Patent GB-369912-A (GB)
Title: Improvements in or relating to the manufacture of cellulose products
IPC: D21C3/00
Filed: 1930-09-24
Abstract: Cellulose and cellulosic materials are produced by a process which comprises subjecting wood, straw, grasses, and like lignified materials to treatment whereby the cellulose contained in such materials is dissolved out from the ligneous and like impurities in the form of a metal compound or complex, separating, by filtration, centrifuging, or the like the solution obtained from the said impurities and thereafter regenerating the cellulose from the solution.  The cellulose may be dissolved out in the form of a xanthogenate or as a cuprammoniumcellulose solution.  The wood &c. is preferably in as fine a form as possible and may be first treated with hot water or alkali or organic solvents to remove resins. Xanthogenation treatment may be effected in any suitable way, e.g. the materials may be immersed in, impregnated or kneaded with caustic soda solutions of 15-20 per cent and preferably 17-19 per cent strength, the resulting soda cellulose after any desired ageing or ripening being treated with carbon bisulphide.  Preferably the materials should be treated with excess of solution, e.g. 6-10 times their weight, the excess being subsequently removed to leave about 2 molecules of alkali for each molecule of cellulose.  The quantities of alkali and carbon bisulphide may be those usually employed in viscose manufacture, or smaller quantities may be employed and the process described in Specification 183,882, [Class 2 (ii), Cellulose &c.], utilized for the xanthogenation. The cellulose may be separated from the xanthogenate solution by treatment with acids, or carbon dioxide, or by heating, &c.  The separated cellulose may be employed for the production of cellulose esters or ethers, e.g. in accordance with Specifications 6463/15, 14101/15, 100,009, 101,555, 164,374, 164,375, 164,377, 176,420, 207,562, 263,939, 264,937, 277,721, 308,323, 309,201, 311,790, 312,095, 312,096, 325,822, [all in Class 2 (ii), Cellulose &c.], or viscose solutions, cuprammonium-cellulose solutions, &c. for the production of artificial silks, films, &c. The solutions obtained after separation from the impurities may be directly employed for the production of artificial silk, films, &c., preferably after further filtration.  The cellulose may be subjected to bleaching prior to rexanthogenation, esterification, or etherification.  Prior to esterification, the cellulose may be pretreated as in Specifications 249,173, 263,938, 288,657, 308,322, 308,348, 312,098, [all in Class 2 (ii), Cellulose &c.]. In an example, ligno-cellulosic material, e.g. wood in the form of fine chips or sawdust, is first treated with 5 per cent caustic soda to remove resins and is then steeped in 8-9 times its weight of 18 per cent caustic soda at a temperature not exceeding 25 DEG  C. until impregnated homogeneously after which excess liquor is removed to leave about 2 molecules of alkali to each molecule of cellulose; the alkali cellulose is allowed to ripen at 23-25 DEG  C. for 2-3 days and is then mixed with carbon disulphide, in quantity equal to one molecule of carbon disulphide per molecule of cellulose, for about 2-3 hours at 23-27 DEG  C.; the product is dissolved in 3-4 per cent caustic soda and the solution separated from the undissolved materials by filtration, centrifuging, &c., and the solution is then coagulated, preferably by spraying or atomizing the solution into an atmosphere of steam and/or gaseous hydrogen chloride.  The precipitated cellulose is desulphurized and washed.  In a second example, wood &c. after treatment to remove resins, is treated, in a vessel provided with stirrers, with a copper-oxide-ammonia solution of density 1,004.  About 100 parts by weight of solution are employed for every 15-16 parts dry weight of the material treated, and the mixture is churned, at room temperature or lower, for 10-15 hours, after which it is subjected to filtration &c. and the solution is then coagulated with 20-40 per cent sulphuric acid.  The precipitated cellulose is thoroughly washed with dilute acid and water to remove any residual copper.