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Lecture 8
CELLULOSIC FIBRES
(Viscose Rayon and Acetate Rayon,
Cuprammonium Rayon)
LECTURE 8
CELLULOSIC FIBRES
(Viscose Rayon and Acetate Rayon, Cuprammonium Rayon)
Rayon is derived from French word “rays of light” and was first sold as artificial silk. Rayon is
made from cellulose derived from naturally occurring material. The first manufactured cellulosic
fibre was invented in France in 1884, however first commercial production was in 1910 by
Avtex fibre Inc. in USA [http://www.authorstream.com/Presentation/lovelight1989-1258602-
introduction-vfy/]. Some of the common rayon are viscose rayon, acetate rayon, cup ammonium
rayon. Other rayons are cuprammonium rayon, pyroxylin rayon. some of the natural material
based are casein fibre, alginate fibre, vicara, soyabin. fibre Amongst the various rayon viscose
rayon is most commonly commercially manufactured rayon and find wide application in textile,
tire cord industry. Various types of viscose rayon are regular rayon, High tenacity rayon, high
wet modulus (HWM) rayon, Flame retardant rayon, Super adsorbent rayon. Some of the major
rayon producing units in India are given in Table M-VIII 8.1. Global demand of viscose fibre is
3,20,000 tonnes per annum.
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Viscose rayon has a silk aesthetic with superb drape and feel and retains its rich brilliant colour.
It has high moisture absorbency similar to cotton, breathable, comfortable to wear and easily
died. It is comfortable, soft to skin and has moderate dry strength and low abrasion resistance, no
static buildup, moderate resistance to acid and alkali, excessive flammable. Thermal properties
poor and losses strength above 149 oC, chars and decomposes at 177 to 244 oC. Tenacity ranges
between 2.0 to 2.6 g/den when dry and 1.0 to 1.5g/den when wet. It has poor crease recovery and
crease retention in comparison to polyster. Because of low melting point lower application in tire
cord. Application of vicose rayon is given in Table M-VIII 8.2.
Various Grades: Flat yarn, high tenacity, mono-filament, fibres, tow/tops, spun yarns
Types of Rayon: Regular rayon, high wet modulus rayon, high tenacity Rayon, Microfibres,
tencel rayon, lyocel, Special rayon flame retardant fibres,superabsorbent rayons, microdenier
rayon finres
Raw Material
Cellulose, NaOH, Carbon disulfide, Sulfuric acid, Titanium dioxide to delustre the yarn, sodium
sulfide, sodium sulfite, sodium hypochlorite additives. Cellulose is obtained from rayon grade
pulp or cotton linter.
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Rayon grade Pulp: Rayon grade (also called dissolving pulp) is high cellulose content pulp.
wood pulp is major source of rayon grade pulp. During production of rayon grade pulp more
drastic condition is used to obtain high quality dissolving pulp. During selection of raw materials
process conditions in pulping and bleaching, pulping and bleaching chemicals and further
processing of pulp special precaution is taken.
Pulp 1030 kg
NaOH 650 kg
H2SO4 960 kg
CS2 330 kg
Zinc sulphate 30 kg
Bleach Chemical 50 kg
Coal 6250 kg
Water 600 m3
Power 2000 kg
Process Steps: Details of manufacturing process of viscose rayon is given in Table M-VIII 8.3.
Figure M-VIII 8.1 show the process manufacture of Viscose rayon. Various steps involved in
manufacture of viscose rayon are:
Shredding and The alkali cellulose obtained after pressing are fed to shredder at about
white crumb 28oC for 90-120min.This involves shredding of pressing sheet to produce
white crumb which is fluffy which allow air to penetrate effectively.
Aging After shredding the white crumb are aged to bring down degree of
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polymerization. This involves aging of crumb through exposure of white
crumb to oxygen. It helps in maintaining proper viscosity.
Xanthation After ageing, the soda cellulose crumbs are fed into a air tight rotating
churns The process involves treatment of white crumb with carbon
disulphide under controlled condition at 20-30oC to form a cellulose
xanthate. This is called yellow crumb. The yellow crumb is dissolved in
caustic solution to form viscose.
Ripening, filtering The process involves ripening of viscose by keeping for 4-5 days at 10-
and de-aeration 18oC which varies according to type of fiber being made. Ripeness
measured by Hotteen number. After ripening the ripen viscose is filtered
and degassing is done to remove air bubbles
Spinning of the
Viscose Spinning of viscose is done by wet spinning by passing through spinerrate
in acid bath resulting in formation of rayon filament.
Spinning Bath
Sulfuric acid 10 parts
Sodium sulfate 18 parts
Glucose 2 parts
Zinc sulfate 1 part
Water 69 part
Sodium sulfate precipitates sodium cellulose xanthate into filament form
and acid converts it into cellulose. Zinc sulfate gives added strength.
