Chemical Treatmentsof Textile Fibers

194882597.doc.
ms_office
By Chemist: Samy Mostafa
/ ( )
Chemical Treatments Of Textile Fibers

Pretreatment , dyeing , printing & finishing
-1-
194882597.doc.ms_office

Chemical Treatments of Textile Fibers
Pretreatment , Dyeing ,
Printing and Finishing

/

-2-
Chemical Treatments of Textile Fibers

)Pretreatment, Dyeing, printing and Finishing )

) , , (
Schematic digrame
Illustrates The Different Stages of Cotton fibers from (A to Z)
Cotton
seeds
Cotton
cultivation
PRETREATMENT
Separation of
fibers
From Cotton
seeds
Collection
of Cotton
Woven
Goods
Fibers
Knitted
Goods
White
Goods or
Half
Bleach
Full White
Printing
Dyeing
Yarn
Finishing
Garments
-3-
Using
Spinning
Textile fibers divided into 4 groups :

1Artificial fibers
2Mineral fibers

3Animal fibers

4- Vegetables fibers

* Artificial fibers (Synthetic fibers)
a- Acrylic fibers these are made from polymerization of acrylonitrile.
n(CH2 CH C N)
CH2 C ( CH2 CH )
CH2 CH
n
CN
CN
CN
.
b- Polyester fibers these are made from condensation of terephethalic
acid (P.carboxlic gps) with ethylene glycol
ester.
HooC
CooH+2 CH2 CH2

oH
o
oH
Ho CH2 CH2 o C
Ester molecule (monomer)
o
o CH2 CH2 o C
-2H2O
o
C o
CH2 CH2 oH
polymerization
o
C o CH2 CH2 o
Theses are Polyester fibers

c- Niylon-66 (polyamide) are made from adipic acid and
hexamethylene diamine )(
Hooc (CH2)4 CooH+H2N (CH2)6 NH2 -2H2O amide
6 ) )
-4-
o
Hooc (CH2)4 C NH (CH2)6 NH2 2 mole Polymerization
o
C NH (CH2)6 NH C (CH2)4
Hooc (CH2)4
C NH (CH2)6 NH2
n
( )

) ) d- Vegetables fibers as Cotton fibers , Linen
Chemical Composition of cotton fibers :

Cellulose
95-96%
Protein
1%
Wax
1%
Oils (fatty acids) 1%
Ash
1%

Row Cotton (crude) is yellow ()
.To gray
Also this row cotton contain about 2% from wax and oils these
impurities cause the cotton is very hard to wet processes
(hydrophobic) .....

) (Sizing Operation
( : )
%20
) (soft
) (friction

( )
() ( ).
-5-
Structure of Cellulose
H
Ho
H
oH
oH
H
H
CH2-oH
CH2oH
H
CH2oH
H
oH
oH H
oH
Ho
oH
H
oH H
CH2-oH
n H
Ho
1 ry hydroxyl gp. is more active

General formula is (C6H10O5)n
From the above st. cellulose is a long chain polymer produced by
linking together of a large no. of monomers (glucose units) also
cellulose fibers contains both a crystalline and amorphous regions.
:
(ordered) ( compact)
(disordered) ( amorphous)
X
By X-Rays measurements appears as
after
Pretreatment
Order or crystalline

) (
disordered or amorphous

)(

) (
) (
-6-
Pretreatment Operation

inspection ( chick up ) :
- :
( ,
, , ).............
- :
-1 : , %100 , %100 ,
) 70% (H2So4
1
50/50 , 35/65 , 20/80
%100 .
wet after
= %of pes.
100 = %
wet before
-2 kind of sizing agent present

* Starch
)detected by (I2 KI
blue to black
)* Polyvinyl alcohol (PVA
detected by boric acid
green to blue color
)* carboxy methyl cellulose (CMC
detected by 2.7 dihydroxy naphthalene
blue to purple color
-3
Effect of chemicals which added in different operations
()

)(wash and wear
* Washing test

5 / 60 20
pass or
()
reject
* Bleaching test
) )
BL
-7-
pass or reject
* Mercerizing test

1
By caustic soda cold 25-28 Be (230-270 g/l)

. Approved or Rejected

A Singeing Process

First singeing operation : is mean burning operation . and this
process is formed by tow methods
- by hot plates or

- by direct flame

This method is famous and this operation (singeing) is pure
mechanical finishing without chemicals.

