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/lovelight1989-1258602introduction-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
Fabric
Apparel

Domestic textiles

Industrial textiles

Embroidery, chenille, cord, novelty yarns

Crepe, garardine, suiting, lace, outwear fabrics and lining
of coats and outwear
Dresses, blouses, saris, jackets, lingerie, linings,
millinery(hats), slacks, sport shirts, sports-wear, suit, ties,
work cloth
Bead spreads, Bed sheets, blankets, curtain, draperies,
slip covers, table cloths, up hosiery
High tenacity rayon is used as reinforcement to
mechanical rubber goods(tires, conveyor belts, hoses)
applications within aerospace, agricultural textile
industries, braided cord, tapes
Sausage casing, cellophane, feminine hygiene

Miscellaneous
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
cellulose

Steeping

Pressing
Shredding
white crumb
Aging

of 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
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
This is done to remove excess liquid.
and The alkali cellulose obtained after pressing are fed to shredder at about

28oC for 90-120min.This involves shredding of pressing sheet to produce

white crumb which is fluffy which allow air to penetrate effectively.
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 10and 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
Viscose

of

the

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
cutting

and 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 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
+ 2xH2O

3C6H9O4-O-C
SNa

C18H27O12(OH)2O-C

SNa

+ 2XCS2 + 2xNaOH
S

C18H27O12(OH)2-O-C

+ x/2 H2SO4 (C6H9O4OH)3x + XCS2

SNa

Viscose Rayon

+ x/2 Na2SO4

For regulating
viscosity

18-20% NaOH

Cellulose
Sheets

Steeping Press

Shredder

20-22oC
1 - 4 hr

28oC
90-120 min

Deaeration

Ripening

Alkali Cellulose
Aging Tank
20-35oC
2 - 3 days

Xanthating
Barattes
20-35oC
2 hrs

Viscose

Feed Tank

Filtration
Honey like
appearance

10-15oC for 4 - 5 days

SpinningSpeed:6080m/min
Viscose
Spinning

1
Spent
bath

Dissolving
Tank
10oC
4 - 5 hrs

1 - Washing
2 - Desulfurising
3 - Bleaching
4 - Conditioning
5 - Drying

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

Cellulose

OH

O
O

OH

OH

OH

OH
OH

OH

OH

Acetic anhydride/H2SO4

CH2OAc

CH2OAc

CH2OAc
O
O

OSO3H

O
O

OSO3H

OSO3H

OAc

OAc
OAc

OAc

Hydrolysis

CH2OAc

Cellulose acetate

CH3COOH + H2O

CH2OAc

CH2OAc
O

O
O

OH

OH

OAc
OAc

OAc

OAc

OH

OAc
OAc

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 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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