TECHNOLOGY OF TEXTILE

PREPARATION AND FINISHING

(TXL141; 3-0-0; 3 CREDITS)

PREPARATION OF PROTEIN FIBRES

Preparation of Wool

Carbonization
Scouring
Bleaching

CARBONIZATION
Objective: To remove cellulosic impurities
from wool by treatment with acid/acid
producing salts.

Raw wool may be contaminated with vegetable

matter of cellulosic nature, consisting of seeds,
burrs, grass etc.
It needs to be removed in fibre stage itself from
wools with high content of vegetable matter

Generally done by treatment with sulphuric acid

Mineral acids turn cellulose into brittle
carbonaceous mass which can be removed by
crushing it

SEQUENCES
Acidification Drying/Baking Crushing Dusting
Neutralization
Processing Stages:
Treatment with (5-7% w/v) sulphuric acid and acid stable
wetting agent.

Hydro extraction

Drying at 60-70oC to low regain

Baking at 110oC in dry heat for 2 min. (wool is relatively

stable to acidic conditions. The vegetable matter turns
brown/black, becomes brittle)
Crushing to break the degraded vegetable matter to small
fragments by passing through heavy fluted rollers
Dusted and Neutralized with sodium bicarbonate.
Bleaching with acidic hydrogen peroxide to
yellowing caused by carbonization

minimize

WOOL SCOURING
The high amount of impurities may hinder the processing of
wool.

The transfer of wool grease from fibres to metallic machine

parts may lead to

Dirt/oil accumulation on processing equipment

Poor drafting performance

Therefore, wool is generally scoured at fibre stage.

Presence of scales on wool fibre surface leads to a tendency

to felt/shrink.

Scouring involves treatment with aqueous scouring liquors

containing mainly surfactants.

Efficacy of scouring can be increased by mechanical

agitation or stirring action. However this may also lead to
fibre entanglement.

WOOL SCOURING- SALIENT FEATURES

Generally done at raw wool stage.

Residual grease/wax is kept around 0.5-0.75%.

Modern machines used Hopper bottomed

bowls.

Older machines Long bowls with flat bottoms.

Older machines 4-5 long bowls (35-40 m.)

Modern machines At least six bowls (16-28 m)

Scouring may be carried out in a series of bowls

Wool fibre mass is transported from one bowl to

another with gentle stirring
Non ionic surfactants are primarily used for
contaminant removal
Sodium carbonate may be used as builder
sometimes to facilitate contaminant removal
As wool gets cleaned progressively, the
composition of treatment bowls keeps changing.

AUXILIARIES USED
The most important auxiliary for wool scouring is
a detergent.
Alkyl phenol ethoxylates have been used as
highly effective detergents but are being phased out
due to environmental concerns.
Due to the Eco-friendly nature, fatty alcohol
ethoxylates are nowadays being preferred over
Alkyl phenol ethoxylates.

TYPICAL COMPOSITION OF AUXILIARIES IN

A WOOL SCOURING MACHINE:

I BOWL

Soap
(%)
0.75

Alkali
(Na2CO3 %)
0.20

Temperature
(oC)
49-52

Time
(Min)
2.5-3

II BOWL

0.5

0.1

46-49

2-2.5

III BOWL

0.25

0.1

43-46

IV BOWL

Water
only

40-43

1.5

pH should never be above 10.

Temp. 35 40oC but never above 60oC.

WOOL SCOURING MACHINES

There is a mechanism to continuously agitate wool in

a rectangular bowl or shallow tank

Wool is transported to the next bowl.

Before being transported to the next stage, the wool
mass
is
squeezed
to
minimize
upstream
contamination.
A feeding conveyor transfers the raw wool to the
scouring trough.
The wool is agitated and at the same time moved
forward by the action of a unit situated just above the
bowl.
An output conveyor transfers the wool to the other
bowl with an intermediate pad unit squeezing the
wool between the two bowls.

SWING RAKE TYPE MACHINE

The rakes move individually by a cam and crank

arrangement. The rakes come down, press the
wool, move it forward and rise vertically up in
the process getting detached from the wool mass.
They then move back, come down again and the
cycle continues.

HARROW TYPE MACHINE

For a gentler treatment. Here all the prongs move
together. This is more suitable for finer wool,
which can undergo damage and felting in a more
vigorous swing rake machine.

BOWL DESIGN
In modern machines, the emphasis is on reducing
the total length of bowls to reduce chances of
fibre entanglement.
This is achieved with hopper bottomed (deeper)
bowls which ensure better dirt removal.

