TRM 2
TRM 2
2
of the staple fibre depends on its use. Staple fibre is a unit of
matter which is usually at least 100 times longer than its thick.
3
4
Fibre
6
3. Whitening agent: To resists the yellowing and to make whiter
fibre fluorescent whitening compounds (dyes) added to the
solution. This whiteness is permanent to washing and dry
cleaning.
4. Light stabilized: To make lightly resistant.
Features of Spinneret:
1. Spinneret holes are slightly wider at the entry than the exit.
2. The denier of filament extruded through a hole does not depend
upon its size, but it has some significance on the efficient
extrusion depending on melt delivery speed.
7
3. Special spinnerets are required for the production of hollow fibres
and bicomponent fibres.
4. After long use the spinnerets get checked and it is essential to
clean them.
5. The spinneret holes may be broken spotted.
Problems:
Breaking (On account of high pressure and temp)
Clogging (The holes can be blocked for solid particles mix
with polymer solution).
Remedies:
For breaking problem: the spinneret is to be changed.
For clogging: the spinneret should be cleaned after some days.
2. Spinning:
The conversion of polymer into fibre is called spinning. The fibre
forming substance is made temporarily fluid, extruded through
spinneret and then returned to solid state (by solidification) in
fibre form.
Three types of spinning process:
1. Melt spinning (Synthetic).
2. Wet spinning.
3. Dry spinning.
1. Melt spinning:
The process of spinning by which fibre or filament is produced from
melted polymer chips by extruding through spinneret continuous
filament produced here. Number of filament depends on number of
9
holes in spinneret. It is the most critical operation is the production of
nylon polyester, and polyolefin, poly propylene fibres as number of
fibre properties such as uniformity, crystallinity, and orientation are
imparted to the yarn during processing.
Melt spgn process: Synthetic polymer spgn:
I) At first the fibre forming polymer/polymer chips are fed
into a hopper then to the melter.
II) At the melter the polymer is heated over melting point.
III) The full chamber is filled by N2 or inert gas.
IV) The polymer solution is pumped to the filter to removing
impurities.
V) The polymer is then extruded through the spinneret holes.
VI) Cold air is passed over the filament to bring solid form.
VII) Then the Solid filaments are converted by converging
guide to give a slight twist.
VIII) Apply spin finish.
Requirements:
4. The polymer should not be volatile.
5. The melting point of polymer should be 30oC less than
its decomposition temp.
Advantage:
1. Can be used for both staple and continuous filament.
2. Direct and simple process.
3. No environment pollution.
4. No solvent required.
5. Non toxicity and no risk of explosion.
6. High production speed (2500 – 3000 ft/min)
7. Low investment cost.
10
Flow Chart
Feed
Melting
Metered
extrusion
Cooling &
solidification by
cold air.
Moisture
conditioning
Lubrication
Yarn driving
Packaging
Disadvantage:
1. Required more proper maintenance of the m/c.
2. For flat yarn separate stretching operation is reqd.
3. Heat of input is high.
11
Dry spinning:
In dry spgn, the fibre forming polymer dissolved in a volatile solvent
is introduced into a heated drying chamber where the solvent is
evaporated and solid fibre is obtained through spinneret. This process
is used for Acetate and some polyacrylonitrile fibre.
Dry spinning process:
1. Firstly the Solid polymer and suitable solvent is dissolved
together in a solution vessel.
2. The solution vessel is filtered and stored to a feed vessel.
3. The solution is slightly heated by a heat exchanger.
4. Then it is pumped to the filter and to spinneret at specific
rate of pressure.
5. Hot N2 gas is passed through the spgn cabinet
6. The evaporated gas is passed to the solvent recovery plant
7. Solid filament is treated to spin finish and then wound on
a suitable package.
12
Flow Chart
Feed
Metered extrusion
Solidification by solvent
Evaporation
Lubrication
Yarn driving
Packaging
Advantage:
- Suitable for producing fire denier fibres.
- No need of wash of fibre.
Disadvantage:
- Investment cost is high.
- Toxic and risk of explosion.
- Heat input is very high.
- Can not be used for staple fibre production.
Properties of solvent:
- Solvent should not be volatile.
- It should be organic.
- It should have low boiling point.
- It should be comparatively cheap.
13
- It should have low latent heat of evaporation.
- It should be thermally stabilized.
- It should be non toxic.
Wet spinning:
In wet spinning a suitable solvent is used to prepare fibre forming
solution and another coagulant is used in coagulating bath. Solution
is extruded through spinneret and in contact of coagulant cellulose is
regenerated.
Process:
Wet spinning is carried out by the following steps:
1. Dope preparation
2. Extrusion
3. Spgn
4. Stretching
5. Spin finish
6. Drying & steaming
Procedure:
I) At first solic polymer and suitable solvent is dissolved in a
solution vessel.
II) The solution is then heated in heat exchanger.
III) The solution is passed/extruded to spinneret which
immersed in a coagulation bath/spin bath by pump.
IV) The polymer is then precipeted or is chemically regenerated
and it is converted into the filament of solid form.
V) The filament is converged and wound on bobbin.
VI) The wended filament is then drawn and finally it is washed
& dried and is also wound on suitable package.
14
Flow Chart
Feed
Metered extrusion
Decomposition of soluble
Derivatives or
solvent removal
Stretch
Washing Drying
Drying Packaging
Wet spgn solvent & coagulant:
Fibre Solvent Coagulant
Viscose Alkaline water Dill H2SO4 + Na2SO4 +
ZnSO4
PVA Water Aqueous NaOH
PAN DMF/DMC + Aq DMF/DMC + 40% ZnCl2
60% ZnCl2
Advantage:
1. Suitable for staple fibre.
2. Both organic and inorganic solvent can be used.
3. Low temp reqd.
4. Higher production due to continue spgn.
15
5. Softener process.
6. Investment cost is low.
Disadvantage:
1. Slow spgn speed.
2. Washing and bleaching of fibres are needed.
3. Toxic.
Advantage:
Spgn is integrated with polymerization.
Simple solvent may be red.
Disadvantage:
Not suitable for higher denier.
Skin contains polymer of higher molecular wt. than the care.
2. Emulsion spinning:
This spun method is applied for those polymers which
have very high melting point and difficult to solubilised. PTFE poly
Tetrafluoro ethylene is produced by this method.
nCF2 = CF2 [- CF2 – CF2 -]
17
The grind polymer is dispersed in water containing a
water soluble polymer. Matrix is then spun into filament. When the
filament is sintered (heated to near Tm). Polymer particle join
together. Then the matrix polymer is removed by dissolving or
evaporating.
3. Fibrillated spinning:
Filament yarn may also be prepared by the extrusion
of a thin film which is slit or fibrillated.
Fibrillated yarns are formed when a polymer film is passed through a
line of rotary knives, usually spaced 2 – 4 mm apart. Fibrilate4d yarns
are made by stretching a narrow sheet film longitudinally until it is
highly oriented and then cracking it into thousands of fine filaments
called fibrils by stretching laterally.
Factors of spinning:
The spinning process depends on –
- Melting point of fibre.
- Decomposition temp of fibres.
When decomposition temp is higher than melting point of
fibre then fibre is spun by melt spgn.
When fibre forming polymer is decomposed (components
breakdown) at melting point then the dry spgn is used.
18
system which removes stable, weak and brittle properties of
filament.
Object:
- To increase strength.
- To reduce elongation at
break.
- To reduce creep
property.
- To increase orientation
and crystallinity.
- To remove brittleness and instability of the filament.
Drawing process:
1. Drawing unplasticized condition
2. Drawing in plasticized condition
3. Wet stretching (during wet spgn)
1. Un plasticized condition:
In cold un plasticized condition- If the Tg of fiber is about room
temperature , then no extra heat is used. At first, un drawn yarn are
19
passed between two control roller and then arranged into snubber pin
and stretched through the draw roller. In hot un plasticized
condition-A heater is used between the pin and draw roller and
heated at suitable temperature. As for example, for Polyester
(Terylene)and Acrylic the draw temperature is 800C
2. Plasticized condition:
In this process, at first the un drawn yarn is passed through the two
pair stretching roller which is taken in a plasticizing bath . Then it is
rinsed and wound in a bobbin.
3. Wet stetching:
a) Godet controlled wet stretch of nascent yarn:
In this process, the stretching is done by godet wheel directly.
Orientation effect:
1. The molecules align them-self parallel or nearly so to the
fibre axis.
2. The molecules because of their improve alignment are able
to pack themselves in a more orderly manner so that the
fibre becomes more crystalline.
3. In some cases the molecules unfolds particularly incase of
Nylon.
4. The molecule slide over each other.
22
5. As a result of the improved packing there is more
opportunity for interatomic attractive forces to be exerted
in particular hydrogen bonds.
4. Texturisation:
Textured yarn:
23
Reduce strength.
