Report on

Making Rayon Fibres

By : Momin Saeed Shah For Course : Polymer Laboratory(CHM6401) MSc Polymer & Polymer Composite Science & Engineering 2010/2011 Date : 1st Nov. 2010

The University of Sheffield Department of Chemistry

Abstract Introduction
Rayon is the oldest commercial manmade fiber.It is neither natural nor Synthatic fiber rather it is a semi-synthetic fiber.but the U. S. Trade Commission defines rayon as "manmade textile fibers and filaments composed of regenerated cellulose" 1. The process of making viscose was discovered by C.F.Cross and E.J.Bevan in 1891. Rayon's versatile nature is the result of the fiber being chemically and structurally engineered by making use of the properties of cellulose source. However, it is somewhat difficult to control the synthesizing processes as every batch differs and it also requires high experience involvement. The Commercial manufacturing is prepared continuous process which is the main method for producing rayon. The methods of production l ead to distinctly different types of rayon fibers.The pre form of rayon i.e viscose is either be made by cellulose from cotton or from paper by cuprammonium sythasis method this viscose method is relatively inexpensive and of particular significance in th e production of non -woven fabrics. The performed experiment's results give you an idea about the comparison of the rayon fibers, synthesized by different sources of cellulose. In this experiment cotton wool and filter paper were used to see the difference in rayon fibres.

Materials & Methods

Apparatus : Beakers(250 ml , 500ml) , measuring cylinder , Magnetic Stirrer equipment ,electronic weighing machine Plastic Syringes ,hypodermic needles of various size , Strainer for straining fibers .Spatula , Safety Equipments Lab coat , safety glasses , rubber gloves(anti corrosive), fully covered shoes. Materials & Chemicals : Cotton wool , filter papers, Copper Carbonate(CuCo 3) powder , Ammonia solution (880) , Sulfuric Acid (1M or 2M) , Distilled water. Method : (i) (ii)

(iii) (iv)

A 250ml beaker was taken and pre weighted 10gms of CuCO 3 was added to it. Freshly made 880 solution of Ammonia of volume 100cm 3 was added to beaker containing CuCO 3, and was stirred well for 2 minutes with the help of magnetic stirrer. The resulting deep blue solution was decanted and was divided into two beakers equally. The first beaker was weighted, now the shredded cotton wool was added slowly with continues mixing of solution until the blended solution became as viscous as shower gel without any lump ,which is known as Viscose.

In second beaker add similar amount of shredded filter paper ,and perform the same procedure. (vi) Two 500ml beakers were prepared with the 1M solution of H 2SO4 of 250ml. (vii) The Viscose solution was taken in plastic s yringe up to few cm3 (5 to 10 ml) with hypodermic needle attached. (viii) Steadily inject the viscose at bottom surface into the sulfur ic acid solution beaker. (ix) The thin blue rayon fibers will form. Wait few minutes until the fibers are neutralized( tetraminecopper (II) solution) and turned white. (x) Repeated the same procedure with other viscose solution (xi) Waited for 10 minutes the fibers were rinsed with water and were dried naturally. By leaving it onto filter paper.
(v) Chemistry of the Process :

Rayon is a regenerated fibre which was once called artificial silk. The polymer of rayon contains about 270 glucose units per molecule compared with cotton, which is between 2000 and 10,000.
The Reaction that takes place during the synthasis is :

[CuCO3.Cu(OH)2.H2O(s) + 4NH3(aq)

CuCO 3(s) + [Cu(NH3)4] 2+(aq) + 2OH(aq) + H2O(l)]2

When the insoluble cellulose is added to this solution it is converted to a soluble complex compound. This in turn is converted into insoluble rayon once the pH is reduced to the acidic value found in molar sulfuric acid. Accordingly, rayon precipitates out when extruded into the acid. The blue colour quickly fades away after the copper(II) ions diffuse into the solution.
Strength of the Fibers :

The strength of the fibers is weak just a fter the synthesis. They can easily break by a light pull. As per comparison of the fibers from cotton wool and filter paper relatively rayon ma de from cotton wool is stronger than the one made from filter paper. The strength of the fiber slightly increases as it dries out.
Differences between the two fibers :

In the synthesis process the cotton wool is eaiser to process because dissolution of cotton in the cuprammonium complex is fast and easy as compared to the filter paper ,which takes more effort and time to dissolve. Also the undissolved pieces of the filter paper causes difficulty in fiber drawing step, as the residue particles choke the syringe needle and stops the consistant flow of the syringe. .
Room for Improvement : Industrial Manufacturing of Rayon

The Basic Method

The basic method of producing rayon filament is similar to the natural silk manufacturing process followed by the silk worms who transform the cellulose of mulberry trees into two fine filaments. A liquid substance of cellulose is forced through a metal cap or nozzle called spinneret. The spinneret is perforated with small holes through each of which, a filament is extruded. The extruded filament gets solidified by a liquid bath as it comes from the spinneret. The number of holes in the spinneret vary from 1 to 20,000 and filaments of equal size are produced simultaneously. Subsequently, these filaments are combined by twisting to make rayon yarn of required diameter. There are basically two types of rayons- viscose rayon and high-wet-modulus (HWM) rayon- categorized on the basis of two principal methods of making rayon. As t he two methods differ in specific features of manufacture so the two fibers differ in important characteristics.. However, both, the viscose fiber and high-wet-modulus fiber are classified as regenerated rayons because the original raw material (cellulose) is changed chemically into another form, which is then changed (regenerated) into cellulose again. Purified cellulose in fiber form is produced due to these changes.
Viscose Rayon- The Viscose Process for Manufacturing Rayon

