  t  tt  tt
tliquil t t   lttliquil iluxtt
itill tit-u 

i 
ili  2t!u  (*i ttixtuli ii t! lxit 

ili
t !t
ili itt 2ti  tt t
ili itit
ut 


  2tiitill ti itill ti
u i!u itRi
l!it
i ti tititli tititill t 

"it$2 ! " #Ê ## 

ili itti  2tl t 
 xi   2t
t  uuitiu!it,i
lt
i t
ili itt  
tt
xliti tii  uuu ;tu l  tt
2tiit!
ut ulilt
 iiti lut l tu xiiti
t 2tiit &t
i i  tu !tt
ili itl l  
t 2ti
i   

it tt ti lt itill ti!
utit ttti l
 
 

4 tiu!  uuui tu
ili itt
itill tquit tt
ulttitill t u
i lttt
 uuu % li  illtqui iti l  i
l
quit   l t 

lt til!iitiu qui!t   l   t
u! ut

uui2 ti ti i  i tiui ititill ti!u
iti!utti t tuquitt
ili 

uiiti litill tiilll u  iiti!ititi ti 

#$"!  

u-i itill tiiti llt  tuiiti litill tiut
 
2tiixtu!
ut
titi  tiu 
l "Ê

Ê
 

$


i  it ti ttltiittitill ti  ll it"Ê

 

$
t
tii2 ut txtu t tu qui l 
iu ii tiul lit tii l li ti 

u-i itill tiilui tiuti luii titl t t tit
 t ltitit l 
[edit]Ind strial distillation

Typical ind„ strial distillation towers

w

Π




 

Large scale 

‘ 


applications incl… de both batch and contin… o…s fractional, vac…… m,
azeotropic, e† tractive, and steam distillation. The most widely … sed ind…strial applications of
contin… o…s, steady‡state fractional distillation are in petrole… m refineries, petrochemical and chemical
plantsand nat… ral gas processing plants.

Ind… strial distillation[14][20] is typically performed in large, vertical cylindrical col… mns known
as 



 ‘ or 


 
 with diameters ranging from abo…t 65 centimeters to 16
meters and heights ranging from abo… t 6 meters to 90 meters or more. When the process feed has a
diverse composition, as in distilling cr… de oil, liˆ… id o… tlets at intervals …p the col… mn allow for the
withdrawal of different 
  or prod‰ cts having different boiling points or boiling ranges. The
"lightest" prod‰ cts (those with the lowest boiling point) eŠit from the top of the col‰ mns and the
"heaviest" prod‰ cts (those with the highest boiling point) eŠ it from the bottom of the col‰ mn and are
often called the à

.
 

i   ti liuti litill tit 

%uti ltuluxt i lt  tiut Rluxtt

tit liquiut itill ti ti titt ti
tuttu ttt it tii   ti l!l  - l
iuti litill tit %itt!tli luxliquiili  
 tituli  t
i i tiititill tit 
luxt tii  iu
tti ll t!t
tttt,  ti
l
ili  ti li 
ili  ti l 
lt til!tluxt ti
i  ii  ti!ttu
tti ll tqui 

uiuti l ti ti t  lui i  ti!ui liquix !liqui
it ! i uit   itill tilil  l
ltutii -
uitiliu  iut 

ti iuti litill titi t ilt it
u

l 
Design and operation of a distillation tower depends on the feed and desired prod‹ cts. Given a simple,
binary component feed, analytical methods s‹ ch as the McabeŒThiele method[14][21] or theFenske
e‹ ation[14] can be ‹ sed. For a m‹ ltiŒ component feed, sim‹lation models are ‹sed both for design and
operation. Moreover, the efficiencies of the vaporŒli‹ id contact devices (referred to as "plates" or
"trays") ‹sed in distillation towers are typically lower than that of a theoretical 100%
efficient e‹ilibri‹ m stage. ence, a distillation tower needs more trays than the n‹ mber of theoretical
vaporŒ li‹ id e‹ilibri‹ m stages.

In modern ind‹ strial ‹ses, generally a packing material is ‹ sed in the col‹ mn instead of trays,
especially when low press‹ re drops across the col‹ mn are re‹ ired, as when operating ‹ nder vac‹‹ m.

Large Žscale, ind strial vac m distillation col mn[22]

This packing material can either be random d‹ mped packing (1Œ 3" wide) s‹ ch as Raschig
rings orstr‹ ct‹ red sheet metal. Li‹ids tend to wet the s‹ rface of the packing and the vapors pass
across this wetted s‹rface, where mass transfer takes place. Unlike conventional tray distillation in
which every tray represents a separate point of vaporŒ li‹ id e‹ ilibri‹ m, the vaporŒli‹id e‹ilibri‹ m
c‹ rve in a packed col‹ mn is contin‹ o‹ s. owever, when modeling packed col‹ mns, it is ‹ sef‹l to
comp‹te a n‹ mber of "theoretical stages" to denote the separation efficiency of the packed col‹ mn
with respect to more traditional trays. Differently shaped packings have different s‹rface areas and
void space between packings. oth of these factors affect packing performance.