Machine type
Bowl design

Width
No. of bowls
Cumulative length of
bowls (m)
Temperature (oC)

Old
Shallow and
flat
Long
4-5
35-50

New
Deep
(hopper bottomed)
Short
6
16-28

~40- 50

~30

WOOL BLEACHING

Wool is bleached with hydrogen peroxide. The

chlorine based oxidative bleaching agents are not
suitable for wool.
General bleaching sequence is: pH -8.5-9 at 50-60C
for two hours.
The activator should be mild alkali.
The stabilizers used are phosphates, tetra sodium
pyrophosphate or sodium tri polyphosphate.
Since wool can be damaged under alkaline condition,
an alternative is to bleach in acidic conditions using a
per acid activator (pH 5-6).
This is a BASF promoted process, bleaching is done at
pH 5 with activator Prestogen W at 80C for an hour.

CONTD
H2O2 and peroxy compounds can cause
progressive oxidation of disulphide bonds in wool
Resulting
in fibre damage which can be
accentuated in subsequent dyeing.
Hence
prebleached wool should be dyed
preferably below 80C.
Another
variant of acidic bleaching was
developed by IWS and BASF.
In this process, wool is padded with 350 gpl H2O2
solution acidified by 2 gpl formic acid.
By batching (cold-pad-batch) overnight, excellent
bleaching is obtained.

REDUCTIVE BLEACHING
Reductive bleaching of wool is carried out with following
agents.

Thiourea dioxide
Sodium dithionite
Zinc formaldehyde sulphoxylate
Sodium formaldehyde sulphoxylate
Sodium dithionite is the preferred reducing agent.
Bleaching is carried out at 45-65C at pH- 5.5-6 for 1
hour.
Bleaching can also be carried out with thiourea
dioxide.
To prevent heavy metal catalyzed decomposition of
bleach bath, inclusion of a sequestering agent is a
must. The bleaching is carried out at pH 7 at 80C for
an hour.

COMBINED OXIDATIVE REDUCTIVE

BLEACHING
Peroxide bleached wool has a reddish tone
Whereas reductively bleached wool often has a
greenish tinge but a natural white is generally
the demand of the industry.
A sequential oxidative and reductive bleaching
process is supposed to peroxide a neutral white
colour.
Bleaching with thio urea oxide is 3 times cheaper
in cost and also has the advantage of low COD &
BOD.

In this approach wool is first bleached with

alkaline H2O2 at 60C for 1 hour.
To the bath thiourea is added and pH adjusted to
4.5-5.5.
Thiourea is converted to thiourea dioxide and
bleaching is carried out at 60C for another 25
min, followed by washing and rinsing.
Thus in the first stage oxidative bleaching
occurs with H2O2 and reductive bleaching
takes place in the 2nd stage with thiourea dioxide.

SILK DEGUMMING
Objective:

To impart soft

handle and lustre to silk

by removing sericin, any
impurities picked up during

reeling throwing etc. Some

natural wax, coloring matter
and minerals may also be
removed during degumming.

Sericin is a protein which forms bulk of the gum

or the outer protective coat in a silk filament
Hence the process consists of cleavage of peptide
bonds of sericin, either by hydrolytic or other
methods, and its subsequent removal from
fibroin by solubilization or dispersion in water.

FOLLOWING ARE THE MAIN DEGUMMING

PROCESSES:

Extraction with water.

Boil-off in soap.

Degumming with alkalies.

Degumming with acids.

Degumming with enzymes.

Degumming with organic amines.

Although both fibroin and sericin are proteins,

they differ significantly in their constitution.

GIVEN BELOW IS THE TYPICAL AMINO ACID COMPOSITION

OF FIBROIN AND SERICIN:

The main constituents of fibroin are glycine,

alanine and serine whereas
In sericin it is serine, aspartic acid and
glycine.
Hence any degumming method should target the
peptide bonds between the amino acids found in
majority in sericin.
However, in practice, methods have been
developed on empirical basis.

EXTRACTION WITH WATER

Sericin removal can be achieved in water at high

temperatures.

It is not a commercial process.

Upto 96% sericin can be removed by extracting it
with water at 115oC for 3 hours.
Although there is still a doubt if the removal
occurs through hydrolysis or dissolution.

BOIL-OFF IN SOAP

It is an old process and seems to be still favored

commercially.
Olive oil soap (Marseille soap) is the most widely used
soap.
Following is a typical recipe:

Marseille soap

20-30% owf

Time

90-120 min.

Temperature

90-100oC

M:L

1:40

Amount of sericin removal also depends on the type of soap used in

the degumming process.

Degumming depends on the alkali formed on hydrolysis of soap and

the soaps hydrolyzing the most have the highest degumming power.