Decrease abrasion resistance.
Creates hairiness of fibre.
Process of Texturisation:
False twist method.
Stuffer box method.
Gear box method.
Knit – de knit method.
Stress – curled method.
Knife – edge crimping method.
Physical/ chemical crimping method.
Air Jet method.
25
Incase of viscose only air is passed because water (steam)
reduces strength of viscose.
5. Intermingling:
The process by which can be made the synthetic yarn smooth by
adding additives or spot welding to protrude filament ends is called
intermingling.
It is very hard and costly to twist the man made fibre. The fibres that
are composed of more that filament those are interminglinged.
26
Ways of intermingling:
I) Spot welding: Heat treatment/ Adhesive s are used.
6. Heat setting:
The process of imparting dimensional stability to fibre, yarns, fabrics
or garments with successive heating and cooling in dry and moist
conditions is called heat setting.
The different levels of heat setting may be defined as:
I) Temporary set.
II) Semi – permanent set.
III) Permanent set.
Objects:
To make the yarn, fabric, fibre dimensionally stable.
To remove shrinkage of fabric.
Disadvantage:
The fibres become very stiff.
Uneven shade due to uneven heat set.
If heat set is done after dyeing then elimination of dyes as a
result of patchiness.
27
7. Spin finish:
Spin finishes are the lubricant which provides surface lubricating,
plasticizing and static protection to man made fibre. It is applied in
fluid condition just before wind up.
Objects:
To lubricate yarn.
To reduce static electricity.
To increase the cohesion of the yarn.
To plasticize the fibre.
28
3. It must be provided with cohesiveness to the filament.
4. It should not be oxidized in the air.
5. It should give stable emulsion.
6. It should not be carcinogenic.
7. It should have good wetting property.
8. It should be non- toxic.
9. It should be cheap and easily available.
10. It should not affect dyeing or finishing process.
11. It should be chemically inert.
12. It should not object able color or odor.
8. Additives:
Additives are chemical compound which are added to fibre forming
polymer before polymerization reaction or before spgn to change the
properties of fibre and improve its performance. Additives can cot be
used when filaments come out from the spinneret.
Classification of additives:
1. Delusturing agent:
These arte used to reduce transparency increase whiteness and to
prevent undesirable lusture in the fibre Titanium oxide (TiO2) is
widely used as delusturing agent. TiO2 is a white pigment having
very fine molecules. Substances having large through the spinneret
and can not disperse well within fibre.
Its characteristics —
Chemically inert, not affected by wet processing.
Available in fine form of molecules and uniform particle size.
Resistant to sunlight.
Its in corporation reduces fibre strength.
29
2. Mass pigmentation: Pigments for mass coloration:
Addition of color pigments or certain dyes to the spgn soln or to the
resin polymer is Mass pigmentation. In this process maximum
inorganic pigments are used.
Advantage:
High evenness.
Pigment dyeing.
Chapter
2 Viscose
Viscose: Rayon
viscose is a man made, natural polymeric cellulose or regenerated
cellulose filament or staple fibre, viscose regenerated cellulose
obtained by the viscose process. The name viscose was derived from
the word ‘viscous’ which describe the liquid state of the spinning
soln. a viscose solution is as thick as honey.
31
Basic unit or monomer:
H OH CH2OH
HO H H O OH
H H
OH H
H OH
H O O H
CH2OH H OH
Regenerated fibre:
The fibre which we get by regeneration from its main origin is termed
as regenerated fibre. The regenerated fibres are divided into the
following four groups —
I) Cellulosic fibres – Viscose Rayon, cupro, modal etc.
II) Cellulosic esters – Acetate, triacetate.
III) Protein fibres – Casein, Zeir, Azlon.
IV) Miscellaneous – Alginate, Rubber.
32
Cell – ONa + CS2 Cell – O – CS – SNa
Soda cellulose Sodium cellulose xanthate
Cell – O – CS – SNa + H2SO4 Cell – OH + Na2SO4
Sodium cellulose xanthate Regenerated cellulose
So viscose rayon is a regenerated fibre.
33
bleached with hypochlorite and converted into paper boards or
sheets.
2. Steeping & Pressing:
The flat, white sheets of board contain about 90 to 94% of pure
cellulose. They are first conditioned by storing in a room at a definite
humidity and temp. This conditioning is necessary. The sheets are
then stacked vertically in the press and then soaked in a 17.5%
solution of caustic soda for 1-4 hrs. This process is known as Steeping.
Then the excess alkali is pressed put by a hydraulic ram in the press.
3. Shredding:
The shredding m/c consists of a drum inside which revolve a pair of
blades with serrated edges. The shredders are water cooled and will
take 200 lb of pressed soda cellulose at a time. In two or three hrs they
break it up into fine “Crumbs” (break into very small pieces).
4. Ageing:
After shredding, the crumbs are aged. They are contained in a
galvanized vessel with a lid and through oxidation with atmospheric
oxygen, degradative changes set in. Some depolymeriastion occurs
and the degree of polymerisation falls from about 800 to 350 in this
process. The higher the temp, the more rapidly does ageing – which is
mainly a process of depolymerisation.
5. Churning:
After ageing, the soda cellulose crumbs are introduced into rotating
air-tight hexagonal churns. About 10% of their own (crumbs) weight
of carbon disulphide is added and the crumbs and disulphide are
churned up together, a deep orange, gelatinous mass of sodium
cellulose Xanthate is formed. Churning is continued for about three
hrs, the churns rotating at about 2 rpm.
34
6. Mixing (Solution):
In the mixers the sodium cellulose xanthate is stirred with dilute
caustic soda for 4 to 5 hrs, the vessel being cooled. The xanthate
dissolves to a clear clear-brown, viscous liquid, similar in appearance
to honey this liquid is known as “Viscose” but is still too impure, too
acetated and too young to spin.
7. Ripening:
The viscose solution is stored for 4 to 5 days at 10o-18oC and during
storage it ripens.
During the ripening the viscosity at first falls and then rises, so that
by the time the solution is ready to spin. The test which is available to
determine when viscose is ripe enough to be spun is as given below -
Acetic acid test: Before it is ripe the viscose solution will dissolve in
40% acetic acid but when it is ripe the viscose will precipitate in this
acid.
8. Spinning:
35
1. Selection of main
viscose feed.
2. Pump
3. Candle filter
4. Glass rounder end
5. Coagulating bath
6. Selection of acid
replenishing
pipe
7. Spinneret
8. Bottom godet
9. Top godet
10. Funnel
11. Topham Box
12. Drive for topham box
13. Traverse
14. Fresh air Inlet
15. Fumes sucked out
16. Sliding windows
17. Cake
Ripen viscose soln extruded through the spinneret mostly made of platinum alloys. The jet of
viscose enters a co-agulating bath containing the followed composition of mixture-
Sulphuric acid 4-12 parts by weight.
Sodium sulphate 1 0-22 parts by weight.
Zinc sulphate 1-5 parts by weight.
The operation in co-agulating bath follows two routes to convert
regenerated cellulose.
Fast route:
Sodium cellulose Xanthate
Regenerated cellolose
37
Slow route:
Sodium cellulose Xanthate
Regenerated cellolose
The topham box: This is the take up device for cake spun viscose rayon.
9. Purification:
The yarn collected in the Topham Box is impure and relatively weak, it has to be purified.
Purification consists of 4- operation –
I) Washing
II) Desulphurising, a process which is sometimes called sulphiding.
III) Bleaching
IV) Washing.
The first wash is with water, the second is with Sodium sulphide solution to remove Sulphur
and possibly compounds of Sulphur residual from the Xanthate. The yarn is still not quite
white, so it is not treated with a slightly alkaline solution of a sodium hypochlorite to bleach it.
This is followed by a wash with dilute hydrochloric acid and a final wash with water. The cakes
are then dried.
Spinning process:
1. Discontinuous: a) Pot/cake spgn
b) Bobbin spgn
2. Continuous: a) Nelson spgn
b) The industrial rayon corporation of America process.
38
Preparation of wood pulp
Shredding
(In two or three hours, formation “Crumbs”)
Ageing
(In atmospheric oxygen, D.P. falls from 800 – 350)
Churning
(Xanthation or Sulphidising)
Mixing
(Solution)
Drying
39
Recipe Reaction
Temperature - 40o-55oC
Chemical properties:
1. Effect of acid:
40
Acids like Suphoric acid, Hydrochloric acid etc. break down the cellulose macromolecules of
viscose rayon and produce hydrocellulose. Cold acid solutions for short time do not attack
viscose rayon. Even acids like euphoric, hydrochloric and nitric acid can be used in surprisingly
strong concentrations, if the temp is not high. (Viscose rayon is attacked by hot dilute or cold
concentrated mineral acids which weaken and disintegrate the fibre).
