Patent GB-466996-A (GB)
Title: Improvements in the manufacture and production of high quality lubricating oils
IPC: C10G71/02
Filed: 1936-08-17
Abstract: Lubricating-oils are produced by polymerization of ethylene or gas mixtures containing it by means of aluminium chloride or its addition compounds with olefines in the presence of inert solvents, the gases being free from oxygen and sulphur and their compounds, free iron being excluded from the reaction, and anhydrous aluminium chloride containing less than 5 per cent, preferably less than 2,5 per cent of non-sublimable residue being employed.  Purification of the gases can be effected first by physical methods such as adsorption, or liquefaction and fractional distillation but, for removing the last traces of impurities such as carbon oxides or oxysulphide, hydrogen sulphide, aldehydes, alcohols, esters, and mercaptans, chemical methods such as treatment with caustic alkali, organic bases, salts of strong bases with weak acids, e.g. the sodium salt of alanine, calcium chloride, chromic acid, or fused sodamide must be used, advantageously at about 5--50 atmos.  Gases such as hydrogen, nitrogen or methane are harmless but the concentration of ethylene should generally be at least 70 per cent.  The reaction vessels must be free from ordinary iron or non-alloy steels and may be constructed of nickel or chromium or steels alloyed therewith, or lined with lead, tin or zinc.  The aluminium chloride should contain less than 5 per cent of residue such as aluminium oxide, hydroxide or oxychloride, or iron oxide, and is preferably in the form of its liquid addition compounds with olefines to prevent hydrolysis by atmospheric moisture. Suitable inert solvents are paraffin hydrocarbon mixtures such as petroleum ether or hydrogenation products of cracked paraffin waxes, fats, and fatty oils, fused paraffin waxes, or crude products or first runnings of a previous polymerization. Reaction is slow at room temperature or below and the reaction vessel is preferably heated to 70--80 DEG  C. or higher when the reaction may cause a temporary rise up to 230 or 250 DEG  C.  The products are miscible in all proportions with natural lubricating oils.  In examples: (1) gas obtained by dehydration of ethanol, after washing at 60 atmos. with concentrated caustic soda and treating with anhydrous calcium chloride, is forced at 50 atm. into an alloy steel autoclave containing the aluminium chloride and petroleum ether and heated to 120 DEG  C.; (2) a similar purified ethylene is treated at 90 DEG  C. using a first runnings oil, as obtained in working up the product of (1), as solvent; (3) an addition compound obtained by treating the aluminium chloride with first runnings and a paraffin wax cracking product is used as catalyst; (4) a hydrogenated paraffin wax cracking product is used as the solvent.ALSO:Lubricating-oils are produced by polymerization of ethylene by means of aluminium chloride in the presence of inert solvents, the gas being free from oxygen and sulphur and their compounds, free iron being excluded from the reaction, and anhydrous aluminium chloride containing less than 5 per cent of non-sublimable residue being employed.  The products are miscible in all proportions with natural lubricating oils.