MELTING TEMPERATURES OF FATTY ACIDS

Acid Name

Structure

Lauric (C12)
Palmitic (C16)
Stearic (C18)
Oleic (C18)
Linoleic (C18)
Linolenic (C18)
Arachidonic (C20)

CH3(CH2)10COOH
CH3(CH2)14COOH
CH3(CH2)16COOH
CH3(CH2)7CH=CH(CH2)7COOH
CH3(CH2)4(CH=CHCH2)2(CH2)6COOH
CH3CH2(CH=CHCH2)3(CH2)6COOH
CH3(CH2)4(CH=CHCH2)4(CH2)2COOH

COMPOSITION OF OLIVE OIL

Fatty acid
Oleic acid
Linoleic acid
Palmitic acid
Stearic acid
-Linolenic acid

Percentage
55 to 83%
3.5 to 21%
7.5 to 20%
0.5 to 5%
0 to 1.5%

Melting
Point
+44
+63
+70
+16
-5
-11
-50

c) Degumming with Alkali Buffer

With alkalis, the pH of the boiling bath should be maintained

between 9.5-10.5.

Below pH 9.5, the rate of degumming is too slow and above 10.5,
the risk of chemical damage is high.

Hence many times, alkaline buffers like

Sodium carbonate/sodium bicarbonate,
Sodium hydrogen phosphate/trisodium phosphate,
Potassium tetraborate/boric acid etc. have been used.

Typical recipe is given below:

Sod. Carbonate (0.5M)

5.3 gpl

Sod. Bicarbonate (0.05M)

4.2 gpl

Non-ionic Surfactant

3gpl

Temperature

95oC

Time

20 min.

d) Degumming with Organic Acids

Mineral acids may cause significant damage to silk, hence generally

only organic acids are used.
A typical recipe is given below:

Tartaric acid (0.05 M) pH- 2.3

8 gpl

Non-ionic Surfactant

3 gpl

Temperature

110oC

Time

60 min

The mechanism of acid attack on silk peptide bonds is shown below:

TREATMENT CONDITIONS AND OBSERVED RESPONSES FOR YARNS

DEGUMMED WITH ORGANIC ACIDS

e) Degumming with Enzymes

Considered to be a safer method which results in minimal damage

to silk.

Carried out at milder temperature and pH

The natural hydrophobic impurities are not removed effectively.

One of the advantages lies in the fact that enzymes specifically

targeting peptides bonds occurring in majority in sericin can be
selected.

Since the constitution of sericin and fibroin is different, such

enzymes will have minimum action on fibroin.

The main enzymes used are trypsin, papain and bacterial

enzymes.

Trypsin

Trypsin is a serine protease with the highest activity at pH range 7-9

and 37C.
Ammonium bicarbonate (0.1 M/l) can be used as buffer. It is applied at
1-2% owf for 1-4 h.
Better degumming results when alkalis are combined with proteolytic
enzymes.
Pretreatment with alkaline solution swells sericin and results not only in
better degumming but also in better scouring (wax, fat removal).

Papain

Obtained from papyrus latex.

Most effective at 70-90oC temperature and at pH-5.
It is a sulphydryl enzyme and hence requires a sulphydryl (-SH)
compound as an activator.
Has a wider specificity towards polypeptides as compared to trypsin.

Bacterial enzymes

Alkalase, developed by Novo nordisk is claimed to be

more effective than trypsin or papain.

Specificity of proteases

f) Degumming with Aliphatic Amines

Methyl, dimethyl, ethyl and trimethyl amines can be used.

Amines show good degumming (upto 90 % sericin removal) with

little loss in tensile strength.

Typical recipe:

Trimethyl Amine
N.I.D.

0.25 M
3 gpl

Temperature

80oC

Time

45 min.

M:L ratio

1:25

COMPARATIVE ASSESSMENT OF DIFFERENT

DEGUMMING METHODS

Different methods have been evaluated on the basis of

weight and strength loss after degumming.
Agent

Weight Loss

Strength Loss

Marseille Soap

100

100

Carbonate + Bicarbonate buffer 100

82.2

Tartaric Acid

100

81.3

Methyl Amine

97.7

119

Alkalase

85.5

112.9

BLEACHING OF SILK

Bulk of the naturally occurring colour in the silk is actually

contained in sericin.
Since the degumming process is not able to remove the sericin
completely, retains some of its natural tint after boiling off.
Widely bleached with hydrogen peroxide with a typical recipe:
Parameter

Mulberry silk

Wild silk

H2O2 (35% w/v)

15-20 ml/l

20-30 ml/l

Stabilizer

2 gpl

4 gpl

M:L ratio

1 : 20

1 : 30

Temperature

75-80

80-90

Time (hr)

1-2

3-4

pH

8.5-9

8.5-9

Alkali used is either ammonia or tetra sodium pyrophosphate.