Further processing involves washing desulphurising, bleaching
conditioning and drying
Drawing and Drawing is the process of stretching the rayon filament which straighten
cutting out the fibres. The continuous yarn is cut into for producing staple fibres.
Crimping The staple fibre is made like wool by crimper. Sarille is crimped viscose
staple having wool like fabrics
Dyeing of Viscose Viscose rayon has high affinity dye and can be dye easly with cotton dyes.
rayon
Reactions :
SNa
Cellulose Xanthate
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S S
SNa n SNa X
+ 2XCS2 + 2xNaOH
S C18H27O12(OH)2-O-C
+ x/2 H2SO4 (C6H9O4OH)3x + XCS2
18-20% NaOH For regulating
viscosity
Evaporator Na2SO4
Make up
Tank
To coagulating bath
Figure M-VIII 8.1: Process flow diagram for Viscose Rayon Manufacture
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Variables in Spinning:
Temperature and composition of bath.
Speed of coagulation
Length of immersion
Speed of spinning
Stretch imparted
ACETATE RAYON
The purified cotton linters or cellulose is fed to the acetylator containing acetic anhydride and
acetic acid and conc. Sulphuric acid and acelylation is carried out at 25-30oC. The reaction
mixture called acid dope is allowed for ripening for about 10-20 hrs. During reopening
conversion of acetate groups takes place. After reopening, the mixture is diluted with water with
continuous stirring. During the process flakes acetate rayon is precipitated which is dried and
send to spinning bath where dry spinning of acetate rayon takes place by dissolving in solvent
and passing trough spinnerated. The solvent is evaporates by hot air. The dope coming from the
spinnerate is passed downwards to feed roller and finally to bobbin where spinning is done at
higher speed.
Raw Material
Purified cotton linters, wood pulp, acetic anhydride, acetic acid and sulfuric acid.
Process Steps
Activation with Acetic Acid: The process involves steeping of purified cotton in acetic acid
which makes. Swelling and makes cellulose more reactive
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Acetylation: The pretreated cotton with acetic acid is then acetylated with excess acetic acid,
acetic anhydride, with sulphuric acid to promote the reaction.
One part of purified cellulose
Three part of acetic anhydride
Five parts of acetic acid
Sulfuric acid 0.1 part (as catalyst)
Reaction exothermic
Temperature 20 oC for the first hour
25-30oC for the next 7-8 h
Hydrolysis of Triacetate: The triacetate formed is hydrolysed to convert triacetate to diacetate.
The resultant mixture is poured in water to precipitate the cellulose acetate
DP 350-400
2.35 – 2.4 acetyl groups per anhydro glucose unit.
Spinning: Secondary acetate is dissolved in acetone, fitered, dearerated and passed through
spinerrate in hot air environment, which evaporates the solvent.
Economical Production
Low cost and availability of acetic acid and acetic anhydride
Recovery of acetic acid
Recovery of acetone
Process flow diagram for the manufacture of acetate Rayon is given in Figure M-VIII 8.2
Properties: Tenacity 1.4 g/denser, M.P. 230oC and decompose when melted, readily soluble in
acetone, methyl ethyl ketone, methyl acetate, ethyl acetone, chloroform, ethylene chloride.
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CH2OH CH2OH CH2OH
O O O
Cellulose O
OH OH O OH
OH OH
OH OH OH
N
Acetic anhydride/H2SO4
OSO3H O O
OSO3H OSO3H
OAc OAc
OAc OAc OAc
N
Cellulose acetate OH O O OH
OH
OAc OAc
OAc OAc OAc
N
Figure M-VIII 8.2: Process flow diagram for the manufacture of Acetate
rayon
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is washed with acid to remove traces of ammonia and dried. Process flow diagram for the
manufacture of cuprammoium rayon is given in Figure M-VIII 8.3.
REFERENCE
1. Austin, G.T., “Cyclic Intermediates and dyes” Shreve’s Chemical Process Industries Fifth
Edition, McGraw Hill International editions1984, p. 772
2. COINDS “Comprehensive industry document Man-made Fibre Industry” Central Pollution
Control Board New Delhi, 1979-80
3. Gupta, B.S. “Manufacture of textile fibres p.735 Riegel’s Handbook of Industrial chemistry
Ninth edition Edited by James A. Kent CBS Publishers & Distributors, Fifth edition 1997
4. http://www.authorstream.com/Presentation/lovelight1989-1258602-introduction-vfy/
5. Woodings, Calvin “Fibre regenerated cellulose” Kirk Othmer Encylopedia of Chemical
technology fifth edition, Volume 11 Wiley inter science, 2006, p.246
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