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INTRODUCTION

TO

PRETREATMENT

Textile Effects
Fibre production

Cotton
Bast fibres
other CEL fibres
Polyester
Polyamid
Polyacryl
other SYN fibres
Wool
Silk

56.5 % cellulose fibers


39.5 % synthetic fibers

Textile Effects
Aim of the pretreatment

 High and even hydrophilicity / rewettability


 Good desizing effect
 High degree of whiteness
 Removal of seed husks
 Removal of foreign substances from the
fibers
 Lowest possible fiber damage
 High color yield
 Neutral pH
 Levelness of the effects

Textile Effects
Pretreatment is dependent on

 Fibres (natural or synthetic materials)

 Structure / Makeup / End use (Woven goods, knit


goods, yarn ….)

 Machine (Continuous, Discontinuous, Semi-continuous)

 Chemicals (Wetting-/Washing agents, Complexing


agents ….)

 Pretreatment processes (Desizing, Scouring, Bleaching


….)

Textile Effects
Fibres

POLYAMIDE

ACRYLIC POLYESTER

LINEN
SILK

COTTON

VISCOSE
WOOL

Textile Effects
Fibres: Classification of natural fibers

n a t u r a l f i b e r

m i n e r a l f i b a en r i m a l f i b e r v e g e t a b le f i b e r

s ilk w o o l a n d h a i r s h a r d m a n s o b n a i st et f i b e r p l a n t h a ir

t h i c k w o o l a n d f r u i t f i b e r l e a f f i b e r
a n i m a l h fa i in r es a n i m a l s h a i r s

Asbesto Silk Goat-hair Wool (sheep’s wool) Coco Sisal Flax Cotto
s Tussa Beef-hair - Alpaca wool Manila Hemp n
a.o. h Horse- - Lama wool Jute Kapok
hair Camel-wool Sunn
Rabbit-hair Kenaf
- Angora wool Ramie
Goat-hair
- Mohair
- Kashmir hair
- Tibet hair

Textile Effects
Fibres: Classification of synthetics fibers

c h e m i c a l f ib e r

c h e m i c a l f ib e r w i t h c h e m i c a l f ib e r w i t h
s y n t h e t i c p o l y m e r n a t u r a l p o l y m e r

P o l y a d d i t i oP no sl y- m e r i s aP t o i ol y n c so - n d e n s a at in o i nm s a- l v e g e t a b le
f i b e r f i b e r f i b e r d e r i v a t i o n d e r i v a t i o n

T i e r e i w e v i es sg - e t a b l eg u m p a p e r c e ll u l o s ic
f a s e r n p r o t e i n f i fb i be re r f i b e r f i b e r

Polyurethan Polyamide Polyester Casei Zein Gum Spinning- Viscose


e Polyacryl Polyamide n Ardei paper Cupro
Elasthan Polypropylene Polyester- n Cellulon Acetate
Polyethylene Ether Triacetat
Elastodien e
Modal acryl Modal
Vinyl
Polystyrol
Polychloride

Textile Effects
Machines

Discontinuous Semi continuous Continuous


systems systems systems

Jigger, Pad batch, Pad steam,


Jet, Pad roll L/J/U box,
Winch and other Immersion system,

Textile Effects
Machines: Discontinuous system

Textile Effects
Machines: Semi-continuous system

Textile Effects
Machines: Continuous system

Textile Effects
Analyses of different cotton qualities

Ca
Ca Mg
Mg Fe
Fe Cu
Cu Mn
Mn

Brazil
Brazil --Paranah
Paranah 2700
2700 1100
1100 250
250 66 30
30
--San
SanPaulo
Paulo 940
940 760
760 70
70 <1
<1 66

Peru
Peru 700
700 440
440 15
15 <1
<1 <1
<1

USA
USA --Texas
Texas 810
810 365
365 75
75 <1
<1
<1
<1
--California
California 600
600 540
540 40
40 <1
<1 <1
<1

Russia,
Russia,Turkey,
Turkey,
India,
India,Pakistan
Pakistan 1300
1300 570
570 110
110 33
66

Egypt 640 450 11 <1 <1


Textile EffectsEgypt 640 450 11 <1 <1
mg/kg
mg/kg (ppm)
(ppm)
Chemicals

 Surfactants (Wetting- and washing


agent)