2. Effect of alkali:
Concentrated alkali will cause swelling and reduce strength. But weak alkali does not damage
viscose.
3. Effect of solvent: Good resistance to organic solvent.s
4. Effect of bleaching:
Viscose rayon can withstand both oxidizing and reducing bleaches. Attacks by strong oxidizing
bleaches.
5. Biological agents: Action of microorganism:
Microorganisms like moulds, mildew, bacteria etc. affect the color, strength, dyeing property
and lusture of rayon. Clean and dry viscose rayon is rarely attacked by moulds and mildew.
6. Action of light:
Prolonged exposure to sunlight weakens viscose rayon. This weakening is due to moisture and
Ultra Violet light of the sunlight and % loss of strength or exposure to Ultra Violet light.
7. Action of heat:
Long exposure to high temp yellows viscose rayon. At 3000F (1500C) or more, viscose rayon
loses its strength and begins to decompose at 3500 -4000F.
8. Dye ability:
Better affinity for dyes than cotton. Applied dyes – Vat, Direct, Sulphure.
9. Conductivity: Good conductor of heat.
10. Flammability: Burns rapidly.
High Tenacity viscose rayon: Research of the spinning of rayon has been intensive and
unceasing. Every aspect of viscose production and spinning has been studied and increased
understanding of the factors involved has made possible the production of rayons with
characteristics that are suited to particular application. The most important of these are the high
tenacity rayon.
The name of some high tenacity viscose rayons are –
I) Tenasco
II) Cordura
III) Durafil
IV) Forfisan
41
1) Retaining a higher than usual degree of polymerization in the cellulose.
2) Better filtration more frequent change of filter cloth.
3) Stretching the fibre before it is set, usually as much as 150% as maximum stretch.
4) The presence of more zinc than usual in the coagulating bath. The high concentration
of zinc ions causes coagulation of the xanthate on the skin and this delays
regeneration of the cellulose. So giving time for the stretching to be carried out.
5) Because color and dye ability are unimportant in type yarn, removal of sulphur from
the yarn is unnecessary in fact, it the sulphur is left in it may help the bonding of
fibre to rubber.
6) Use modifiers in spun bath.
7) Two spgn bath twice.
Properties:
1. Tenacity: 1.7-2.3 g/d (dry), 1.1-1.35 g/d (wet)
2. Elongation at break: 10-19% (dry), 17-33% (wet)
3. D.P.: 500
4. Cross section: Round
5. Recovery from stretch: Good
6. MR%: 11%
2. Polynosic:
Polynosic or modal regenerated cellulose obtained by process giving a high tenacity and high
wet modulus.
In other words, Polynosic is a regenerated cellulose fibre which, when wet remains stronger and
distorts less than either Cuprammonium or Viscose. Polynosic means many fibrils, whilst
modal is derived from modules. The Intl. Organization for standardization prefers the name
modal.
Properties:
1. Tenacity: 3.9 g/d (dry), 2.9 g/d (wet)
2. Elongation at break: 11% (dry), 13 %(wet)
3. D.P.: 450-500
42
4. Cross section: Round
5. Recovery from stretch: Good
6. MR%: 11.8%
3. Tancel:
General name is Lyocel. Tancel is solvent spun cellulosic fibre of new generic class produce a
clear viscose solution which is treated and spun into a bath contain dilute solution of the
solvent. Tencel is the best fibre among regenerated cellulose fibres. The fibre is called CF0001 in
USA.
Properties:
1. Tenacity: 3.5 (dry), 2.5 (wet)
2. Elongation: 11.8%
3. X-section: Round
4. Specific gravity: 1.56
5. MR%: 11.5
4. Viscose:
Differentiate between three generated fibers:
Topic Viscose rayon Polynosic Cupro Cotton
1. Tenacity 1.5-2.4 (dry) 3.9 (dry) 1.7-2.3 (dry) 3.2 (dry)
0.7-1.2 (wet) 2.9 (wet) 1.1-1.35 (wet) 3.5 (wet)
15-30% (dry) 10-19% (dry)
20-35% (wet) 17-33% (wet)
2. Elongation at break 250-300 11% (dry) 500 9%
13% (wet)
Serrated Round
3. D.P.
Poor 450-500 Good 5000
4. Cross section
Round Flat/kidney
5. Recovery from stretch 13% 11% shaped.
Good Good
6. MR%
11.8% 8.5%
Blending process:
This solution of Na- cellulose xanthate cellulose is blends in a big horizontal mixer to balance
any irregularity and to get more uniform quality of final product. Removal of air from is carried
out in an air tight vessel by applying vacuums.
Viscose is blends: because —
It is not fully synthetic.
43
Its cost lower than natural fibre.
By blending fibre HSO, we can improve absorbency of lower absorbent fibre such as polyester.
Special viscose:
Evlan: Evlan is viscose rayon staple fibre used by the carpet trade. It has a smoother cross-
section than standard viscose. It has a higher crimp usual. It has a higher strength than usual
and this gives durability. Evlan has been widely used since its introduction in 1962. Evlan is
used for Carpets.
Topel: This fibre is an x-section cellulosic fibre. It has much less affinity for water, in which it
swells only very little. It has good resistance to caustic alkali, a properly useful in package
dyeing. It is used for blending with cotton for better appearance, handle and drape.
Chapter
3 The Ester–
Cellulose Fibre
Acetate fibre:
Textile fibres which are composed of ester cellulose are called acetate fibres.
44
The generic terms acetate and tri acetate were adopted by the FTC for acetate fibre definition —
Acetate is a manufactured fibre in which the fibre forming substance is cellulose acetate. Where
not less than 92% of the hydroxyl groups are acetylated the term tri acetated may be used as a
generic description of the fibre.
The term acetate is derived from acet and ate. The former comes from acetic acid (The acid of
vinegar), whilst the latter denotes a chemical salt. Acetate means a salt of acetic acid. In organic
chemistry, a salt is known as an ester. As a result acetate fibres are at times referred to as
cellulose ester. There are two types of acetate fibres —
I) Acetate
II) Triacetate
I) Tri acetate:
Tri acetate is a man made, natural polymer based, primary cellulose acetate filament or staple
fibre. It is formed by the fully acetylation of purified cotton linters with acetic acid and
anhydride. Six acetate groups are formed in each glucose unit, in six –OH groups.
H COOCH3 CH2OOCCH3
O H H O O
COOCH3H H
H COOCH3H H
H
O O H
H
CH2OOCCH3 H COOCH3
n
n = 225
II) Acetate:
Acetate is a man made, natural polymer based, secondary cellulose acetate filament or staple
fibre. To obtain acetate or secondary cellulose acetate fibre, triacetate is hydrolyzed, i.e. reacted
with water so that only 2.3 to 2.4 acetyl groups are present per glucose unit.
H COOCH3 CH2OOCCH3
O H H O
O
H H
OH H
H OH
H
O H H
O
H
CH2OOCCH3 H COOCH3
n
n = 130
The Polymer System:
Both the acetate and triacetate polymers are cellulose polymers whose –OH groups have been
acetylated to form the ester of acetic acid or acetate. In the manufacture of ester cellulose fibres,
tri acetate is produced first; hence it is also known as primary cellulose acetate fibre. It is meant
45
to be fully acetylated, that is in the place of the six –OH groups of the cellubiose unit, six acetate
groups (—OCOCH3) are formed.
H COOCH
3 CH2OOCCH
3
O H H O
O
H H
COOCH
3
H 3H
COOCH
H O H
O H
H
CH2OOCCH
3 H COOCH
3
n
Fig: The chemical formula of the repeating unit of the triacetate.
Degree of polyn, n = 225
To obtain the secondary cellulose acetate fibre, the primary cellulose acetate is hydrolyzed, that
is reacted with water, so that only 2.3 to 2.4 acetyl or acetate groups per glucose unit occur.
H COOCH3 CH2OOCCH3
O H H O O
H H
OH H
H OH
H H
o O H
H
CH2OOCCH3 H COOCH3 n
Fig: The chemical formula of the repeating unit of
secondary cellulose acetate.
Degree of polyn, n = 130
Both acetate and triacetate fibres are very amorphous fibres. The polymer system of both types
of acetate fibres are held together mainly by Vander Waal’s forces. Some hydrogen bonds
contribute towards inter polymer cohesion in the polymer system of the secondary cellulose
acetate fibres.
The acetate or secondary cellulose acetate polymer is about 160 nm long and about 2.3 nm thick,
whilst the triacetate or primary cellulose acetate polymer is about 240 nm long and 2.6 nm thick.
46
for triacetate, 90% methylene chloride + 10% ethanol
8. Spinning: Acetone, methylene chloride.
H OH CH 2OH
HO H H O O
H H H
OH H
OH
n H
O O H
Acetylation
H
CH 2OH H OH
H COOCH 3 CH 2OOCCH 3
O H H O O
H H
COOCH 3 H
H COOCH 3
O O H
H
CH 2OOCCH 3 H COOCH 3
n
Triacetate n=225.
