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Course: Chemical Technology (Organic) Module VIII

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.

Table M-VIII 8.1: Indian capacity 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

Properties of Viscose Rayon

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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

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
Dresses, blouses, saris, jackets, lingerie, linings,
Apparel millinery(hats), slacks, sport shirts, sports-wear, suit, ties,
work cloth
Bead spreads, Bed sheets, blankets, curtain, draperies,
Domestic textiles slip covers, table cloths, up hosiery

High tenacity rayon is used as reinforcement to


Industrial textiles 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
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:

Table M-VIII 8.3: Process Details of Viscose Rayon Manufacturing


Production of Cellulose used in the manufacture of viscose rayon is alpha cellulose.
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 20-22oC 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 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 :

(C6H10O5)n + nNaOH  (C6H9O4ONa)n + H2O


S

(C6H9O4ONa)n + nCS2  C6H9O4-O-C

SNa

Cellulose Xanthate

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S S

3C6H9O4-O-C + 2xH2O  C18H27O12(OH)2O-C

SNa n SNa X

+ 2XCS2 + 2xNaOH

S C18H27O12(OH)2-O-C
+ x/2 H2SO4  (C6H9O4OH)3x + XCS2

SNa x Viscose Rayon


+ x/2 Na2SO4

 
18-20% NaOH For regulating
  viscosity

  Cellulose Alkali Cellulose Xanthating


Steeping Press Shredder
Sheets Aging Tank Barattes
  20-22oC 28oC 20-35oC 20-35oC
1 - 4 hr 90-120 min 2 - 3 days 2 hrs
 
Viscose
Dissolving
  Feed Tank Deaeration Ripening Filtration
Tank
Honey like
  appearance 10oC
4 - 5 hrs
10-15oC for 4 - 5 days
Spinning Speed : 60‐80 m/min 
Viscose 1 - Washing
Spinning 2 - Desulfurising
3 - Bleaching
  1 2 3 4 5 4 - Conditioning
5 - Drying
  Spent
bath H2SO4

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

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 25-30oC. 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

CH2OAc CH2OAc CH2OAc


O O O

OSO3H O O
OSO3H OSO3H
OAc OAc
OAc OAc OAc
N

Hydrolysis CH3COOH + H2O

CH2OAc CH2OAc CH2OAc


O O O

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

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” 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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