 Complexing agent / Cracking agent

 Processor / Stabilizer

 Defoamer

 Enzyme

Textile Effects
The classical steps of pretreatment: cotton
woven goods

Singeing Burning down of the protruding


fibers

Desizing Removal of sizing agents

Scouring/ Improvement in hydrophilicity


Alkaline Cracking Cracking of seed husks
Removal of foreign substances

Acid Cracking Complexing/dispersing/cracking


of
alkaline earth metals and heavy
metals

Bleaching Destruction of colored


substances
Removal of seed husks
Textile Effects
Singeing

To obtain a smooth,clean fabric surface (Napless / pile less


finishing)
Parameter :
• fabric speed (up to 250 m/min)
• flame intensity (gas-/air-mixture; 1200-
1300°C)
• burner distance / burner position

receipt of goods brushing singeing tension beater impregnation


batching

Singeing: Parex-Mather
Textile Effects
Desizing: Sizes

Natural sizes (water insoluble) Synthetic sizes


(water soluble)

Starch is a polysacharide and consist of:


Polyvinyl alcohol size (PVA)
• 14 - 27% amylose (water soluble) Polyacrylate size (PAC)
• 73 -86% amylopectin (water insoluble) Polyester size (PES)

starch- amylose
Carboxymethyl cellulose
content in the starch
(CMC)
potato 20% 23%
maniok/tapioka 25% 18%
sago 27% 26%
wheat/maize 60% 25%
rice 75% 19%

Textile Effects
Desizing

Starch CMC PVOH Acrylate PES VA


copolymer
CO ++ ++ + +

CEL/PES ++ + + + +

CV-staple ++ ++ + +

CV-filament ++

PAN ++ ++ +

PA-filament + ++

PES-filament + ++ ++

CA/CT ++ ++

Textile Effects
Desizing: Starch size

DESIZING

ENZYMATIC SURFACTANT

 Starches  Water soluble sizes


OXIDATIVE
 Starches in
combination with  Starches
water soluble sizes
 Starches in
combination with
water soluble sizes

Textile Effects
Enzymatic Desizing - Advantages /
Disadvantages
Advantages of enzymatic desizing
• No fibre damage
• No use of aggressive chemicals
• A lot of process possibilities
• High biological degradability

Disadvantages of enzymatic desizing


• Low additional cleaning and cracking effect
• Low effects on certain starches, e.g. tapioca starches
• Effects can be reduced by certain size additives and other
impurities

Textile Effects
What are surfactants ?
Surfactants are water-soluble,

surface active agents

Surfactants are used in textile


applications as,

 Detergent
 Wetting agent
 Emulsifier
 Softener
 Lubricant

Textile Effects
Detergency / Washing power

hydrophob
ic
air

water
hydrophilic

oil, wax or
soil

material

Textile Effects
Scouring / Alkaline Cracking

Boiling out is the treatment of cellulose under strong alkaline


conditions.

Raw cotton contains a great number of foreign substances


such as hemicelluloses, proteins, lignins, pectins, fats, waxes,
natural dyes and seed husks. These are partly water-soluble,
partly only removable by an alkaline process. In some cases
an acid treatment is necessary.

Seed husks and cotton waxes can only be eliminated by


longer alkaline boiling or kier boiling. This process is
important to improve the hydrophilicity (a must for
continuous dyeing and printing). A boiling process is also
useful to reduce the danger of a catalytic damage in a
subsequent peroxide bleach.

Textile Effects
Bleaching

Bleaching means, to destroy the natural dyestuff in the fibre.

There are two chemically different bleaching processes:


 Oxidative bleaching with hydrogen peroxide, sodium
hypochlorite,
sodium chlorite or peracetic acid
 Reductive bleaching with stabilized hydrosulphite
preparations and
sulphoxylates.

The choice of chemicals depends on the required degree of


whiteness, on technological and ecological aspects, on the
machinery and on economic aspects.

Overdosing of the bleaching chemicals, insufficient temperature


regulation, too long bleaching times, existence of catalysts,
insufficient stabilizing, etc. may lead to damaging of fibers.
Textile Effects
Processor / Stabilizer

Bleaching agents, e.g. hydrogen peroxide, are “stabilized” during


manufacture. In bleach liquors which contain hydrogen peroxide,
bleaching only occurs after activation, e.g. by the addition of
alkali or/and by increased temperature.

This bleaching activity must be “regulated” to prevent rapid,


spontaneous decomposition of the bleach and to minimize
damage to the fibre, to avoid waste of bleaching chemicals as well
as undesirable side reactions.

This process of regulation or control is also called as stabilization.

