VISCOSE FIBER
(RAYON FIBER)
Applications of Viscose Fiber
• Apparel: Accessories, blouses, dresses, jackets, linings, millinery,
slacks, sports shirts, sportswear, suits, ties, work clothes.
• Home Furnishings: Bedspreads, blankets, curtains, draperies,
sheets, slipcovers, tablecloths, upholstery.
• Industrial Uses: Industrial products, medical surgical products,
nonwoven products, tyre cord.
• Other Uses: Feminine hygiene products, baby wipes and kitchen
wipes.
Cellulose, which is found in plant walls, is the most abundant raw material on Earth.
It is capable of producing a number of fibrous products with excellent properties
whose utility extends into numerous end uses and industries.
Because of the strong intermolecular bonds, cellulose does not melt and does not
dissolve readily in ordinarily available solvents; chemists have resorted to the
derivatization of cellulose to render it soluble and processable.
Today, the production of rayon represents an example of the most complex case of
fiber formation by a wet-spinning process.
The prime attributes of rayon-comfort, attractiveness, ease of processing, price,
and raw material availability will assure its viability for many years to come.
The first patent on the viscose process was granted to CROSS and BEVAN in
England in 1893, then in 1904 Samuel Courtauld purchased the British rights to
manufacture textile yarn from viscose . A plant was built at Coventry, and the first
yarn was produced in November 1905.
THE VISCOSE PROCESS
In this process, because of the poor solubility of cellulose in most of the
common solvents, the cellulose is converted to a soluble derivative to prepare a
solution for spinning.
For this, short-fibered cellulose (i.e wood pulp) is converted in a series of
controlled and coordinated steps to a spinnable solution and then into longer
filaments, which may be precisely controlled to obtain desired length, denier,
cross-sectional shape and other physical properties.
That is the reason Viscose or Rayon is also termed as REGENERATED
CELLULOSIC FIBER
STEP 1: STEEPING
The pulp is first steeped (soaking) in an aqueous solution of sodium hydroxide (17–18%)
at ambient temperature. The fiber structure swells and hemicelluloses (short length
cellulose molecules) and other impurities gets dissolved in the alkaline solution.
The basic reaction is one in which cellulose is converted to sodium cellulosate or alkali
cellulose, as in the following equation:
An initial decrease in the average chain length (DP) is observed when pulp is steeped.
This has been attributed to oxidative degradation involving dissolved and absorbed air
and alkali sensitive groups such as carbonyl on the cellulose.
Because alkaline hydrolysis produces short-chain material, it is desirable to continue
the steeping for the shortest time needed to obtain uniform distribution of alkali in the
pulp.
STEP 2: PRESSING & SHREDING
After steeping, the swollen mass is pressed with high pressure rollers to obtain a
precise ratio of alkali to cellulose (alkali cellulose weight is approximately 2.8 times
that of the original pulp).
Pressing tends to compress the alkali cellulose that then must be opened or fluffed
to provide uniform access to air and carbon disulfide vapor. This is accomplished by
shredding either in a batch or continuous process to separate the fibers into a loose
mass known as ‘‘crumb.’’
STEP 3: AGEING
Control of average chain length or DP of the cellulose is achieved by aging the alkali
cellulose crumb under conditions yielding the appropriate extent of de-
polymerization.
Cellulose chains are randomly cleaved by alkaline oxidation (during steeping). On
the other hand, hydrolysis involves end-group attack, which removes single units
from the ends of the cellulose chains.
Therefore, de-polymerization by this mechanism (Ageing process)occurs much more
slowly and in a controlled manner than with oxidation and yields alkali-soluble
degradation products.
Thus, in ageing process, the shredded crumbs of alkali-cellulose is kept in large slow
rotating drums where de-polymerization of cellulose takes place. The time required
for aging crumb can be reduced from more than 24 h to as little as 1 or 2 h by using
suitable metal catalyst and temperature.
STEP 4: XANTHATION
The aged alkali cellulose crumbs are then treated with CS2 gas in closed churning
chambers kept under vacuum.
CS2 is introduced in weight proportion of 32-35% of the weight of cellulose. The
churn is rotated slowly at 1 to 4 rev/min for a period of 1-3 hours at a temp. of 20-30°
C.
Approx. 65% of CS2 reacts with the cellulose while remaining undergoes other side
reactions . The prominent reaction being the formation of Na 2CS3, which is
responsible for orange colouration of the flakes.
A yellow to orange coloured crumbs are formed upon reacting with carbon disulfide
gas to form sodium derivative of cellulose termed as “cellulose xanthate”.