Acetate:
Triacetate is hydrolyzed, that is reacted with water, only 2.3 to 2.4 acetyl or acetate groups per
glucose unit occur.
H COOCH3 CH2OOCCH3
O H H O O
H H
COOCH3
H COOCH3 H
O O H
H
CH2OOCCH3 H Hydrolysis
COOCH3 n
H COOCH 3 CH 2OOCCH 3
O H H O O
H H
OH H
H OH
O O H
H
CH 2 OOCCH 3 H COOCH 3
n
Acetate n=130
47
The cotton linters are purified by kier boiling for 4-10 hrs with alkali soln of Na2CO3 then they
are bleached with NaOCl. Then the linters washed and dried.
II) Activation:
In this stage, the purified cotton linters or wool pulp are steeped in glacial acetic acid (3:1) at
room temperature for easy acetylation. To swell the fibre and to increase their chemical
reactivity.
III) Acetylation:
a) Non – solvent: Esterification is done by anhydride in presence of catalytic H2SO4.
b) Solvent: The typical recipe of solvent process
- 100 lbs purified cellulose
- 300 lbs acetic anhydride
- 500 lbs glacial acetic acid
- 8-10 lbs H2SO4
Then the mixture is kept at a temp of 25o-30oC for 8-10 hrs. After acetylation a thick clear soln of
primary cellulose acetate or triacetate is obtained.
IV) Hydrolysis:
Hydrolyze acetylated cellulose is performed by H2O presence of 95% acetic acid, for 15-20 hrs
at a high temp of 40o-50oC. Thus an acetone soluble product is obtained.
R-Cell-OOCCH3 +
H2O R-Cell-OH + CH 3COOH
CH 3CO
O + H20 2CH3COOH
CH 3CO
V) Precipitation:
After hydrolysis, for destroying catalytic H2SO4. Na/Mg/Ca acetate is added.
CH3COONa +H2SO4→NaSO4 +CH3COOH
Then dilute aqueous acetic acid is added and hence acetate is precipitated.
VI) Washing and drying:
In this step, acetate is washed and centrifuged so that the amount of water is not exceeding 20%,
then dried.
VII) Blending:
Before dry spgn blending is performed —
To control product quality.
To decrease cost.
VIII) Dope preparation:
48
For acetate:— By dissolving acetate in the solvent of 85% acetone and 15% ethanol, spgn soln is
prepared. In this time, pigment and dellustrants etc are added.
For tri acetate: — Dope is prepared by dissolving primary cellulose acetate in 90% methylene
chloride + 10% ethanol.
IX) Spinning:
Dry spinning process is applied for acetate, tri acetate spinning Acetone and methylene chloride
used as solvent.
49
Blending : To control product quality & to decrease cost.
↓
Dope preparation : For acetate; 85% acetone + 15% ethanol.
↓ For triacetate; 90% methylene chloride+ 10%
ethanol.
Dry spinning : For manufacturing acetate, triacetate.
Physical properties:
1. Tenacity:
Both types of acetate fibres are weak due to the amorphous nature of their polymer systems,
which limits the number of inter polymer forces of attraction which can occur.
Acetate and triacetate become weaker when wet. This is because water molecules enter the
amorphous regions of the fibres polymer systems. The fibre polymers move further apart, the
cohesive effect of the Vander Waal’s forces is sufficiently reduced to cause a loss in tenacity of
the filament or staple fibre.
Tenacity of acetate fibre 1.1-1.3 gm/den when dry and 0.65-075 gm/den when wet and
For triacetate fibre 1.2-1.4 gm/den when dry and 0.7-0.8 gm/den when wet.
2. Elastic – plastic nature:
Both acetate and triacetate are plastic because of their amorphous polymer systems.
Both acetate and triacetate fibres become more plastic when wet as sufficient water molecules
can enter their amorphous polymer systems to break a significant number of inter polymer
forces of attraction.
3. Elongation:
For acetate fibre 23-30% (standard) when dry and 35-45% when wet and
For triacetate fibre 25-30% when dry and 30-40% when wet.
4. Hygroscopic nature:
Despite their very amorphous polymer system, both acetate and triacetate fibres have only a
fair of moisture absorbency because of the relatively low polarity of the acetate and triacetate
polymers.
Standard moisture regain of acetate fibre is about 6.5% and
For triacetate, regain before heat treatment 4.5%, after treatment 2.5-3.0%.
5. Specific gravity:
Specific gravity for acetate fibre is 1.30 and
For triacetate fibre 1.32.
Thermal properties:
Acetate:
50
It is thermoplastic mtls.
It becomes sticky at 1900C.
It becomes soft at 2050C.
It melts about 2320C.
It is not readily flammable.
Exposed to a naked flame cause melt and burn.
Triacetate:
It is thermo plastic.
Heat treatment of triacetate increases the crystallinity and molecular orientation.
It’s softening point 2250C.
Melting point 3000C.
Triacetate melts and shrivels to a molten bad when ignition.
Chemical properties:
1. Acid:
Acids hydrolyze both type of acetate, causing polymer degradation and resulting in weakening
and eventual destruction of their textile mtls.
Dilute solutions of weak acids do not affect acetate, but the fibres are decomposes by strong
acids in concentrated solution.
Triacetate is resistant to dilute acids but is attacked by strong acids in high concentration.
2. Alkali:
Alkaline hydrolysis occurs on the surface of the filaments resulting in the yellowing of white or
the dulling of colored acetate and triacetate textile mtls.
For acetate, Alkali up to 9.5 — little effected.
Strong alkali — causes saponification and cell-acetate
changed to regenerated cellulose.
For triacetate, dilute alkali — greater resistance
hot strong alkali — attacked and hydrolyzed.
3. Bleaches:
Acetate is attacked by strong oxidizing agents, but is not affected by normal bleaching
solutions of hypochlorite or peroxide .
Triacetate is not affected significantly by common bleaching agents including hypoclorites,
chlorites, per acetic acid and hydrogen peroxide.
4. Organic solvent:
Acetate swells or dissolves in many solvents including acetones and other Ketones, Phenol,
Chloroform etc. and insoluble in petroleum chemicals.
51
Triacetate dissolves in Methylene chloride, Chloroform, Formic acid and swelled by Acetone,
Ethylene chloride and Trichloro ethylene and not affected by Benzene, Toluene, Xylene.
5. Color fastness:
The acetate fibres are not easy fibres to dye or print. The disperse dyes, which are the only dyes
which will readilydye or print. Acetate or triacetate textile materials had to be specially
developed.
6. Light:
For acetate deterioration after prolonged exposure, resulting in some loss of strength, the color
remains good. Retention of tenacity is improved by certain colored pigments.
But triacetate is highly resistant on exposure to severe outdoor weathering there is little loss in
strength and no yellowing.
7. Heat:
For acetate, after a week at 120oC, it remains much of its original tensile strength.
In triacetate after two weeks exposure at 130oC, triacetate retained 68% of its strength.
Biological properties:
1. Insects:
Moths and other insects do not normally attack acetate.
Triacetate is not attacked by moths or most topical insects or larvae which commonly attack
textile fibres.
2. Micro organisms:
Fungi and bacteria may cause surfaces damage and discoloration bet resistance is greatly high.
Triacetate is highly resistant to attack by micro organisms.
Electrical properties:
Excellent insulator in case of acetate. The electrical resistance
of triacetate is very high.
52
4. Specific gravity 1.5 4. Specific gravity 1.30
5. D.P. 250-300 5. D.P. 130
H OH CH 2OH H COOCH 3 CH 2 OOCCH 3
O H H O O O H H O O
H H H H
OH OH H
H OH H H OH
O O H
O O H
H H
CH 2OH H OH CH 2 OOCCH 3 H COOCH 3
6. n 6. n
O H H O O O H H O O
H H H H
COOCH3 OH
H COOCH3 H H OH H
O O H
O O H
H H
CH2OOCCH3 H COOCH3 CH2OOCCH3 H COOCH3
n n
53
13. Melting
300oC 232oC
point
Chemically:
14. Acid Dilute acid — resistant Dilute acid — not affected
Strong acid — attacked Strong acid — decomposed
15. Alkali Alkali up to pH 9.5 — little
Dilute alkali — greater resistance affected
Strong alkali — attacked and Strong acid — causes
hydrolyzed. saponification, cell acetate change
to regenerated cellulose.
16. Bleaches Not effected significantly by
Attacked by strong oxidizing
common bleaching agents such as
agents.
hypochlorite.
17. Heat After two weeks exposure at
After a weak at 120oC it remains
130oC, triacetate remain 68% of its
much of its original strength.
strength.