Textile Effects
Tinoclarite CBB/G-I

STABILITY
in hot oxidizing
and alkaline
bath
INHIBITION DISPERSING
of of impurities
precipitations

PROCESSOR
ACTIVATION and
ENCAPSULATION REGULATION of
and INACTIVATION bleaching
of catalysts / active peroxide
heavy metal ions
THRESHOLD EFFECT
CPS principle

Textile Effects
Peroxide Killing

■ The leftover peroxide can cause serious problems in


further reactive dyeing

■ The depth of certain dyes can be lost up to 40%

■ Turquoise, blues and reds are especially sensitive to


peroxide

■ For peroxide killing either a reductive base product or


a catalase enzyme based product can be used.

Textile Effects
Influence of peroxide on reactive dyeing
With Invatex PC Without Invatex PC

Textile Effects
Influence of peroxide on reactive dyes

no residual peroxide 5 mg/l H2O2 30 mg/l H2O2


in bath in bath in bath

Rel. Depth 89 % Rel. Depth 76 %

Without
Ciba® TINOZYM® CAT

With
Ciba® TINOZYM® CAT

Rel. Depth 100 % Rel. Depth 100 % Rel. Depth 100 %

-
O2
Residual peroxide
in bath or on material 2 Merckoquant® 1.10011.

can be tested with Peroxide - Test


Merckoquant® test strips
analytical test strips
MERC
K
0 0.5 2 5 10
25
mg/l H2O2

Textile Effects
Reductive bleach

 Bleaching agent: Derivate of sulphurous acids


sodium di-thionite (Na2S2O4)
stab. sodium di-thionite
sodium bi-sulfite

Usually stab. sodium di-thionite (e.g. Ciba® CLARIT®


PS) is used

 Application only efficient as pre- or subsequent


bleach
 Low importance for cellulose fibers
 Use for PA and wool
 No full white possible

Textile Effects
Mercerizing

Caustic concentration 270 - 330 g/l NaOH 100% (28-32 °Bé)


Caustic temperature 15 - 20 °C (hot mercerization 60 - 90 °C)
Reaction time 45 - 60 sec. (hot: shorter time)

Tension against shrinkage


Stabilizing up to about 50 g/l NaOH 100%
Mercerizing wetting agent for quick and even wetting
Pretreatment raw, desized, boiled off, bleached

Textile Effects
Mercerizing Effects

Increase in colour depth:


By modification of the inner fibre surface, the number of
absorption places for the dye uptake is increased. Depending on
the class and type of dyestuff savings of up to 40 % are possible.

Covering immature and dead cotton:


Fibres which died off before maturity, so-called dead cotton, as
well as immature cotton which has been picked too early, form
small knots during the spinning process. These knots are
differently dyed or not dyed at all in the dyeing process.
Mercerizing and a suitable selection of dyestuff can level out these
differences.

Textile Effects
Mercerizing Effects

Dimensional Stability:
The latent tensions in the fabric are eliminated. During the washing
process after mercerization new hydrogen bonds are formed, which
"set" the fabric. An optimal dimensional stability of the goods can
only be obtained, if the alkali concentration in the fabric is
decreased below 50 g/kg NaOH 100 %, before leaving the stabilizing
zone.

Increase in tensile strength:


Due to the transformed orientation of the cellulose chains in the
cotton fibres their mechanical properties are changed. This leads to
an improvement of the tensile strength. In the case of yarn
mercerization the tensile strength may increase up to 40 %.

Textile Effects
Assessment of the pretreatment effects:
General
 Degree of desizing
 Water soluble / Residual fat
content
 Hydrophilicity / rewetting effect
 Ca-, Mg-, Fe-content
 Degree of whiteness
 Remove of seed husk
 DP-value, fiber damage value
 pH value on the fabric
 Mercerizing effect

Textile Effects
Assessment of the pretreatment effects:
Desizing

TEGEWA-Violet scale

Target: Assessment of the degradation degree of starch size

Procedure: Put fabric sample in iodine solution for about 1 min,


short
washing out with cold water, dap with filter paper
and
compare immediately with violet scale.