Viscose rayon is finished from cotton linter or cellulose from trees by and large obtained from pine, spruce, or hemlock trees. This Cotton linter is the deposit cotton fiber which stick to cotton seed after the ginning procedure. timber chips or cotton wool are indulge to make sheets of purified cellulose, similar to white blotters. These cellulose sheets are then soaked in caustic soda,which produce sheets of alkali cellulose. The follow-on substance is broken up into fluffy white flakes or grains known as cellulose crumbs. These crumbs are aged in metal containers for 2 to 3 days under controlled heat and moisture. Liquid carbon disulfide is added to the aged bits which turn the cellulose into cellulose xanthate, light orange -colored crumbs. The cellulose xanthate is dissolve in a weak solution of caustic soda, resulting into a thick viscose solution that appears like honey in color and consistency. The viscose is aged, filtered and vacuum treated to remove air bubbles which cause the filament to break. The solution of viscose is then enforced through a spinneret into sulfuric acid which coagulates the cellulose of the soluble cellulose xanthate to produce pure redeveloped cellulose filaments.staple fiber can also be produced but with, a large spinneret with large holes . If filament fiber is being produced, then a spinneret with smaller hole s is used. After the extrusion of viscose, rayon fibers are processed into filament or spun staple yarns by one of several methods. There are basically three methods of such processing - Pot, or Box Spinning; Spool Spinning; and Continuous Spinning. In Pot Spinning, the filaments are removed from the coagulating bath by passing over a series of godet wheels and are stretched thereon under controlled tension. This stretching reduces the diameter of the filaments and makes them more uniform in size. It also make the filaments more strong. The filaments are then put into a rapidly spinning cylinder called Topham Box, resulting in a cake -like strings that stick to the sides of the Topham Box. After

removing the cake, it is thoroughly washed, treated to remove a ny residual chemical substances, bleached, rinsed, dried, and wound on cones or spools. In Spool Spinning, the filaments may be drawn from the coagulatin g bath over guides and rollers and wound on perforated spools. A washing solution is forced through the spools' holes to cleanse filaments which are then bleached, rinsed, dried, and wound on cones or spools or put in skeins. In Continuous Spinning, upon e xtrusion from the spinneret, the filaments may be carried in one continuous process over the godet wheels through a series of reels as they are washed, purified, bleached, dried, twisted, finished and wound onto desired package. After treatment with textile chemicals, various weaving processes are carried out to produce rayon fabrics. Different varieties of yarns such as monofilament yarns, multifilament yarns, spun yarns etc. permit the manufacturing of a wide variety of fabrics. Spun rayon yarns can be used for making fabrics similar to cotton fabrics, linen fabrics or wool fabrics. Rayon filament yarns can make fabrics resembling silk fabrics. Finally, various finishing processes are carried out to enhance the appearance of these fabrics and to improve their serviceability. Most common finishes include calendaring for smoothness, embossing for decorative effects, f lame resistance, napping (spun rayons only) for softness & warmth, preshrinking for greater dimensional stability, stiffening, water resistance, wrinkle resistance etc.

High-Wet-Modulus (HWM) Rayon The Differences in Manufacturing Process Viscose rayon has its own limitations. It loses up to 70% of its strength when wet. In fact, in 1950s, when first developed, rayon was used in industrial products and home furnishings only and not for clothing. This was due to the fact that viscose rayon fibers were too weak as compared to other fibers intended to be used in apparel making. In 1960, commercial production was started for a rayon that had similar strength as of cotton fabrics and retained most of the strength, even when wet. It was high -wet-modulus (HWM) rayon. It is also known as 'modified rayon'. The process for manufacturing high -wet-modulus rayon is almost similar to that for making viscose rayon but with a few exceptions. caustic soda is used while making HWM rayon. Alkali crumbs or the viscose solution, neither of the two are aged in the HWM process of making rayon. When making HWM rayon, the filaments are stretched to a greater degree than when making viscose rayon.

Results : For the fibers the amount of cellulose used to make fibers give more than 90% yield. i.e in performed experiment 1 gram of cotton resulted in almost 1 gram of rayon fiber. Also it was noticed that the rayon made from cotton cellulose was stronger as compared to one made by filter paper.

Discussion : In my Opinion the above Experiment gives a good experience o f physical Involvment in Polymer science , rather than just the theoretical studies.The experiment showed quite well results . Although this process of rayon making is focused on just a single method.This experiment can also be performed by using other var ious chemicals showing similar results. i.e rayon fibre. Conclusion :

References : http://www.mindfully.org/Plastic/Cellulose/Rayon -Fiber.htm ,Authors: Praveen Kumar Jangala and Haoming Rong (Textile Science, University of TN)