18. Organic Dissolved in methylene chloride, Swells or dissolves in chloroform
solvents chloroform. acetones.
19. Primary cellulose will remain a
Acetate can not be heat set
heat set more satisfactory than
satisfactory.
acetate.
20.Fabric Fabrics are dimensional higher
than acetate.
21. Crisper hand than acetate.
22. More expensive Less expensive
54
End use of triacetate fibre:
Many warp knitted fabrics and garments.
Ladies dress goods.
Blended with wool & acetate for making suiting.
In staple fibre form triacetate is blended with wool nylon and viscose. High bulk tricel is
used in knitwear.
Table cloths.
Chapter
4 Polyester
Polyester:
The word “ester” is the name given to salts formed from the reaction between an alcohol and
acid. “Polyester” means many organic salts. Polyester is a man made, synthetic polymer,
polyester filament or staple fibre. The most commonly polyester apparel filament or staple fibre
is usually composed of Polyethylene Terephthalate polymers. Definition of polyester according
to F.T.C-.
Polyester fibre are chemically composed of at least 85% by wt. of an ester of a
substituted aromatic carboxylic acid, including but not restricted to substituted Terephthalate
units and Para substituted hydroxybenzoate units.
Polyethylene Terephthalate, the repeating unit of the polyester polymer with a degree of
polymerisation of 115-140 units (i.e. n= 115-140).
COO C
H2
O C
Manufacturing process:
1. Continuous process of PET:
Raw mtls:
The main raw mtls required for the manufacture of polyester fibre are P-xylene, ethylene glycol
and methanol.
1) Terephthalic acid or D.M.T:
55
Terephthalic acid is made by oxidizing P- xylene with air and nitric acid.
CH 3 CH 3 COOH
Air
HNO 3
CH 3 COOH COOH
Terephthalic acid is esterified with methyl alcohol to form Dimethyl terephthalate (DMT).
COOH COOCH 3
CH 3OH
COOH COOCH 3
2) Ethylene glycol:
Ethylene glycol is made by catalytic oxidation of ethylene.
CH2 [O] H2C CH2 H2O H2C OH
CH2 O H2C OH
Ethylene oxide Ethylene glycol
Polymerization:
PET is produced by condensing ethylene glycol with Terephthalic acid or Dimethyl
terephthalate.
Condensation of ethylene glycol with TPA is an esterification reaction, water being eliminated
as the reaction takes place.
Condensation of Ethylene Glycol with DMT is an ester interchange reaction, methyl alcohol
eliminated as the reaction takes place.
In either case, the condensation is carried out by heating the ethylene glycol and Terephthalic
acid and removing the water or methyl alcohol in Vacuo. When the desired degree of
polymerisation has been reached, colorless polyester is extruded through a slot on to a casting
wheel. The polymer solidifies into an endless ribbon which is fed to cutter and cut into chips in
1 1
the form of cubes with inches sides. The chips are dispatched to the spgn room via a
8 4
suction pipe.
Spinning:
PET melts at about 2600C, and the molten polymer is stable. In
56
spinning, the chips of polymer are dried to remove moisture and then passed to storage
hoppers. From the hoppers the chips are fed as required to the spinning m/cs. In spinning, the
molten polymer from hopper is pumped through holes in a spinneret. Then filaments emerge
and solidify and are wound into packages of undrawn yarn. The undrawn yarn is stretched to
about 5 times its original length on draw-twist m/cs then the drawn filament is wound.
In case of staple fibre production, the filaments from spinning head are passed through draw
rollers, and the crimped mechanically and the crimp is set in the fibre by heat treatment. The
tow is then cut into staple of the desired length.
Reaction in polymerization of PET polyester:
COOH
H2C OH Polymerisation
n +n HO OC COO-(CH2)2-O H + (2n-1) H2O
H2C OH
n
COOH
PET
Terephthalic acid
57
COOCH3
CH2OH
Polyn
n +n CH3O co COO(CH2)2O H
CH20H n
PET
COOCH3
+ (2n-1)CH3OH
2. Batch process:
The raw mtls required for the manufacturing of polyester fibres are Dimethyl Terephthalate
and Ethylene glycol.
1. Terephthalic acid is esterified with methyl alcohol to form DMT.
COOH COOCH3
+ CH3OH + H2O
COOH COOCH3
CH2 H2C OH
O
58
1) Ester interchange reaction is occurred by mixing DMT with excess EG with catalyst (0-1.4%)
by heating of temp of 130-250oC and removing CH3OH.
COOCH3
H2 H2
H2C OH
+H C HO C C OOC COO C C OH + CH OH
3
OH H2 H2
2
COOCH3
2) Polycondensation reaction,
Polyn O
HO (CH2)2 OOC COO (CH2)2 HO CH3O C COO (CH2)2O H
By collecting polymer of chips with pressure 0.1 mm Hg. Polymer are kept spinneret for
spinning.
DEG
and from this there occur in the polyester a few (1-3%) groups such as:
59
OCH2CH2OCH2CH2OO CO
R R
Modified polyester
II) By sulpho isophthalic acid:
60
For modification, sulpho isophthalic acid is used as following,
HOOC COOH
H2C OH
HOOC COOH + +
H2C OH
HO3S
O
C OOC (CH2)2 COO OOC (CH2)2 O
HO3S
O
C OOC (CH2)2 COO OOC (CH2)2 O
Types of polyester:
Polyesters are subdivided into the following types, based upon their chemical structures and
abbreviations shown are used in referring to the fibres:
1) Polyethylene Terephthalate fibre (PET polyester)
2) Poly- 1,4- cyclo hexylene Dimethylene Terephthalate fibres (PCDT polyester fibres)
3) Other types of polyester fibres.
1. PET polyester:
PET is made by the condensation of Terephthalic acid or a derivative such as dimethyl
terephthalate with ethylene glycol.
61
COOH COOCH3
+ CH3OH + H2O
COOH COOCH3
COOCH3
H2
H2C OH
COO C C OH
+H C 2 OH
HO (CH2)2 OOC
H2
Diethylene Glycol Terephthalate
COOCH3
PET
2. PCDT:
PCDT polyester fibres are spun from poly -1,4- cyclo hexylene dimethylene terephthalate made
by condensing Terephthalic acid with 1,4- cyclo hexane dimethanol,
H2 H2
C C
HOOC COOH + HOH2C CH
CH CH2OH
CH2 C
H2
1,4-Cyclo hexane dimethanol
H2 H2
C C
O CH2 CH
CH C COO CO
H2 n
C C
H2 H2
PCDT
3. Special type of polyester fibre:
Dacron:
The fibres are made by the polymerisation of Terephthalic acid and ethylene glycol.
OH OC COO(CH2)2O H + (2n-1)H2O
n
Dacron
Terylene: Terylene is made by polymerizing the dimethyl terephthalate and ethylene glycol.
62
COOCH 3
H 2C OH
+ n
H 2C OH
COOCH 3
H2
H3CO C
O
COOC C
H2
O H
+ (2n-1)CH3OH
n
Terelene
Kodel: It is polymerization of 1,4- cyclo hexane dimethanol and terephthalic acid.
H2 H2
C C
HOOC COOH + HOH2C CH
CH CH2OH
CH2 C
H2 H2
H2
C C
H2
H O CH2 CH
CH C COO CO OH
C C
H2 H2
Kodel
n
+ 2nH2O
Polymer system:
63
The polyester polymer is linear and is usually based on Polyethylene Terephthalate. The degree
of polymerisation range from about 115 to 140 resulting in a polymer length of about 120 nm to
150 nm with a thickness of about of 0.6 nm.
The important chemical groups in the polyester polymer are the methylene groups (-CH2-), the
slightly polar carbonyl groups (-CO-), and the ester groups (-OCO-). As the polarity of the
polyester polymer is only slight, it is considered to be held together mainly be Vander Waal’s
forces and a lesser extent some very weak hydrogen bonds. The polymer system is estimated to
be about 65-85% crystalline and about 35-15% amorphous. This is supported by the
hydrophobic nature, poor dye ability, but good overall chemical resistance of polyester
filaments or staple fibres.
O O O O O
C C O (CH2)2 O C C O (CH2)2 O C C O
O n
ester group ethylene glycol terephthalate unit
Fig: A section of polyester polymer.
It is thought that the carbonyl oxygen of the ester group gives rise to very weak hydrogen
bonds with the relatively non polar hydrogen atoms in the methylene groups of adjacent
polymers. The degree of polyn, n, is about 115-140.