Textile Effects
Assessment of the pretreatment effects:
Water soluble

Water
Water extract
extract
(2x20
(2x20min.
min.after
afterpetrol
petrol
ether
etherextract)
extract)

grey
grey fabric
fabric 66 -- 10
10 %
%
good
good desized
desized <
< 0.7
0.7 %
%
moderate
moderate desized
desized 0.7
0.7 -- 0.9
0.9 %
%
Reference for 100% cotton

Textile Effects
Assessment of the pretreatment effects:
Residual fats

Petrol
Petrol ether
ether
extraction
extraction (3
(3hh
extraction
extractionin
insoxhlet)
soxhlet)

grey
grey fabric
fabric 0.8
0.8 -- 1.2
1.2 %
%
good
good scouring/bleaching
scouring/bleaching << 0.4
0.4
%%
moderate
moderate scouring/bleaching
Reference for 100% cotton
scouring/bleaching 0.4
0.4 -- 0.6
0.6
%
%

Textile Effects
Assessment of the pretreatment effects:
Hydrophilicity

Several methods: TEGEWA-drop test


Wicking-test
“modified wicking-test”

“modified
“modified wicking-test”
wicking-test” (measurement
(measurement of
of the
the capillary
capillary
rise)
rise)

time
time goodness
goodness of
of the
the hydrophilicity
hydrophilicity
(sec/cm)
(sec/cm)

-- 33 extremely
extremely high
high
33 -- 55 very
very good
good
55 -- 88 good,
good, acceptable
acceptable
88 -- process
process to
to be
be examined
examined
Reference for 100% cotton

Textile Effects
Assessment of the pretreatment effects:
Whiteness
Whiteness is a relative term , measured with the help of an instrument
known as – SPECTROPHOTOMETER

The instrument helps to measure the reflectance data of the substrate


( without color) and using this data in formulas coverts it into various
whiteness readings such as :

Ganz
CIE
Stensby
Berger
ISO/Tappi .. etc

Textile Effects
Assessment of the pretreatment effects: pH
value

The pH value of textile material is determined by the


extraction into a neutral medium – 0.1M KCl and
then checking on the pH meter .

Alternately the pH on textiles can also be checked


by dropping a drop of universal indicator &
immediately matching the color obtained with the
standard scale .

Textile Effects
Assessment of the pretreatment effects: Iron
content

The iron content on textiles can be determined qualitative by spotting


with nitric acid + pottasium thiocyanate .
The presence of iron will be indicated by the appearance of a red
color. The higher the intensity of the the coloration more is the
amount of iron present.

calcium
calcium // iron
iron
magnesium
magnesium

grey
grey 600
600 -- 2500
2500 ppm
ppm 10
10 -- 100
100
ppm
ppm
good
good pretreatment
pretreatment <
< 300
300 ppm
ppm <
< 10
10
ppm
ppm
Textile Effects
Assessment of the pretreatment effects: Residual
peroxide

The residual peroxide on the textile material can be


evaluated by spotting with 0.1M Titanum Chloride . The
orange coloration in presence of hydrogen peroxide is
the matched with the T scale .
The reading of which will immediately give
approximately the
mg of H2O2/ kg of fabric.

Textile Effects
Typical process route for
Elastane

Relaxation

Heat-setting

Scouring / Bleaching

Dyeing / Printing / Finishing / Whitening

Textile Effects
Typical process route for Lyocell
Woven goods
Woven goods Knit goods
Knit goods

Singeing Pre-wash
wide rope

Desizing +/- Bleaching


wide rope

+/- Bleaching T-I-O Process Fibrillation


wide wide
rope

+/- Caustifying Defibrillation


wide
rope

+/- Singeing
wide Dyeing
rope / wide

Fibrillation
rope +/-
Defibrillation
Defibrillation rope
rope
Finishing
rope / wide

Dyeing
rope / wide

Finishing
Textile Effects rope / wide
Linen / flax
Adjacent substances

Cotton Linen/flax

cellulose 90 – 95 % 60 – 65 %
pectines/hemicelluloses 1– 5% ~ 20 %
lignins - ~ 3%
waxes ~ 0.6 % ~ 1%
watersoluble parts ~ 2.5 % ~ 12 %

With cellulose representing more than 90% of the total fiber


composition, cotton is a relatively pure raw product in contrast
to linen, which contains only around 60% cellulose. Many more
impurities need to be removed from linen.

