AIM

To prepare a sample of cuprammonium rayon threads from filter paper.

Apparatus Required
Beakers
Conical Flask
Filtration Flasks
Vacuum Pump
Bent Tube
Glass Rod
50% Ammonia Solution
Dilute H2SO4
Filter Paper/ Waste paper

Procedure
The cellulose is dissolved in cuprammonium hydroxide [Cu(NH3)4](OH)2

To Prepare Cuprammonium Hydroxide Solution

Weigh about 20 g of crystalline copper sulphate in a clean watch glass.
Dissolve it in 100ml of water in a beaker. Add dilute NaOH solution to
this solution slowly with stirring and note the separation of the Cu(OH)2.
Filter the precipitate on a water pump and wash the precipitate thoroughly
with water so that a portion of filtrate does not indicate the presence of
sulphate ions on testing with BaCl2 solution. Now transfer the precipitate
to a 250ml beaker and add 50 ml of liquid ammonia. The precipitate will
dissolve resulting in a deep blue solution of cuprammonium hydroxide
(Schweiers Solution). This is the solvent to dissolve cellulose.
DISSOLVING THE CELLULOSE MATTER
Weigh about 1g of ordinary filter paper and cut it into small pieces. Add
these pieces to the cuprammonium solution taken in a conical flask. Close
the flask with a rubber stopper and allow it to stand for 3-4 days. In this
time, filter paper completely dissolves leaving a viscous solution called
viscous

Formation of Rayon Filament

The viscous solution is taken in a syringe. Then the nozzle of the syringe is
dipped into 5M H2SO4 solution taken in a wide-mouthed beaker. Squeeze
out the viscose into the acid solution and at the same time keep moving the
nozzle in the acid. Long filaments of rayon will be formed in the beaker.
The acid bath is left undisturbed for 24 hours, until the blue colour of the
filament changes to white.

Rayon filaments are then removed from the acid bath, washed with water
and dried by keeping them on a filter paper. When the threads are
completely dried, weigh them and determine the maximum length of the
fibre formed

Precautions
a) Addition of excess NH3 should be avoided.
b) Before taking the viscose in the syringe make sure that it does not
contain any particles of paper, otherwise, it would clog the needle of the
syringe.
c) Addition of NH3 should be done in a fume cupboard and with extreme
care. The fumes if inhaled may cause giddiness.
Introduction
Cellulose is natures own giant molecule. It is the fibrous material that
every plant from seaweed to the sequoia makes by baking glucose
molecules in long chains; the chains are bound together in the fibres that
give plants their shape and strength. Wood has now become the main
source of cellulose. Since it contains only 40% to 50% cellulose, the
substance must be extracted by pulping. The logs are flaked, and then
simmered in chemicals that dissolve the tarry lignin, resins and minerals.
The remaining pulp, about 93% cellulose, is dried and rolled into sheets-
raw material for paper, rayon and other products.
It can be obtained in 2 ways:
1. Viscose Process: Cellulose is soaked in 30% caustic soda solution
for about 3 hrs. The alkali solution is removed and the product is
treated with CS2. This gives cellulose xanthate, which is dissolved
in NaOH solution to give viscous solution. This is filtered and forced
through a spinneret into a dilute H2SO4 solution, both of which
harden the gum-like thread into rayon fibres. The process of making
viscose was discovered by C.F.Cross and E.J.Bevan in 1891.

2. Cuprammonium Rayon: Cuprammonium rayon is obtained by

dissolving pieces of filter paper in a deep blue solution containing
tetra-ammine cupric hydroxide. The latter is obtained from a
solution of copper sulphate. To it, NH4OH solution is added to
precipitate cupric hydroxide, which is then dissolved in excess of
NH3.

Reactions:

CuSO4 + 2NH4OH Cu(OH)2 + (NH4)2SO4

Pale blue ppt

Cu(OH)2 + 4NH4OH [Cu(NH3)4](OH)2 + 4H2O

[Cu(NH3)4](OH)2 + pieces of filter paper left for 10-15 days give a

viscous solution called VISCOSE.
Background
Rayon is a synthetic fibre produced from cellulose. Developed in an
attempt to produce silk chemically, it was originally called artificial silk or
wood silk. Rayon is a regenerated fibre, because cellulose is converted to a
liquid compound and then back to cellulose in the form of fibre. For
example, cuprammonium rayon is made by dissolving cellulose in an
ammoniacal copper sulphate solution.

The characteristics of rayon fibres are:

They are highly absorbent,

Soft and comfortable,
Easy to dye &
Drape well.

HISTORY
The invention of rayon can be related to the invention of an apparatus in
1840 that drew synthetic filaments through small holes. In 1855, Georges
Audemars, a Swiss chemist, discovered how to make cellulose nitrate.
Later in 1884, Count Hilaire de Chardonnet made the first manmade fibres
from nitrocellulose. He came to be known as the 'father of rayon'. He got
the original French patent and also won financial support through which,
he established the world's first rayon factory. Subsequently, other
scientists developed more cost-effective ways of making many other types
of rayon.

The Federal Trade Commission (FTC) officially recognized manmade

textile filaments in 1925 when it allowed the use of the name, "rayon"
for yarns obtained from cellulose or its derivatives. Till now, it was known
as artificial or imitation silk. With the production and types of manmade
fibres increasing and given various trademarks, the FTC again made a rule
in 1937 that any fibre or yarn produced chemically from cellulose must be
designated as rayon. However, confusion prevailed among the masses
because at least four different types of rayon with some similar and some
different properties came into being. It was because of the fact that there
were basically two groups of rayon- one consisting of regenerated pure
cellulose and the other of a cellulose compound. These different
compositions gave different properties. Therefore, in 1952, the FTC ruled
that there would be two categories of cellulose fibres- rayon fibre (pure
cellulose) and acetate fibre (cellulose compound).
HEALTH HAZARDS
Highly toxic carbon disulphide is used in the production of viscose. It is
released into the air during production.
Workers breathing it in suffer serious neurological, cardiovascular, and
liver problems, burns, and blindness. People and animals near a rayon
factory can also be harmed by carbon sulphide emissions. However, the
volatile carbon disulphide is lost before the rayon gets to the consumer; the
rayon itself is basically pure cellulose.
Studies from the 1930s show that 30% of American rayon workers
suffered severe effects. Rates of disability in modern factories (mainly in
China, Indonesia and India) are unknown. The production of rayon poses a
serious health risk to unprotected factory workers.
Viscose factories vary widely in the amount of CS2 they expose their
workers to, and most give no information about their quantitative safety
limits or how well they keep to them. It is more harmful to produce rayon
blends than pure rayon, as the threads are pulled from the vat still dripping
carbon disulphide.
Viscose manufacturers have not been forthcoming about the risks of their
manufacturing processes, have actively suppressed publication of such
risks, have knowingly chosen more-polluting manufacturing processes for
financial reasons, and have engaged public relations consultants to work
on the image problem created by reports of harms from their carbon
disulphide emissions.
While it is possible to contain CS2 emissions, or eliminate its use as a
solvent, it is more expensive. Legal limits for occupational exposure to
CS2, even in the US, are still far higher than recommended by medical
researchers.