Patent GB-474305-A (GB)
Title: Improvements in or relating to the manufacture of cellulose from lignocellulosic materials
IPC: D21C3/00
Filed: 1936-05-05
Abstract: A process for the manufacture of cellulose for the manufacture of paper, cellulose solutions or cellulose derivatives comprises removing lignin from lignocellulosic material, e.g. wood, straw or grass, by treatment with a mixture of a lower aliphatic acid, e.g. formic or acetic acid and nitric acid, followed by a treatment with alkali.  The acid may be concentrated or in aqueous solution, e.g. aqueous acetic acid of concentration of the order of 15--75 per cent. The aliphatic acid or its solution may be employed in an amount of 10--25 or more times the weight of lignocellulosic material.  The amount of nitric acid employed is 10--30 per cent of the weight of lignocellulosic material.  The acid treatment may be at elevated temperature up to 100 DEG  C., e.g. 75--95 DEG  C.  The pressure may be atmospheric, or the vapour pressure of the liquor or higher, e.g. produced by inert gases such as nitrogen.  With pressure substantially exceeding atmospheric less nitric acid is needed than at atmospheric pressure.  At 95 DEG  C., the treatment may take 1--4 hours and at 75 DEG  C., 12--16 hours.  After acid treatment, the material may be pressed, centrifuged and washed. The alkali treatment may be with cold moderately strong alkali, e.g. 7--20 per cent caustic soda at 10--25 DEG  C. or with hot alkali of lower concentration, e.g. less than 5 per cent at the boiling point under atmospheric pressure, or at boiling point or lower under superatmospheric pressure, advantageously in excess of the vapour pressure of the solution, nitrogen or other gas being introduced. Thus, the pressure may be 6--10 atms. above the vapour pressure of the solution and the temperature 100--130 DEG  C. The alkali treatment may be two-fold, first with hot dilute alkali, and then with cold more concentrated alkali.  The treatment with acid may also be preceded by an alkali treatment, e.g. with 1--5 per cent caustic alkali at 100 DEG  C. or more, continued until a substantial proportion of the lignin has been removed.  In any case, the materials may first be treated with dilute alkali or with water at atmospheric or higher pressure to remove gums, resins and like materials.  Part of the lignin may also be removed by an acid treatment, e.g. with sulphite liquor before the acid treatment of the invention.  Any one or more of the various treatments may be carried out in stages, and if desired a washing with water or alkaline solution may be interposed between two acid treatments.  The lignocellulosic material is preferably finely divided, e.g. as wood chips, sawdust, or mechanical wood pulp.  The cellulose obtained may be bleached with chlorine or hypochlorite.  For the manufacture of organic esters of cellulose, the cellulose may be pretreated with acids, e.g. formic, acetic, hydrochloric, sulphuric, or nitric acid. Treatment with a lower fatty acid which may be as liquid or vapour may be combined with introduction of a catalyst for the esterification process.  Mineral acid used during a pretreatment may be neutralized before esterification.  Further details of pretreatment are given in French Specification 565,654, and in British Specifications 263,938 and 312,098, [both in Class 2 (ii)]. In an example, sawdust is heated to 95 DEG  C. at atmospheric pressure with 20 times its weight of 25 per cent aqueous acetic acid containing 1 per cent nitric acid for 3 hours.  Acid is removed by filtration, the solids washed, and boiled with 3,4 per cent caustic soda.  The product is bleached with chlorine and boiled with 2 per cent NaOH and/or treated in the cold with 12 per cent NaOH. According to the Provisional Specification, the process may be applied to the purification of chemical pulps, hydrogen peroxide may be substituted partly or wholly for the nitric acid, the acid treatment need not be followed by a treatment with alkali.