RcellO-Na+ + CS2 RcellOCSSNa + Na2CS3
Alkali Carbon Sodium
Disulphid Sodium Cellulose trithiocarbamate
Cellulose Xanthate
e Gas (orange coloured)
STEP 5: MIXING or DISSOLUTION
The xanthate crumb is dissolved in a dilute aqueous solution of sodium hydroxide of
about 5–8% concentration to form a viscous solution. (That’s why the name is VISCOSE
Rayon)
A low mixing temperature is preferred because this will minimize xanthate
decomposition and byproduct formation. A thick viscous and orange-colored solution
is obtained.
RcellOCSSNa + NaOH Viscose solution
STEP 6: FILTRATION
Following the dissolution step, the viscose is carefully blended to achieve the best
uniformity of properties.
The viscose is filtered in a number of steps to remove undissolved particles and
contaminants.
STEP 7: RIPENING
Ripening is a process where viscose solution is transferred to large tanks and
kept for 1 to 3 days at constant temp. of 15-25 °C.
During ripening, chemical and physical changes occur in the viscose.
Spontaneous decomposition of xanthante and distribution of xanthate groups
both within the cellulose polymer molecule and among the cellulose polymer
chains takes place.
When cellulose is xanthated, the reaction is heterogeneous as the most accessible
hydroxyl groups reacts first, resulting in a very non-uniform distribution. Therefore, to
achieve homogeneous distribution of xanthate group, the cellulose xanthate is
dissolved in alkali and the viscose solution is stored for 1-3 days.
The viscosity of xanthate solution initially drops as redistribution of xanthate groups
increases dispersion, and then increases as dexanthation and agglomeration of
cellulose molecules gradually reduces solubility.
The degree of ripening is controlled by time and temperature until the required
ripeness is obtained.
Ripeness is usually expressed as a Salt index (SI) or Hottenroth number,
Salt Index (SI): The conc. Of NaCl solution at 15 C needed to coagulate 1 drop of viscose
solution from a glass rod of 3/16 in. dia.
Hottenroth Number: The volume in ml of a 10% ammonium chloride solution which is
needed to coagulate 20 g of viscose solution diluted with 30 ml of water.
Regular rayon is usually spun when the SI is from 4.5 to 5.0 for a given viscose.
Hottenroth numbers are higher and could be 11–14 for the same viscose.
STEP 8: WET SPINNING
The spinning of viscose is basically the recovery of cellulose from cellulose xanthate
by an acid decomposition reaction.
Initially, the action of the acid in spin-bath causes the viscose to coagulate and
forms a skin around the filament. Then, as the acid penetrates into the viscose
filament, neutralization of the alkali occurs. At the same time, cellulose xanthate is
decomposed regenerating cellulose and carbon disulfide from which it was made.
The principal reactions beginning at the spinnerette are coagulation, neutralization, and
regeneration. Coagulation, in which the viscose sets up as a gel, occurs quite rapidly and
can be regarded as leading to primary structure formation.
A conventional coagulation bath (SPIN BATH) contains following ingredients;
A salting out agent, like Na2SO4 (16-24%)
A regenerating agent, ;like H2SO4 (8-10%)
A compound forming agent, like ZnSO4 (1-2%)
Temp-25 °C
Spinning speed-20-30m/min
Stretch-150-300%
ROLE OF ZINC IN SPINNING BATH
The presence of zinc results in formation of intermediate zinc cellulose xanthate
complex which is more stable against induced regeneration.
Zinc being bivalent, forms cross-links between adjacent xanthate groups. This cross-
linking prevents swelling of viscose solution and forms tough zinc xanthat gel which
can be stretched to a high degree before regenration, resulting in highly oriented
structure with large number of crystals having small crystal sizes.
PROCESS DIAGRAM FOR VISCOSE FIBER PRODUCTION
STEP 9: Drawing:
The rayon filaments are stretched while the cellulose chains are still relatively mobile. This
causes the chains to stretch out and orient along the fibre axis. As the chains become
more parallel, inter-chain hydrogen bonds form, giving the filaments the properties
necessary for use as textile fibres.
STEP 10: Washing:
The freshly regenerated rayon contains many salts and other water soluble impurities
which need to be removed. Several different washing techniques may be used.
STEP 11: Cutting:
If the rayon is to be used as staple (i.e., discreet lengths of fibre), the group of filaments
(termed "tow") is passed through a rotary cutter to provide a fibre which can be
processed in much the same way as cotton.
