Patent GB-416549-A (GB)
Title: Improvements in the manufacture of cellulose and lignocellulosic materials
IPC: D21C3/20
Filed: 1933-03-07
Abstract: Cellulose is produced from ligno-cellulosic materials by extracting the lignin from the materials by means of organic solvents or mixtures of organic solvents with water under a pressure in excess of that developed by the solvent or solvent composition.  Solvents specified are acetone, methyl ethyl ketone, methyl cyclohexanone, pyruvic acid, diacetone alcohol, tetrahydropyrone, ethyl alcohol, isopropyl alcohol, ethylene glycol, diethylene glycol, glycerol, diethyl ether, ethyl propyl ether, di-isopropyl ether, dioxane, methylene ethylene ether, dimethyl dioxane, mono- or di-methyl or -ethyl ethers of ethylene glycol, acetic acid, formic acid and methyl or ethyl formate or acetate.  These solvents may be used alone or in admixture with water.  There may be used mixtures of solvents of different polarity, for example, alcohols, ketones, aldehydes, esters, or acids may be employed in admixture with non-polar solvents such as benzene, toluene, xylene, carbon tetrachloride or hexachlorethane, or strongly polar liquids may be employed admixed with less strongly polar liquids, or again three or more organic liquids of different polarity may be employed.  The excess pressure may amount to 100 atmospheres or more.  At temperatures between 165 and 220 DEG  C., the total pressure may be between 20 and 150 atmospheres.  The excess pressure may be obtained by introducing compressed nitrogen or other inert gas.  To facilitate impregnation, the cellulosic material may be finely divided, or the method of Specification 374,047, [Group VIII], may be employed, according to which a liquid is caused to evaporate suddenly within the material. The ligno-cellulosic materials may be given a preliminary treatment with hot or boiling water, or water under pressure, or with alkali or acid solutions, or the solvent or solvent composition may be employed in association with small quantities of acid or basic substances. The products obtained may be converted, if required, after a pretreatment by the process of Specification 249,173, [Class 2 (ii)], into cellulose esters or ethers, or may be used in the manufacture of paper.  The following examples are given: (1) Wood chips are extracted with a 50--60 per cent aqueous solution of dioxane under an excess pressure of 20--25 atmospheres, and at a temperature of 170--190 DEG  C.  (2) Wood chips are first treated with a mixture of concentrated hydrochloric acid and acetic acid, and then extracted with a mixture of equal parts of isopropyl ether and ethyl alcohol under an excess pressure of 40 atmospheres and a temperature of 180--200 DEG  C.  (3) In the process of (1), the extraction liquid consists of a 50 per cent aqueous solution of ethyl alcohol.  (4) In the process of (1) or (2), the extraction liquid consists of equal parts of methylene chloride and methyl alcohol, and the temperature is 170 to 180 DEG  C.  (5) In the process of (1) or (2), the liquid used is a mixture of equal parts of dioxane and acetone.  (6) In the process of (1) or (2), the liquid used comprises alcohol, acetone and benzene.  The Provisional Specifications refer also to the use of a volatile liquid such as diethyl ether for the purpose of producing the excess pressure. Specifications 371,000, 371,001, 371,037, 371,038, [all in Group VIII], 398,801; 416,416 and 416,558, [both in Group VIII], also are referred to.