.
.

Before singeing
After singeing

.
Aims of the singeing operation is the removing of the small
hairiness and pilling from the surface of the fabrics or textiles .
:
- speed of machine 80-120 m/ min.

-8-
- distance between fabric and flame.

- type of fabric

-weight of fabric

.

(. )
B- Desizing operation
) )sizing .
.
Desizing : is the removing of any kind of sizing agents which
added during the weaving operation to increase the strength and
softening the yarn specially (warping yarn) and then we obtain the
optimum running without cutting to yarn.

( . )

()

( )

-9-
Sizing Agents
Lubricants

as wax oils animal fats

Film formation

Artificial sizing ag.

As polyvinylal
)(PVA
Natural sizing ag.

as starch or
Carboxy meth CMC
)(CMC

( )
(PVA)
)wetting agents(Surfactants
:
Enzymatic desizing
1
PH

) (wetting age.
()
( ) .
Recipe of the operation

Enzyme 3-10 g/l
)Wetting 1-3 g/l (surfactant
Padding
steaming
) )
C.P.B 6 ( )
exhaustion ...........
Oxidative desizing
2
- 10 -
By using of persulphates as desizing agent patents of (Bohac)

viena or by using Hydrogen peroxide (H2O2)
H2O2 has also been used as Oxidative desizing agent.

.
C- Scouring Process

:
-Sod.hydroxide (NaoH)
20-30 g / l (solid )
-Wetting (surfactant)
8-10 g / l
-Sequest. (EDTA)
1-2 g / l
.
We know that the natural fibers as cotton contains oil wax
heavy minerals as (Fe+2 , Ca+2 , Mg+2) these impurities leads to the
cellulose is hydrophobic and the operation which removing these
impurities is called (Scouring) even though these impurities are
not soluble in water thy can be removed by extraction ( dissolving
in organic solvents)
ph.ph
)Ph.ph ) . .%70
-Emulsification of fats and waxes

Surfactants Wetting
-Saponification
Oil + NaOH
Soap
After converting these impurities into water soluble components
.
5
85-80 5 10095
Chemicals of Scouring Process
1- Sod.hydrox. 20-30 g/l (flacks)
2- Wetting agents (Surfactants) surface active agents which
decrease the surface tension of textiles and increase the
penetration of chemicals. and the fibers become
(HDROPHLIC)

- 11 -
3-Sequestring agent as (EDTA) it is a complexing agent with

heavy metals (Fe+2 , Ca+2 , Mg+2) to prevent the damage of
cellulose specially in case of Bleaching Operation .
BL

.
St. of EDTA
o
CH2 C oH
o
N
CH2 C oH
e-

EDTA .
Ho C CH2
o
N CH2 CH2
Ho C CH2
o
e-
Heavy Metals Fe+2 , Ca+2 , Mg+2
Me+
e-
N
e-

BL
)(exhaustion
5 100-95
- 12 -
(continuous)
Impregnation
Homogenous squzing
Steaming
Washers
) ( ( ) Batching
Drayer
Neutralization

Bleaching Operation
What is the mean of bleaching operation ?
Answer : Natural fibers as cotton , wool , linen .. etc. are off
white in color (yellow grey)
Why : due to the presence of color impurities which present in the
faibers.
And so the bleaching operation is can be defined as :
The destruction or destroy of these colors of impurities and must be
we know the bleaching operation is very important process specially
in dyeing of medium or light shades.
, ( BL
. ) , , ,
Examples of common Bleaching agents:
1- Sodium hypochlorite
(Naocl)
2- Sodium chlorite
(Naclo2)
o
(CH3 C o oH)
3- Peracetic acid
- 13 -
4- Hydrogen peroxide
(H2O2)
BL
) (.(H2O2)
Also H2O2 is the most widely used in textiles bleaching from 1920 by
concentrations from 35-50%.

