Course: Chemical Technology (Organic) Module VIII
Lecture 8
CELLULOSIC FIBRES
(Viscose Rayon and Acetate Rayon,
Cuprammonium Rayon)
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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.
Table M-VIII 8.1: Indian capacity of Viscose Rayon
Properties of Viscose Rayon
Name of the unit Capacity, Tonnes
Century rayon 53,000
Kesoram rayon 17000
Indian rayon 7000
National rayon 13000
Baroda rayon 4500
Domestic demand 54000
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Viscose rayon has a silk aesthetic with superb drape and feel and retains its rich brilliant colour.
It has high moistureabsorbency 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
o
C, chars and decomposes at 177 to 244
o
C. 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
Table M-VIII 8.2: Application of Viscose Rayon
Yarn
Embroidery, chenille, cord, novelty yarns
Fabric Crepe, garardine, suiting, lace, outwear fabrics and lining
of coats and outwear
Apparel
Dresses, blouses, saris, jackets, lingerie, linings,
millinery(hats), slacks, sport shirts, sports-wear, suit, ties,
work cloth
Domestic textiles
Bead spreads, Bed sheets, blankets, curtain, draperies,
slip covers, table cloths, up hosiery
Industrial textiles
High tenacity rayon is used as reinforcement to
mechanical rubber goods(tires, conveyor belts, hoses)
applications within aerospace, agricultural textile
industries, braided cord, tapes
Miscellaneous Sausage casing, cellophane, feminine hygiene
Source: http://www.swicofil.com/products/200vicose.html
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.
Raw Material for per Tonne of rayon fibres
Pulp 1030 kg
NaOH 650 kg
H
2
SO
4
960 kg
CS
2
330 kg
Zinc sulphate 30 kg
Bleach Chemical 50 kg
Coal 6250 kg
Water 600 m
3
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:
Table M-VIII 8.3: Process Details of Viscose Rayon Manufacturing
Production of
cellulose
Cellulose used in the manufacture of viscose rayon is alpha cellulose.
Cellulose is obtained from pulping of wood/bamboo where special care is
taken in pulping and bleaching so that the pulp is of higher strength with
high cellulose content
Steeping This involves pulp sheets are placed in steeping compartment and reacted
with18-20% NaOH at 20-22
o
C for about 1-4 hr. Purpose of steeping is
To break intermolecular bonds of the cellulose to increase solubility
of cellulose xanthate
To convert cellulose into alkali cellulose
To swell cellulose fibre
To dissolve low molecular weight hemi-cellulose
Pressing This is done to remove excess liquid.
Shredding and
white crumb
The alkali cellulose obtained after pressing are fed to shredder at about
28
o
C 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 20-30
o
C to form a cellulose
xanthate. This is called yellow crumb. The yellow crumb is dissolved in
caustic solution to form viscose.
Ripening, filtering
and de-aeration
The process involves ripening of viscose by keeping for 4-5 days at 10-
18
o
C 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
cutting
Drawing is the process of stretching the rayon filament which straighten
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
rayon
Viscose rayon has high affinity dye and can be dye easly with cotton dyes.
Reactions :
(C
6
H
10
O
5
)
n
+nNaOH (C
6
H
9
O
4
ONa)
n
+H
2
O
S
(C
6
H
9
O
4
ONa)
n
+nCS
2
C
6
H
9
O
4
-O-C
SNa
Cellulose Xanthate
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S S
3C
6
H
9
O
4
-O-C +2xH
2
O C
18
H
27
O
12
(OH)
2
O-C
SNa n SNa X
+2XCS
2
+2xNaOH
S C
18
H
27
O
12
(OH)
2
-O-C
+x/2 H
2
SO
4
(C
6
H
9
O
4
OH)3x +XCS
2
SNa x Viscose Rayon
+x/2 Na
2
SO
4
SpinningSpeed:6080m/min
Figure M-VIII 8.1: Process flow diagram for Viscose Rayon Manufacture
Cellulose
Sheets
Steeping Press Shredder
Alkali Cellulose
Aging Tank
Xanthating
Barattes
Dissolving
Tank
Filtration Ripening Deaeration Feed Tank
Viscose
Spinning
1 2 3 4 5
1 - Washing
2 - Desulfurising
3 - Bleaching
4 - Conditioning
5 - Drying
Evaporator
Make up
Tank
H
2
SO
4
To coagulating bath
Na
2
SO
4
Spent
bath
20-22
o
C
1 - 4 hr
28
o
C
90-120 min
20-35
o
C
2 - 3 days
20-35
o
C
2 hrs
For regulating
viscosity
18-20% NaOH
10
o
C
4 - 5 hrs
Viscose
Honey like
appearance
10-15
o
C for 4 - 5 days
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Variables in Spinning:
Temperature and composition of bath.
Speed of coagulation
Length of immersion
Speed of spinning
Stretch imparted
Poly Sonic FIbres(VINCEL, ZANTREL): Polysonic fibres are new kind of
viscose rayon and have uniformity, length luster and microfibrillar structure. During the process
steps are taken to maintain higher degree of polymerization by reducing the severity of chemical
processing. During the initial stage cellulose sheets bathed in weaker caustic soda. Higher
degree of polymeristion ( around 500-700 against viscose rayon around 250) is achieved by
precipitating the viscose gently and slowly. The fibre is much like cotton
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 25-30
o
C. 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
o
C for the first hour
25-30
o
C 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. 230
o
C and decompose when melted, readily soluble in
acetone, methyl ethyl ketone, methyl acetate, ethyl acetone, chloroform, ethylene chloride.
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O
CH
2
OH
OH
OH
OH
O
O
CH
2
OH
OH
OH
O
O
CH
2
OH
OH
OH
OH
N
O
CH
2
OAc
OAc
OSO
3
H
OAc
O
O
CH
2
OAc
OSO
3
H
OAc
O
O
CH
2
OAc
OSO
3
H
OAc
OAc
N
O
CH
2
OAc
OAc
OH
OAc
O
O
CH
2
OAc
OH
OAc
O
O
CH
2
OAc
OH
OAc
OAc
N
Acetic anhydride/H
2
SO
4
CH
3
COOH + H
2
O Hydrolysis
Cellulose
Cellulose acetate
Figure M-VIII 8.2: Process flow diagram for the manufacture of Acetate
rayon
Cupraammonium Rayon: Cupraammonium rayon is made from reaction of Cellulose with
copper salt and ammonia. After bleaching celullose is added in ammonical solution of copper
sulphate resulting in formation of cuprammonium cellulose which is spun into water and the yarn
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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.
Figure M-VIII 8.3: Process flow diagram for the manufacture of
REFERENCE
1. Austin, G.T., Cyclic Intermediates and dyes Shreves 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 Riegels Handbook of Industrial chemistry
Ninth edition Edited by J ames 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