Monomer of polyester:
Monomer Polymer
1. The monomer of most Polyethylene terephthalate
common polyester are ethylene O
glycol O C COO (CH2)2
H2C OH n
H2C OH
and Terephthalic acid
COOH
COOH
1,4 cyclo hexane dimethanol
2. 1,4 cyclo hexane dimethanol Poly-1,4- cyclohexylene-Di methylene
Terephthalate (PCDT polyester)
H2 H2 H2 H2
C C
C C
HOH2C CH
CH CH2OH
O CH2 CH COO CO
CH2 C CH C
H2 H2
C C
and Terephthalic acid H2 H2 n
64
COOH
COOH
Physical properties:
1. Tenacity:
Polyester filaments and staple fibres are strong to very strong because of their extremely
crystalline polymer system. The tenacity of polyester filaments or staple fibres remains
unaltered when wet because of the completely hydrophobic and extremely crystalline polymer
system.
High tenacity filament 7-8 gm/den.
Normal tenacity filament 4.5-5.0”
Staple fibre 3.5-4.0”
2. Elastic plastic nature:
Polyester filaments or staple fibre are about as plastic as they elastic as can be seen from their
distortion on repeated stretching and straining. This is entirely due to the Vander Waal’s forces
which holed the polyester polymer system together. Breaking extension 20-30% and Elastic
recovery 97-100% incase of 2% extension.
3. Hygroscopic nature:
Polyester filaments and staple fibre are hydrophobic. The lack of polarity and the extremely
crystalline structure of polyester polymers resist the entry of water molecules into the polymer
system.
MR% - 0-0.4%.
4. Specific gravity:
Dacron 1.38 and Kodel 1.22.
Chemical properties:
1. Effect of acid:
The ester groups of the polyester polymers are resistant to acid hydrolysis. This resistance is
further enhanced by the extreme crystallinity of the polyester polymer system which prevents
the entry of any acid and water molecules into the filament of staple fibre.
2. Effect of alkali:
Alkaline conditions as encountered during laundering may hydrolyze the polyester polymers at
their ester groups. The extreme crystallinity of the polyester polymer restricts the hydrolysis to
the surface of the polyester filament or staple fibre.
3. Effect of bleaches:
65
Normally polyester textile mtls do not need to be bleached. If bleaching is required this is
affected using Sodium Chlorite.
4. Sunlight:
The acid resistance of polyesters helps protect polyester textile mtls from the slightly acidic
conditions that occur in polluted atmospheres. The benzene rings of the polyester polymer
provide stability to the whole polymer, enabling the polymers to withstand the detrimental
effect of the sun’s ultra violet radiation.
5. Dye ability:
It is very difficult for dye molecules to penetrate the extremely crystalline polymer system of
polyester fibres. Only the relatibely small molecules of disperse dyes are used to dye or print
polyester fibres.
6. Biological agents:
Resistance to moths, mildews, fungus.
7. Solvents:
Resistant to all dry cleaning solvents.
8. Flammability:
Burn slowly.
Thermal properties:
Thermo plasticity:
‘Thermo plasticity’ means capable of being shaped or moulded when heated. Thermoplastic
fibres heated under strictly controlled temperatures soften and can then be made to conform to
a flat, creased or pleated configuration. When cooled, thermoplastic fibres will retain the
desired configuration that is remain flat, pleated or creased.
Polyester textile mtls can be permanently heated. Textile fibres classed as thermoplastic are
acetate, triacetate, acrylic, nylon and polyester. Polyesters retain a heat set permanently where
as acetate fibres do not hold a set as satisfactory.
66
High tenacity PET for tire cords, v-belt, ropes, fire hoses, sail cloth, conveyor belts, paper
making.
67
Chapter
5 Polyamide
Polyamide fibre: Fibre
Polyamides are polymers which contain recurring amide groups as integral parts of the main
polymer chain.
Synthetic polyamides are made by a condensation reaction taking place between small
molecules in which the linkage of molecules occurs through the formation of amide groups.
Types of polyamide —
I) Nylon
II) Aramide
Aramide :
Aramide is a long chain synthetic polymer in which at least 85% of amide linkages are directly
attached to two aromatic rings of a long chain synthetic polyamide.
Classification:
1. Kevler —
a) Kevler - 2g: — as filament.
— Used in parachute.
b) Kevler – 4g: — as filament and spun.
— Used for boat making.
2. Nomex —
As filament as spun
Nomex 430 Nomex 450
Nomex 431 Nomex 451
Nomex 432 Nomex 452
Nomex 433 Nomex 453
Nomex 434
Nylon:
Nylon was the first man made organic textile fibre made wholly from raw materials from the
mineral kingdom. Nylon is a manufactured fibre in which the fibre forming substance is any
long chain, synthetic polyamide having recurring amide groups (-CO-NH-) as an integral part
of the molecular chain.
There are different types of nylon —
Nylon-6, Nylon-6,6, Nylon-6,10, Nylon-11, Nylon-7, Nylon 9.
Nylon polymer:
Nylon is a linear polyamide polymer. The nylon 6,6 polymers has a linear but zig zag
arrangement of carbon atoms. The carbon atom can bear four single covalent bonds which are
68
arranged about the atom as the verticles of a triangular pyramid i.e. a tetrahedron. This
tetrahedral arrangement of bonds causes the carbon atoms to form a zig zag but linear polymer.
This polymer configuration is partly responsible for the very good elastic properties of nylon.
The polymer system of nylon is estimated to be about 65-85% crystalline and correspondingly,
about 35-15% amorphous. This gives nylon a very crystalline, very well aligned or oriented
polymer system. With the inter polymer distances on average about 0.3 nm.
Chemistry involved:
I) Nylon 6,6:
Nylon 6,6 fibres is spun from Poly Hexa Methylene Adipamide, a polyamide made by the
condensation of Hexa Methylene Diamine and adipic acid.
NH2-(CH2)6-NH2 + HOOC-(CH2)4-COOH
Hexa methylene Adipic acid
Di amine
-CONH(CH2)6-NHCO-(CH2)4-CONH-(CH2)6-NHCO-(CH2)4-CO-Nylon 6,6
-NH(CH2)6-CONH-(CH2)6-CO-
Nylon 6,10
V) Nylon 7:
69
NH2(CH2)6-COOH -NH-(CH2)6-CONH-(CH2)6CO-
Amino Heptanoic acid Nylon 7
Raw materials for production of:
1. Nylon 6 : 6 amino caproic acid / caprolactam.
2. Nylon 6,6 : Hexa-methylene diamine and adipic acid.
3. Nylon 6,10 : Hexa-methylene diamine and sebasic acid.
4. Nylon 11 : 11-Amino undecanoic acid.
5. Nylon 7 : Amino Heptanoic acid.
NH
(HOOC (CH2)4COOH). CO
CH2
CH2
70
They are evaporated at a temp of 1050-1150C over a period of 20-30 min until a solid
content fo 60-75% is reached .
They are then passed through a high pressure reactor at 240-260 psig with a temp of
235oC, residence time is 2 hrs. At this stage, the nylon salt solution is converted to a pre
polymer. Pressure is released at a temp of 260o-290oC in a flasher.
The polymer is pumped to a finisher, a thin film evaporator. The nylon 6,6 is maintained
at temp of 2600-2900C for a period of 5-10 min in a finisher and is discharged from this
unit when the desired viscosity is reached for spinning into fibres.
Chemical reaction:
NH2(CH2)6NH2 + HOOC-(CH2)4-COOH
-CONH(CH2)6-CONH-(CH2)4CO-
Nylon 6,6
40-50% Solid
110o-115oC
240-260 PSIG
230oc
Residence
Dowtherm in
Time 2 hrs Reactor Dowtherm out
Condensator
250o-290oC Dowtherm in
Flasher Dowtherm out
71
Light charge
280o-290oc
Residence
Time 5-10min
Flasher
[o] HNO3
HOOC(CH2)4COOH
Adipic acid Oxidation
Reduction
NH2(CH2)6-NH2
Hexamethylene diamine Ni catalyst
Nylon salt:
By reacting adipic acid and hexa methylene diamine in the soln of methyl alcohol, we get nylon
salt. This salt is separated and purified at this stage.
H2N(CH2)6NH2 + HOOC(CH2)4-COOH
Hexamethylene Adipic acid
diamine
72
+ -
H2N(CH2)6-NH3 - OOC-(CH2)4-COOH
Nylon 6,6 salt
Manufacturing of nylon 6:
Raw materials:
Caprolactam is the main raw materials of Nylon 6 which is obtained from Coal-tar.
Continuous process:
The VK top has a dephlegmator which refluxes back Caprolactam and allow water to
evaporate off.
Water fed to VK tube is about 1-5% of total Caprolactam. The water fed serves as a
carrier for delustrants and boils off instantaneously after being fed to VK tube.
Boiling of water causes agitation on the top of zone and out going water vapors drive
away any residual oxygen left on the surface of melt in the top zone thus protecting melt
from getting oxidized.
During the passage of melt in the tube, Caprolactam ring opens up to form amino
Caproic acid which initiates polymerization reaction.
Water arising from polycondsation is removed form the reaction system into the form of
vapors which bundle out of the melt favoring further polycondensation.