) .( 1
Analysis x 0.1 N KMno4
(self indicator )
Bao2 + H2So4
BaSo4 + H2O2
(The bleaching on Constitutions) BL
1- half amount of needed water.
2- Stabilizing agent
1-2 g/l.
3- Sequestering agent 1-2 g/l as (EDTA) with heavy metals
Fe+2,Ca+2,Mg+2. (complexing agent)
4- Caustic Soda (NaoH) 8-10 g/l (flacks). Or Liquid ???
5- Wetting agents (Surfactants).
Surface active agents to decrease of surface tension of textiles and
leads to penetration of chemicals inside cellulose as alcohols.
6- Finally Hydrogen peroxide 10-15 c.c/l optical brighteners.
padding (steaming) exhaustion
padding (C.P.B) dewelling time washing on hot
Mechanism of reaction of Bleaching Process:
H2O2 is a weak acid stable at low Temp.and PH but it ionize at high
Temp.and PH to H+ ion and per hydroxyl ion Hoo- this per hydroxyl
ion is very active bleaching agent specially in alkali med. pH (11-12)
-
- + + Hoo
H 2O 2
H
e
Hoo
oH + o0 atomic oxyg. is very active in BL of textiles.
Sequestering shape as in scouring make complex with heavy metals.
) ( optical brighteners

Based on stilbene derivatives
CH = CH
- 14 -

H2O2
By oxygen killer enzyme
D Mercerization
.

.
Mercerizing process discovered in 1844 by English scientist names
John Mercer, Mercerization process is the treatment of cotton fibers
with a strong solution of caustic soda up to 240-270 gm/L . why ? ?
In order to improve the luster, handling (softening), swelling, increase
the dye ability and it increase the strength and elongation of cotton .
The general formula of Mercerization as following .
Cold
Cellu oH + NaoH
cell - oNa
1 ry hyd. gp.
(Exothermic reaction
So the solution of NaoH must be cold 10 15 0c and the ideal

concentration from 25-28 Be. 240 270 g/l
) (
By titration with 1N Hcl using ph.ph as indicator.
:
) ) Batch
Impregnation
Squeezing
(NaoH)
% 80-70

Washing by tension
Complete washing
Swelling time
) 60-50 )
Neutralization
By acid A.A.
pH control
dyeing
Batching
- 15 -
Draying
( )
E- Dyeing Operation

, %100 , %100 , ,

:
: .
:
.

15 min.
wash

.
(
)

)Polyester (120-130
)Cotton (70-80
Or on cold as now
( )
- 16 -
( pes.)
) " ( Disperse Dyes"
Also the dyeing of polyester is classified to tow methods :
1- Dyeing by immersion (exhaust)
()

) ) (pH 4-5) )buffer(.
And adding dispersing leveling agent and dyestuffs by
calculation of amount of dye from the % of Dyeing Lab.
:
Temprature
140
Time of fixation 30-60 min.
Cooling
1-2 0c / min.
130 c
120
1 hour
100
Heat up
1-2 0c / min.
Atomatic
machine
80
60
40
Acetic acid
Dispersing leveling dyestuff
80 0c

R.C
20
Time
10
20
30
40
50
60
70
80
90 100 110 120 130
5 -4 pH
. Buffer %1
What is the mechanism of dyeing of polyester by immersion
method?
The general structure of polyester fibers is appears (by x-ray):
o
o
o
R
1
as :
o
R2
The above structure appears as highly crystalline form

- 17 -
) (
and it quit tightly packed together
) (
So the polymer is very little affinity to dyeing and also
disperse dyes have low solubility in water and there for the dyeing
process applied under (high pressure up to 3-4 bar and high
temperature 120 130 0 ).(sever condition)
Pressure: is the force per unit area
1 bar = 1 kg /cm2 / sec2

i.e 1 bar = 10000 kg /m2 / sec2

i.e 3-4 bar = 30000 40000 kg /m2 / sec2
There for at this server conditions there is thermal excitation
for pes. cause the polymer structure become less crystalline it
opening gaps for the dye molecule to enter .

