Patent GB-427275-A (GB)
Title: Process for the destructive hydrogenation of solid carbonaceous materials
IPC: C10G1/00
Filed: 1934-09-11
Abstract: 427,275. Destructive hydrogenation. INTERNATIONAL HYDROGENATION PATENTS CO., Ltd., Vaduz, Leichtenstein.- (Assignees of 1. G. Farbenindustrie Akt.- Ges. ; Frankfort - on - Main, Germany) Sept. 11, 1934, No. 26046. Convention date, Sept. 29, 1933. [Class 32] In the destructive hydrogenation of solid carbonaceous materials, e.g. coal, peat, wood, &c., the carbonaceous material, prior to destructive hydrogenation, is impregnated with a solution of a catalyst substance in an organic solvent. Suitable catalysts are compounds of groups 2-8, particularly groups 5 and 6 of the periodic system and especially of molybdenum, tin, cobalt, iron or lead; also bromine, antimony or selenium and their compounds. Metal halides, oxides, thiocyanates, salts of thio-metal acids and compounds of phosphorus, also sulphides, are advantageous. Suitable organic solvents include organic acids, e.g. formic and acetic ; acid anhydrides, e.g. acetic; amino acids, e.g. glycocoll ; keto acids, e.g. pyroracemic, and levulic ; acid amides, e.g. formamide ; acid chlorides, e.g. acetyl and benzoyl; esters, e.g. acetic ester, glycol acetate, acetoacetic ester, benzoyl acetic ester, ethyl and methyl esters of formic, oxalic, benzine and salicylic acids, ethyl esters of boric, glyceric, lactic, xanthogenic and phthalic acids, and methyl esters of trichloracetic and tartaric acids ; alcohols, e.g. methyl, ethyl, benzyl, amyl and isopropyl, glycol, glycerine and cyclohexanol; ketones, e.g. acetone, acetyl acetone, acetonylacetone, ethyl propyl ketone, cyclohexanone, and acetophenone; aldehydes, e.g. benzaldehyde and phenyl-acetaldehyde; nitriles, e.g. acetonitrile and benzonitrile ; amines, e.g. pyridine, quinoline, aniline, ethylaniline; ethylamine, benzylamine, methyl aniline and methylamine; nitro compounds, e.g. nitrobenzene and nitromethane ; acid ethers, e.g. ethyl, benzyl and diphenyl ethers. Mixtures of such solvents may be employed. Thus, molybdic acid, ammonium molybdate, ammonium thiomolybdate, tungstic acid, ammonium tungstate, ammonium thiotungstate, chlorides or thiocyanates of metals of the iron group tin oxalate, ammonium phosphomolybdate, or iron or tin sulphides dissolved in formamide ; chlorides of iron, molybdenum &c., or thiocyanates of molybdenum, tungsten or iron dissolved in acetone ; cobalt or iron chloride, cobalt or molybdenum thiocyanate, molybdenum halides or molybdic acid dissolved in acetyl acetone or acetoacetic ester ; halides of molybdenum, iron or cobalt dissolved in acetonitrile ; tungsten compounds, e.g. tungstic acid or ammonium tungstate, or halides of metals of groups 5-8 dissolved in benzonitrile; halides and salts of thio-metal acids in aniline or pyridine ; and halides, thiocyanates or salts of thio-metal acids dissolved in alcohols may be employed. The carbonaceous material in finely comminuted state is sprayed with the solution at ordinary or elevated temperature and, if desired, the solvent is then distilled off. The pretreated coal &c., is preferably made into a paste with a high-boiling oil. In an example, finelyground, bituminous coal, after neutralization of basic constituents with sulphuric acid, is sprayed with molybdic acid dissolved in methyl alcohol so that 0À02 per cent of acid is absorbed ; after evaporation of the alcohol, the coal is made into a paste with heavy oil and treated with hydrogen under a pressure of 200 atmospheres and at a temperature of 470‹ C. A yield of 92À5 per cent of mainly liquid products is obtained, containing 3À7 per cent of asphalt. A solution of molybdic acid in formamide gives similar results.