By the time melt reached the bottom of the tube it gets fully polymerized and is with
drown at a constant rate with the help of a metering pump.
Chemical reaction:
HN(CH2)5CO + H2O H2N(CH2)5COOH
Caprolactam Amino caproic acid
H2N(CH2)5COOH + HN-(CH2)5CO H-[-NH(CH2)5-CO-]n-OH
Polymerization Short chain polymer
xH-[-NH-(CH2)5-CO-]n-OH H-[-NH(CH2)5CO-]-OH
long chain polymer
Features of Nylon:
I) Diameter 14 µm to 24µm.
II) Color slightly off – white.
III) Moisture regains 3.5-5.0% (not absorbent due to crystallinity).
IV) Hand feel- soft and smooth.
V) Resiliency- Excellent.
VI) Abrasion resistance- Excellent.
73
Properties of nylon:
1. Physical properties:
Tenacity : 4-9 gm/den (dry), in wet 90% of dry.
Elasticity : Breaking extension — 20-40%.
Stiffness : 20-40 gm/den.
Moisture regain : 3.5-5%; (not absorbent due to crystallinity).
Specific gravity : 1.14.
Abrasion resistance : Excellent.
Dimensional stability : Good.
Resiliency : Excellent.
Softening point : Nylon 6,6 — 229oC, Nylon 6 — 149oC.
Melting point : Nylon 6,6 — 252oC, Nylon 6 — 215oC.
Hand feel : Soft and smooth.
2. Chemical properties:
Acid: Nylon 6,6 is attacked by mineral acids is disintegrate or dissolve almost. But is
inert to dilute acetic acid and formic acids even of the boil. It is dissolved in the
concentrated formic acid. Nylon 6 is attacked by mineral acid but resistant to dilute
boiling organic acid.
Bleaches: Not affected by oxidizing and reducing bleaches but may be harmed by
chlorine and strong oxidizing bleaches.
Organic solvent : Most organic solvent have little or no effect on nylon. Phenol
metacressol and formic acid dissolve the fibre but solvents used in stain removal and
dry cleaning do not damage it.
74
I) Apparel use:
High tenacity nylons are used for parachute fabrics, cords and ropes. Having good dimensional
stability, nylons are used for ladies gloves, ladies hose, under wear, swimming wear, stocking,
hosiery fabric etc.
II) Domestic use:
Nylon is used for home furnishing, in carpets, in upholstery and in ropes and cords.
III) Industrial use:
In fishing nets, tire cords, filtering cloths, sewing threads, tow ropes are made of nylon. It is
used in manufacturing of belts of various m/cs (Flat belt, V-belts).
Astroturf:
Astroturf is a mono filament of nylon. It is flat and appears like a ribbon. Astroturf is mostly
used in sports fields i.e. in hockey stadium.
Chapter
6 Acrylic &
Acrylic:
Mod-acrylic
It is a manufactured synthetic fibre in which the fibre forming substance is a very ling chin
synthetic polymer composed of at least 85% acrylonitrile units by weight.
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– CH2— CH— CH2— CH— CH2— CH— CH2— CH— CH2— CH— CH2– CH–
CN CN CN CN CN
Commercial name:
Acrylic: End use:
1. Orlon - Spun yarn, high bulk yarn.
2. Acrilan - High bulk yarn, Solara.
3. Creslan - Yarn of dresses and blanket.
4. Cashmillan
5. Zefran
Modacrylic:
1. Verel - Vinylidene chloride and acrylonitrile.
2. Dynel - 60% vinyl chloride and 40%
acrylonitrile.
3. Teklan
4. Lastrile - It is a manufactured fibre in which the fibre forming
substance is a copolymer of acrylonitrile and adbatadiene.
5. SEF
6. Kanekolan
Bifilar Acrylic:
The fibre or filament that contains crimp permanently is known as Bifilar Acrylic. Two soln are
used with acrylonitrile, some monomers cause acrylic fibres to be crimped.
Functional group of acrylic: SO3H, -COOH, OSO3H.
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Ethylene oxide is then treated with HCN and then the product is dehydrated at 350oC in
presence of Alumina (Al2O3) and acrylonitrile is formed.
CH2 – CH2 + HCN HO-CH2-CH2-CN
Ethylene cyanohydrine
O
Dehydration at
350oC
H2O + CH2=CH-CN
Al2O3
Acrylonitrile
Process:
The polymerization of acrylonitrile and its co-monomer is commonly carried out by
stirring the monomers with water in the presence of catalyst and surfactants.
Some of the acrylonitrile dissolves in the water to form a 7% solution, the excess forming
an emulsion.
In a continuous process monomer, water and initiator are fed to a continuously stirred
overflow reactor at atmosphere pressure.
As polymerization proceeds, the polymer (which is insoluble in water) is precipitated to
form slurry.
This is filtered and the polymer is washed and dried.
Spinning:
The dry spinning process is applied for spinning acrylic fibre.
The polymer is dissolved in Dimethyl Formamide to form a solution of 25-40% polymer
and this polymer solution is filtered and heated to boiling point and then extruded
through spinnerets.
These fine jets of solution emerge into a vertical tube through which air at high temp is
flowing.
The filaments are brought together and stretched to 3-10 times their original length.
In case of producing continuous filaments, they are oiled, twisted and wound on to
bobbin.
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Chlorohydrine
Add NaOH
Ethylene oxide
Add hydrocyanic acid
Cyano alcohol
Dehydration
Acrylonitrile
Polymerization
Polyacrylonitrile resin
Add solvent at dry spgn (DMF)
Filter
Spinneret
Dryer
Stretching
Crimping.
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Physical properties:
Tenacity : dry – 5 gm/den, wet – 4.8 gm/den.
Elongation : dry - 16%, wet – 17%
Moisture regain : 1-2%.
Specific gravity : 1.17
Flammability : More flammable, burns rapidly with bright, yellow flames, produces no
residue.
Resiliency : Good.
Abrasion resistance : Good.
Dimensional stability : Good.
Chemical properties:
Effect of acids : Damage by strong concentrated acids. . . . Good resistance to mineral
acids.
Alkali : Resistance to weak alkali but affected by strong alkali.
Solvents : Resistance to common solvents.
Bleaches : Resistance bleaches.
Heat : Most heat sensitive.
Light : Resistance not for long time.
Dye : Acid, basic, premetalized, cationic.
Conductivity : Fair for electrical, medium for lie.
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Uses of Modacrylic:
In manufacturing pile fabrics. i.e. blanket, travel, cloths etc.
In manufacturing knitwear. i.e. sports shirts, underwear, children garments.
In making carpets and used in upholstery.
Industrially used in filter cloths and protective cloth.
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Chapter
7 Polyolefine
Olefine:
Fibre
A manufactured fibre in which the fibre firming substance is any long chain synthetic polymer
composed of at least 85% by weight of ethylene, propylene or other olefine units except
amorphous (non crystalline) polyolefines qualifying as Rubber.
Polyolefine fibres are of two types —
I) Polyethylene fibres.
II) Polypropylene fibres.
I) Polyethylene fibres:
Fibres spun from polymers or copolymers of ethylene.
CH2=CH2
II) Polypropylene fibres:
Fibres spun from polymers or copolymers of propylene.
When propylene is polymerized under certain conditions it will give fibre forming substance,
i.e. polypropylene.
CH3 CH3
n CH3-CH=CH2 –CH–CH2–CH–CH2–CH–CH2–CH–CH2–
CH3 CH3
Polypropylene
Commercial name:
Polyethylene: — Courlene, Vynene-1, Velon LP
Polyethylene: — Reevon, DLP, Meraklon.
Physical properties:
1. Tenacity : 3.5-8.0 gm/den.
2. Stretch ability : 40% elongation at break.
3. Moisture regain : 0.1%.
4. Specific gravity : 0.9 – 0.91.
5. Dimensional stability : unaffected by water
Not shrink below 150oC.
6. Resiliency : Good to excellent.
7. Abrasion resistance : Excellent.
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Chemical properties:
1. Acids : Good resistance to most acids.
2. Alkalis : High resistance to all alkalis.
3. Bleaches : Good resistance to all bleaches below 150oF.
4. Organic Solvents : Resistant to petroleum and fluoro carbons.
5. Sunlight : Suffers loss of strength.
6. Heat : Heat sensitive.
7. Dye ability : Pigment is soluble.
8. Flammability : Slow burning and melt.
9. Electrical : Conductive.
10. Thermal : Good insulator.
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Manufacturing process:
Metal allyl
Metal compound
Catalyst Diluent
decomposition
Polymer slurry
Drying
Palletizing
Polypropylene polymer
Melt spgn
Filament
Uses:
Monofilament yarn: Seat cover of car, outdoor furniture, wedding, carpet backing,
Ropes etc.