Textile Effects
Linen / flax
Objectives / Pretreatment steps

Objectives
Objectives
Possible
Possiblepretreatment
pretreatmentsteps
steps
 Removal
Removalof: of:
--sizes Enzymatic
Enzymatic
sizes
--incrustations Desizing/Cracking
Desizing/Cracking
incrustations
--alkaline Alkaline
AlkalineCracking
Cracking
alkalineearth
earthand
andheavy
heavy
metal Oxidative
OxidativeCracking
Cracking
metalions ions
Acid
AcidCracking
Cracking
 High
Highdegree
degreeofofwhiteness
whiteness
Peroxide
PeroxideBleach
Bleach(+/-
(+/-
 Good
Goodhydrophilicity
hydrophilicity
silicate)
silicate)
 High
Highfiber
fiberprotection
protection
MEGA
MEGABleach
Bleach
 Reproducibility
Reproducibility
Hypochlorite/Chlorite
Hypochlorite/Chlorite
 well-balanced
well-balancedcost-benefit
cost-benefit
ratio Bleach
Bleach
ratio
Mercerizing
Mercerizing
 Consideration
Considerationof of
environmental
Textile Effects Ammonia
Ammoniatreatment
treatment
environmental
Pretreatment processes for linen / flax

Soft handle Harsh


handle
(e.g. dress goods /drapery) (e.g. table cloth)

treatment with treatment with


NaOH soda ash
+ Cracking Agent + Cracking Agent

1–2 2–3 2–4


oxidative bleaches oxidative bleaches oxidative bleaches

Textile Effects
Bulk trials
Circulation apparatus

grey
greymaterial
material

Acid
AcidCracking
Cracking++Peroxide
PeroxideBleach whiteness
Bleach whiteness
Berger 30
Berger 30

Alkaline Cracking + Peroxide Bleach


Alkaline Cracking + Peroxide Bleach
whiteness
whitenessBerger
Berger47
47

Peroxide
PeroxideBleach
Bleach++Peroxide
PeroxideBleach whiteness
Bleach whiteness
Berger 53
Berger 53

Acid
AcidCracking
Cracking++Chlorite
ChloriteBleach whiteness
Bleach whiteness
Berger 73 material:
material: 100%
100%linen
linenrove
rove
Berger 73 country: Lithuania
+ Peroxide Bleach country: Lithuania
Textile Effects + Peroxide Bleach
Pretreatment of Silk

Aim
Aim
 removing

removingofof
Washing
Washingtotoremove
removeDirt
Dirtand
andextrenous
extrenous
matter
matter
Degumming
Degumming
Oxidative
OxidativeBleaching
Bleaching
Reductive
Reductivebleaching
bleaching

Principle
Principle
 The

Thewashing
washingisisdone
done
in

indiscontinuous
discontinuousororcontinuous
continuousmachinery
machinery
as

asdetergent
detergentor
orsolvent
solventscouring
scouring

Textile Effects
Wool
Raw wool - impurities (example)

21%

48%

9%

22%

grease suint sand, dirt, nat. impurities wool fibre

wool type: superfine merino

Textile Effects
Wool
Pretreatment processes

Washing / scouring

Crabbing / potting

Milling

Carbonizing

Chlorinating

Bleaching
(oxidative, reductive)

Textile Effects
Typical process route for viscose

Washing/Desizing

dyeing, printing, finishing


Washing/Desizing Caustifying
grey state

Caustifying Washing

Washing/Desizing Caustifying Bleaching

VISCO-COMBI-BATCH Washing

Textile Effects
VISCO – COMBI – Batch
An ace in Ciba preparation

combines the conventional sequence of


processing:

Desizing (oxidative)

Cleaning (removal of spinning oils and


preparations)

Bleaching

Caustifying

Textile Effects
Benefits of the VISCO – COMBI – Batch

 A combination of different steps (desizing - caustifying -


bleaching)
which results in a considerable rationalization of water
consumption,
energy and time
 No special separate machinery is required
 Extremely clean fabric with a very good removal of all
disturbing
residuals such as size, oils, waxes, sulphuric components,
inorganic and metallic impurities, ….
 Avoidance of folding and creasing as it is an open-width
batching process
Textile Effects
 An almost complete caustifying effect in terms of color yield
Color yield improvement on viscose
After different processes
PB ENZ PB CPB VCB VCB
with silicate/16h 16h
16h

Ciba® TINOZYM® AL g/l 10 - -


-
Ciba® ULTRAVON CN g/l
®
5 5 5 5
Ciba® INVATEX® CRA g/l - 3 3 3
Ciba® TINOCLARITE® BS g/l - 5 -
-
Ciba® TINOCLARITE® CBB g/l - - 12
12
silicate 38°Bé ml/l - 8 - -
NaOH 100% g/l - 10 40 40
H2O2 35% ml/l - 30 10 30
Color Strength in %
Printing
- green (reactive) 100 82 130 105
- orange (reactive) 100 88 124 115
- brown (reactive)
Textile Effects
100 86 142 128
Dyeing