Another factor in addition to the packing shape and s‹rface area that affects the performance of
random or str‹ ct‹ red packing is the li‹id and vapor distrib‹tion entering the packed bed. The n‹ mber
of theoretical stages re‹ired to make a given separation is calc‹ lated ‹sing a specific vapor to li‹id
 ti %tliqui   tliti
ut tuii lt   ittt
 
!tliquit  tiillt
tit 
 tqui  ti
illt
 i  i ill  tt
i l i tqui lt 
tti ll t-ill
  tt xt 
litt i itl
utt
 l-iti
utitluiti t 
 Viqui l-iti
utiiqutlt

lt   i tliquiiti
ututitut luxt 
 
iiti lt i t i tit xiuii Mt lu ti 
tti liquiiti
uttliti
uttliquiti   
 

ui "(0$"(9$i
l 
titi
+ ti tiR !
% l +R% "(.$

"it$itill tiii 

"it$
 !
w

Ê

„

 

 
 t-t ii l t ti l  lltt!ui  ilutlutit l
it iitu i u  
itilli tilutluti
t l ttt t l!ilui  t!t! t ll! llti
t t!i uttl t
  

"it$: ll

  

÷
„
„ „„ 
  
ʌ
„

÷


„



itill tiit ti  liquiutilit
il! tui  li 

tult tt ! llti t  M i 
litiilitill titu   itill ti 


litu
 it

ittil tu lit 
tu titlltitill t! ll 

„! t
t0.** 

%t iitl
 t!itill tii ultl!
t
titii ti tuii ti iu 
ili 
it u'ti
itill ti'ill-i tui
ti lti Ê#"Ê   
itill tiiut#Ê# 
  ti it -l til
l-l til ti l &itui ixtu it

ili it!t  titiiiu lt tixtui
 ullitill 
 

  %#& Ê  2!' 

   

 it i l
litill tiutil!
tt

itii ti tuii ti iu 
ili it  
u;ti
itill ti;ill-i tuit
i lti u
iit 
itii itill tii
utui u
  ti it  -l till-l til
 ti l  uitut it
ili it!t
tt  t ixtutixtuiitill 


ili ititt tu tit utliqui

  uqu ltxt lu ti tu t
liqui xt luiuu llt tiu +it !
i liqui ti l   utliquiill
i  tt tutliquii ! t u
qu lt tiu!tliquiill
il itu
il
titt tu
 u   it!  titi 
u uiti  uill
il tl
t tu 

ili it uu ll u
i t
ili it  
ttili  itill ti itiu
tiu tut itill ti itill ti
t
ili itti ti utt tut 

tliqui it  iquili
iuitt
ili liqui!
t t t tu t
ili liqui  t tu
 tt ttt tui u
 uiuut tt
tu llit
ili liquiixtu!tt tu i ullil

i t t tt  ii
 utliqui 
u t
t i tittu
t ! tit t tuit 
u t utt
ili t tu 

%u ui t
ili ittiti liuiu 

il titl
!uillt it
ili ititt tt
tuu ili it liti iuuitii t ! 
t% ti it 

÷  2  i lt t u 

%ulut
ili it uit u!u

 it tt lutili tl lit tu
ili it
tt 
ilitttii t i t
ili it! 
 ltuittu &ilt ti ll ll
ili itul

t tutu!i littt
ili it
ti   

÷ „ Ê„ Ê j„
Ê

Ê 

 

j ‘ 

  %#'#Ê 

ilitill ti uqutlit iitt i l
 

 uulitlli iut  

÷ tliquiil tilut
 iit !t #*6liqui

t i t
÷ tliqui  -l tilt!x l! lit i t 
÷ tliquiit i t
 liquiit 
ili itt ti

tl t7*/

<il=itill ti 
 i -l i ttt
 ii  i
ittut!iitt  lt t iiilitill tit

iitititiqu %tii llit tt til
itill titii  
ili ititii tiu 

" 

  

t ilt ti itill tit-u 

÷ t ilitill tit-u

>uilitt ilitill tit -u 

÷ il

Ê (Ê##
  

Mixtuliqui
ili it iil   t
lt 

7*/ t
  t
 i lilitill ti %titu ti! 
 ti litill tiiu 

 uuitill tiiitill ti t uu it
ili it

 uil t lxt lu!tuillt
 t
 tt i  t tuiitt
il  uu
itill tiiutitillut t  i 
ili it 
uii tu iti ti  t ti
u  uuiiit
  t i t
  i l
u 

l t  itl 

 ii   uu

itill ti 

>uilitt ti l  uuitill tit -u 

÷  ti l
÷  uu
V