Patent GB-690327-A (GB)
Title: Improvements in or relating to lubricating compositions
IPC: C10M137/16
Filed: 1948-02-03
Abstract: Phosphorus- and sulphur-containing reaction products are prepared by reacting a phosphorus sulphide with a cyclic ketone having at least 12 carbon atoms.  The ketone may be derived from the condensation of acetone to high molecular weight isophorone type fractions; the hydrogenated condensation products may also be used, and other ketones mentioned are dibutyl cyclohexanone, alkyl substituted carvomenthone, menthone, pulegone, carvone and camphor.  The phosphorus sulphide may be phosphorus pentasulphide or heptasulphide. The molecular ratio of phosphorus sulphide to ketone may be from 1 : 2 to 1 : 1.2.  The reaction product may be sulphurized, and before or after sulphurization may be treated with a metal compound, ammonia or an organic base to form a salt. Sulphurizing agents used may be sulphur, sulphur halides, alkali polysulphides, ammonium hydrogen sulphide and hydrogen sulphide. Metal compounds specified are the hydroxides, carbonates or oxides of the alkali, alkaline earth and heavy metals, a number of which are mentioned.  In a typical example, a mixture of cyclic unsaturated ketones containing at least 18 carbon atoms derived from the condensation of acetone is heated with phosphorus pentasulphide in the ratio 8 : 4 in an atmosphere of carbon dioxide, first at 60-80 DEG  C., and then for five hours at 160 DEG  C. The product is extracted with a non-aromatic hydrocarbon of boiling range 164-233 DEG  F., the solution filtered and the filtrate evaporated.  The product obtained is dissolved in mineral oil, lime added and the mixture heated and then filtered to remove excess lime.  The calcium salt may be sulphurized by heating with sulphur at 150-170 DEG  C. in an inert atmosphere.  The products are useful as additions to lubricants (see Group III).ALSO:A lubricating composition comprises a major proportion of a lubricating oil and a minor proportion of a phosphorus and sulphur containing product obtained by reacting a cyclic ketone having at least 12 carbon atoms with a phosphorus sulphide.  The unsaturated cyclic ketones derived from the condensation of acetone or diisobutyl ketone to high molecular weight isophorone type fractions or their hydrogenated products are preferably used; other ketones mentioned are dibutyl cyclohexanone, alkyl substituted carvomenthone, methone, pulegone, carvone and camphor.  The phosphorus sulphide may be phosphorus pentasulphide or heptasulphide.  The lubricating oil may be a mineral oil or a synthetic oil of the hydrocarbon or non-hydrocarbon type. The molecular ratio of phosphorus sulphide to ketone may be from 1 : 2 to 1 : 1.2 and preferably 0.1-2.0 per cent of the reaction product is used.  The reaction product may be sulphurized, and before or after sulphurization may be treated with a metal compound, ammonia or an organic base to form a salt.  Sulphurizing agents used may be sulphur, sulphur halides, alkali polysulphides, ammonium hydrogen sulphide and hydrogen sulphide.  Metal compounds specified are the hydroxides, carbonates or oxides of the alkali, alkaline earth and heavy metals, a number of which are mentioned.  In a typical example, a mixture of cyclic unsaturated ketones containing at least 18 carbon atoms derived from the condensation of acetone is heated with phosphorus pentasulphide in the ratio 8:4 in an atmosphere of carbon dioxide, first at 60 DEG -80 DEG C and then for five hours at 160 DEG C.  The product is extracted with a non-aromatic hydrocarbon of boiling range 164 DEG -233 DEG  F, the solution filtered and the filtrate evaporated.  The product obtained is dissolved in mineral oil, lime added and the mixture heated and then filtered to remove excess lime.  The lime salt recovered from the oil may be redissolved in oil and sulphurized by heating with sulphur. Optional additives mentioned are: detergents, for example salts of acids such as wool fat acids, paraffin wax acids, aromatic carboxylic acids, diphenol sulphides and sulphonic, sulphuric and phosphoric acids, for example calcium petroleum sulphonate or the calcium salt of an alkyl phenol-formaldehyde condensation product; non-metallic detergents such as lecithin and rapeseed oil; anti-oxidants such as alkyl-phenols, amino phenols and amines; corrosion inhibitors such as dicarboxylic acids, sulphonates and compounds such as d  cyano stearic acid; extreme pressure agents such as esters of phosphorus acids, sulphides and disulphides, sulphurized fatty oils, sulphurized olefins and chlorinated hydrocarbons.