.
So this interactions between the disperse dyes and polyester
is Van der - wall,s force No chemical reaction.

( / 5 2-1
After cooling to 85-50 0c hot rinse and drain then we enter to bath
of " Reduction clear " specially " dark shades ".
What is the mean of Reduction clear?
R.c. is the removing of unreactrd or unfixed disperse dye and
cleaning of the staining of cotton fibers( in case of blended fibres)
Mechanism of R.C. ))
Na2S2o4 + 2NaoH
2Na2So4 + 2H (Sod.
Hydrosulphite) is very strong reducing ag. in alkali
medium PH from (11-12)

- 18 -
Chromomphors
N
C O
Sod.hydrosulphite is very strong reducing agent

After R.C. process we make color fastness test
Washing , Rubbing (wet-dry) , Staining
Accept
draying
inspection
setting
dyeing of cotton.
Reject
wash again (reprocess).
2Another method for dyeing of polyester is thermosoling
dyeing which discovered by "Dupont" in 1949 to dyeing polyester
100 % or blended fabrics 50/50,65/35, or 80/20 using very high
temperature 190-220 c0 to obtain rapid fixation of dyes .
Thermosol Scheme (fllow chart) for dying of polyester
polyester
Fibers or blended
Squezing
Drayer
Fixation
Finally
(padding)
impregnation
Leveling ,antmigration
pick up 60-80%
By IR or direct flame
In oven 180-220 0c
to 30-60 sec.
R.C. as in jet machine
by the same method
Then test the color fastness

Accept
dyeing of cotton.
- 19 -
at room
temperature
feeding tank .
Disperse dye,
wetting agents,
dispersing
leveling,
antmigration
Reject
wash again. Till it ok.
% 100 ) / (
:
1- Direct dyes :
Soluble in water and it absorbed on fibers as stilbene type.
Ho
N N
CH CH
So3Na
N N
oH
So3Na
"Brilliant Yellow"
:
Color fastness to ( light - perspiration - washing ) is weak.
2- Vat dyes : (keto form) insoluble in water.

Examples of vat dyes :
Natural vat dyes "indigo dye" ) (
o
H
N
Reduction
C C
C
(0)
N
H
o
Reduction by Na2S2o4 /2 NaoH
Oxidation by H2o2 or by air
As anthraquinone derivative
Enol form
o
C
C
o
- 20 -
2H
3-Reactive dyes :
There is a chemical reaction and it bonded by addition or
substitution .reactive dyes first appeared in 1956 it contain a
reactive group as a haloheterocyle
It activated when applied to cotton fibers in alkali medium to
form a chemical bond.
pH 10-11
Examples for reactive dyes :
* di chlorotriazine ( Procion M )
cl
Dye N
H
))
N
N
cl
+ Ho cellulose
Soda
Ash
cl
Dye N
H
N
N
Cell. o
Not that : pH of the bath must be 10-11 to eliminate Hcl formed.

* mono chlorotriazine ( Procion H )
N
Dye N
H
* di chlorodiazine - primidine derivatives

cl
N
Dye N
H
cl
- 21 -
( Drimarine )
)(Levafix dyes
* Alkylsulphonylprimidine
So3H
N
N
Dye N
H
cl
This kind of dyes is specialized to printing and dyeing on
) cold(C.P.B
:
1 Exhaustion (immersion) method on hot.