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Multifilament: Upholstery, carpet face yarn, pile fabrics backing and industrial uses
materials.
Fibrillated yarn: Carpet backing, ropes, twins and netting.
Spun yarn: All kinds of dresses.
Textured yarn: Carpet, sweater and sports wear.
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Chapter
8 Miscellaneous
FibresGlass Fibre
Glass fiber: A manufactured fiber in which the fiber forming substance is glass.
According to definition of A.S.T.M”Glass is an in organic product of fashion which has cooled
to a rigid condition with high viscosity to resist crystallization.
Types of Glass: The glasses commonly used in making textile fibers are ‘E’ glasses and ‘C’
glasses are made from compositions of the following type-
Ingredients E-glass C-glass
1.Silica-----------------54.5-53.5 62.o-65.o
2.Lime-----------------16.5-17.5 6.0
3.Alluminium-----------14.5 1.0
4. Soda-potash---------<1.0 1.0-3.0
5. Boric oxide--------10.0-10.6 3.0-4.0
6. Mg -----------------4.5-5.5
7. Soda ----------------------------------11.0-15
Manufacturing process:
1. Batches of the raw materials are prepared and fused in an electric furnace at 13700C.
2. The glass that results from the melting together of these mtls is formed into marshes about
5/8 inch dia, weighing about 5 lb.
Flow chart:
Batch formation
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Visual inspection for imperfections.
Spinning
Chemical properties:
Acid : Resistant.
Alkali : Resistant.
Sunlight : Resistant.
Dye ability : Difficult to dye.
Heat : Strength loss at 3150C, soften –7320C.
Bleach : Resistance.
Solvents : Not affected.
Flammability : Flame proof.
Features:
Smooth, Rod like and circular in cross section.
Uses:
Wedding dresses from glass fibres.
Fire proof fabrics for lamp shades.
A wings, screens, curtains and furnisher covers table cloths.
Largely used for filtration purposes.
Can be used to lag hot pipes and cylinder.
Used for Sound insulation.
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Tire cord, conveyor belt, building boat hulls, air craft, radio and TV cabinets.
Reinforcement in plastics.
Car racing suits and suits for astronauts.
Spandex
Spandex:
A synthetic polymer composed of maximum 85% segmented polyurethane is called Elastomeric
fibre. It has a high elongation % of about 600%.
Types of spandex yarn:
Bare yarn.
Covered yarn.
Core spun yarn.
Blend spun yarn.
Commercial name:
Lycra, Blue-C, Numa, Vyrene, Spanzelle, Glospan etc.
Manufacturing spandex:
For manufacturing spandex, wet spgn and chemical spgn may be used. In wet spgn, we will get
spandex fibre and in chemical spgn we will get x-link spandex.
Polyurethane
Spinning tank
Spinneret
Coagulating bath
Drying
Spandex fibre
Winding on tube
Properties of spandex:
Physical:
Tenacity : 7 gm/den.
Stretch : 500% elongation at break.
Moisture regain : 0.6%.
Specific gravity : 1.21 to 1.35.
Dimensional stability : No shrinkage in water but shrinkage in temp.
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Abrasion resistance : Very good.
Resisiliency : Very good.
Chemicals:
Acid : Resistance to acid.
Alkali : Damaged by hot alkali.
Bleaches : Resistant below at 150oF.
Organic solvents : Resistant to all.
Sunlight : Resistant to light.
Heat : High temp reduce elasticity.
Dye ability : Acid, disperse and chrome dyes, used.
Flammability : Burns rapidly.
Electrical : Low conductivity.
Thermal : Poor conductivity.
Uses:
Bare yarn: In knit fabric, socks and hosiery wear.
Covered yarn: Foundation garments, swim wear, support hose.
Core spun yarn: Knitted fabric, sports wear.
Blend spun yarn: Produced fabric suitable for calendaring.
Set % of elastomeric fibre:
Percentage of set may be defined as the elastic nature of elastomeric fibre. Let AB is a fibre
which is elongated C position by pull and it comes to point D, after removing the pull. Then we
will find that the fibre d0es not come to the position B, i.e. 100% is not recovered.
Hence
BD
Set % = 100% A B D C
AB
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Rubber
Rubber:
Rubber is a manufactured fibre in which the fibre forming substance is comprised of natural or
synthetic rubber
[ -CH2-CH=CH-CH2- ]
Physical properties:
o Tenacity : 0.5 gm/den.
o Stretch : 700 to 900% elongation at break.
o Moisture regain : Negligible.
o Specific gravity : 1.
o Dimensional stability : Good.
Chemical properties:
Acid and alkalis: Resist to most except Sulphuric acids.
Bleaches: Chlorine bleaches attack, peroxide and perborate safe.
Organic solvent:Not resistant.
Sunlight:Discolor and harden by light.
Heat:Brittle by heat.
Dye ability:Pigment.
Flammability:Burns slowly with a smoky flame.
Electrical:Non – conductive.
Thermal:Non – conductive.
End Use:
Rubber yarns are used in many different ways either-
1. To perform the functions of garments support
or 2. To maintain garment shape.
For those purpose it is used in-
Corsetry
Swim wear.
Foot wear.
Surgical hosiery.
Mens and children’shosiery.
Ladies,gents and childrens under wear and outer wear.
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Carbon Fibre
Carbon fibre:
Carbon fibres are graphite and fabrics are highly flexible forms of manufactured graphite.
Production:
Organic fibre (PAN, Rayon, and Polyester) is the starting mtls. It is oxidized in air at 200-300oC,
then carbonized at 1000oC and then graphitized by heating by heating at temp up to 3000oC in
argon.
Uses:
Air craft structural compound.
Golf club shafts.
Submarines.
Pressure vessel in chemical industries.
Productive clothing.
Nursery night wear.
The frame of racing cars.
Properties:
Acids : Resistant.
Alkali : Resistant.
Organic compounds : Resistant
Sublimation temp : 3469oC.
Does not melt.
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Casein Fibre
Casein fiber: A manufactured fiber in which the fiber forming substance is composed of
regenerated naturally occurring proteins.
Production:
Casein is obtained by the acid treatment of skimmed milk. The casein coagulates as a curd
which is washed and dried and then ground to a fine powder. 35 Liters of skimmed milk
produce about 1 kg of casein.
Spinning solution:
Casein is blended and then dissolve in sodium hydroxide solution ,then it is allowed to ripen
until it reaches a suitable viscosity and filtered .
Finally wet spun is done.
Properties:
Colour:Natural color white.
Tenacity: 1.1-1.09 gm/den (dry)
0.6-0.3gm/den (wet)
Elongation: 60-70% wet or dry.
Sp. Gravity: 1.30
M.R.:14%
Heat: Decompose at 1500c
Flammability: Burns slowly
Acid: Disintegrates in strong mineral acid but rest in weak organic acid.
Alkalis: strong alkalis cause swelling and dis integrates the fiber but have rest.
Bleaches: Generally rest in H2O2
Organic solvents: Do not cause damage.
Insects: Not attacked.
Use:
-Knitting yarns, casein and wool blends are used which produce ‘T-shirts, cardigans,
jumpers ,etc
-Blend of casein and wool made into pressed felts for use as floor coverings.
-Blend with casein and rayon staple used for needle loom carpeting.
Alginate Fibres
Alginate fibers: This fiber is based on alginic acid obtained from sew weed, which is a polymer
of d-mannuronic acid of molecular weight of 15,000.
Properties:
Flame proof ,but decomposes to ash.
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Dissolved in alkali.
Tenacity: 1.6-2.0gm/den(dry)
0.5gm/den(wet)
Elongation: 2-6%
Sp. Gravity: 1.779
M.R.: Insoluble in water.
Basic and some direct dye stuff.
End use:
Medical use: In dental surgery for plugging cavities, soluble threads for surgical
dressings.
Used as strength provides in producing loosely spun wool yarns in knitting fabrics.
Metallic Fibre
A metallic fibre is a manufactured fibre composed of metal, plastic covered metal, metal coated
plastic or a core completely covered by metal.
Example: Sliver hair ribbon in the tombs.
These fabrics were all made by beating sheets of metal-gold, sliver or copper until thin and then
cutting them in strips which were twined with yarns of other fibre.
Properties:
Tenacity- 1.5gm/den
Extension- 70-130
Moisture regain- 0.3%
Specific gravity- 1.39
Uses:
Women dresses, blouses and skirts.
Foot wear.
Upholstery, Shoe-laces, Bathing dresses, Table linens.
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Suits and jackets etc.
Perfume and liquors.
Used for decorative purpose.
Bicomponent Fibre
The fibre which consists of two components divided along the length of the fibre, into two more
or less distinct regions are termed as Bicomponent fibre.
The polymer may be physically and chemically different.
Ex- Core spun.
Bicomponent fibre may be structured in different ways:
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