BL ( )
.
H2o2
BL H2o2
.
100 200 ,
300 ,
) (1:5) or ( 1:10 .
Hardness of water
(complexing) sequestering .
- 22 -
)(exhaustion
-1
( )80-70
3 ( ) Yellow
""combination

"self shade"
Red
Blue
-2 .
-3 ( Nacl Na2So4)
"electrolyte"
.
-4 : 30.
-5 5 60
5 60 .
-6 .
5
-7 50 40 ) (Ash.
-8 5 80 70
" . "
-9
fixing color at pH4-5, temp. 40 0c .
"2-Cold pad Batch " C.P.B

( ) .
To dyeing of cotton 100% or second step for blended fabrics:
A- Preparation of feeding tank from dyestuff (by calculation of
% of dyeing lab and weight of fabrics).
B- Preparation of feeding tank of fixing agent (generally NaoH
,silicate ).
- 23 -
Dye
NaoH , Silicate
) ( :
4 Dye + 1 Fixing
C- Impregnation of the well prepared fabric (hydrophility)

must be very well.
D- Uniform squeezing of the surplus liquor from the fabric by
passing through amanglenipe.
E- Packing the dyed fabric by plastic and storge it by
"rotation" for dwell time according to the affinity of dye
(chemical reaction 12 16 hours).
F- Wash-off ( to remove the unfixed dye.
G- Drying the washed fabric.
As the following scheme

Impregnation
of dry fabric
in dye bath
Wash-off
Squeezing
70-80% pickup
(o.w.f)
Rotation
- 24 -
Packing
U must be know the dewelling time (Rotation) befor washing .

On continuous machines 6 washer :
1- Cold rinse
2- Acid neutralization
3- Hot rinse
4- Soaping (90-95)
5- Hot rinse
6- Cold rinse
)unreacted(
)--(.

" "
:
Sod.hydrosulphite "Na2S2o4" is very strong reducing agent in
alkali medium.
) . )
Mechanism of the process :
Na2S2o4 + 2NaoH
2Na2So4 + 2H
Attack the unsaturated groups which responsible the color of dye
"chromomphores , auxchromes " as :
C

( Naocl)
- 25 -
E- Printing Operation
:
-1 .
-2 .
-3 .
-4 .
-5
%100 %100
.
Reactive
Disperse
Pigment
Mainely cotton
polyster
Or Co. Curing
150
washing

( )
Polyester
Cotton
Curing
180-190
Curing
101-105
Washing very wellu
* note that : quality tests before finishing .

( ).
E-Finally Finishing Operation
Finishing of textiles is the final process of chemical treatment for

textile fibres to improve a special property . e.g . softening ,
stiffening , crease resisting , waterproof , anti fire , ..

:
, , , ,

.
- 26 -

( )

4 ( ) .
4
1
2
1
3
2
4

:
( )

( )
-
A- Mechanical Finishing : is completely mechanical finishing
without addition of chemicals as
1- Emarising Machine:
: 150
30 15 15

- 27 -

30.
2- Peaching Machine:
: ( ) 900
.150 .
3- Calender Machine:
:

20 .
4- Shiring Machine :
.
5- Sengeing Machine :
.
6- Sanforizing Machine :
.
Which discovered by American " Sanford " to softening and
)adjusting of dimensional stability (shrinkage
.

- 28 -
B- chemical Finishing
Stentre .
:
% 100
%100
.
:
%100 :
12
g/l Acetic acid
)30-40 g/l Silicon soft ( macro emuls. or micro emuls.
20-30 g/l Falty acid
)60-70 g/l Resin (DMDHEU)(as anti crease
)10-12 g/l Mgcl (in organic salt as catalyst to resin
(
) 4-5

) (pick-up 70-80%

Permanent Finishing
( )( . )
3
4
5
150 170 0C
1
In put
Out put
() ( )
- 29 -
* :
)Resin (dimethy dihydroxy ethylene urea ) (DMDHEU
It used as anti crease to improve the crease recovery angel.

( )
()
dimethy dihydroxy ethylene urea
o
CH2
oH
C
N
CH2
CH2
Ho
N
+
CH2
oH
H o Cellulose
Mgcl + 170-180
Cellulose
Cellulose
CH2
C
N
CH2
CH2
Cellulose
N
CH

Hcl
( . )
* :
( - CH2 oH )
HcHo
Quality control lab.
: :

.
- 30 -
.
:
-1 ( ) Row Materials
Machines
-2
Man Power
-3
Method
-4 ( )
Measurements
-5
Environment
-6
.
1 Matching of shades :

On shade
()
Off shade
( )% 5 -1
Reprocess
-2 (Square meter weight : )
7 10 %
-3 Wedth of finished fabric:
12 %
-4 ( )Shrinkage :
12 %
5 Spirality :

6 pH pH Measurement :
.
7 Color Fastness : :
- 31 -
* Washing test
5 / 20 5 60
Gray Scale Staining gray scale .
( ) 1- 3 Refuse
( )3 -5 Pass
5 Excellent

* )Rubbing test (wet dry
10 Gray Scale
* )Perspiration test (acidic alkali
:
1
g/l NaH2Po4-2H2O
10 g/l Nacl
)0.25 g/l Histadine (Hydrochloride-monohydroate
Adjust the pH 3-4 by acetic acid
15 5 37 4
4 ( )
Gray Scale Gray scale .
1- 3 Refuse
3-5 Pass
:
1
g/l Na2HPo4-2H2O
10 g/l Nacl
)0.25 g/l Histadine (Hydrochloride-monohydroate
)Adjust the pH 9-10 by Ash ( Na2Co3
15 5 37 4
4 ( )
Gray Scale
1- 3 Refuse
3-5 Pass
8 Staining test:
- 32 -
2
2 ( ) Gray Scale
-9 Color fastness to light :

Thanks for you

Chemist / Sami Mostafa
Quality control manager
Engineering for Dyeing ,
Printing and Finishing

.... (.... )
- 33 -
:
) (: ) 1(
Procedures:
1- Take (1) mil of NaoH
which to be examined in conical(250)mil.
2- add to it (100) mil of dist water and stir it.
3- add (3) drops ph.ph
pink color.
4- Titrate with (1) N Hcl
till disappear the pink color.
1 N Hcl
1
2
100 mil dist. water

1 mil NaoH conc
Calculations:
From the relation
N V (Soda) = N\ V\ ( Hcl)
Wet gms = N eq.wet
Wet gms = N 40
) ( .
: H2O2 ) 2(
Determination of active oxygen in Hydrogen peroxide by(KMno4)
- 34 -
The reaction involved by this equation

5H2o2+2KMno4+3H2So4 2MnSo4+k2So4+5o2+8H2O
Mn+7 +5e Mn+2 ( No. of e gain is 5)
Procedures:
1- Take 100 mil diluted H2So4 (1:9) in conical.
2- add 1-2 gm from H2O2 to the conical.
3- Titrate with 0.01 N KMno4 (self indicator).
To appear the pink color
0.1 N KmnO4
1
2
Calculations:
%of H2O2 =
%of H2O2 =
100 mil dist. water

1-2 gm H2O2 conc
N V 0.017 100
W ( of sample)
V 1.7
W ( of sample)
- 35 -
( )3 : Naocl

) Na2S2O3 5 H2O ( 24.8 gm / L
0.1 N
KI -
:
0.1 N Na2S2O3 5 H2O
10 mil acetic
2 gm KI
5 mil Hypo
50 mil
4
3
2
1
v1 .
.
%1( 5)
v2 .
V= v2 + v1
:
1 mil Na2S2O3 = 0.003546 cl
gm
1 mil Na2S2O3 = 0.003723 hypo gm
200
........
.
- 36 -
............ ...
/

( )
01003365402
- 37 -

Chemical Treatmentsof Textile Fibers

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194882597.doc.

By Chemist: Samy Mostafa