Patent GB-925806-A (GB)
Title: Neutralized phospho-sulphurized hydrocarbons and lubricant compositions containing the same
IPC: C10M159/12
Filed: 1959-05-26
Abstract: A lubricant composition comprises a normally liquid oleaginous lubricant and, as an additive, an oil soluble, alkaline earth metal and boron containing complex obtained by reacting the phosphorus and sulphur-containing reaction product of a phosphorus sulphide and a normally non-gaseous hydrocarbon with a basic alkaline earth metal compound in the presence of boric acid, boric anhydride or a boric acid ester.  The additives may be used in amounts of from 0,01% to 15% in lubricant base oils, such as mineral lubricating oils, synthetic hydrocarbon lubricating oils, synthetic lubricating oils of the polyalkylene oxide type or of the polycarboxylic acid ester type, such as esters of adipic, sebacic and azelaic acids.  The additives can be used in combination with 0,02% to 10% of other additives such as zinc dialkyl dithiophosphates, and sulphurized terpenes. Concentrates of more than 15% up to 50% or more of the alkaline earth and boron-containing complexes, alone or in combination with other additives, can be used for blending with hydrocarbon oils or other oils to give a product containing 0,01% to 15% of the additive.ALSO:An oil-soluble alkaline earth metal and boron-containing complex is obtained by reacting the phosphorus and sulphur-containing reaction product of a phosphorus sulphide and a mono-olefin polymer or a mixture mono-olefin polymer and iso-mono-olefin polymers having molecular weights ranging from about 150 to about 50,000 or more with a basic alkaline earth metal compound in the presence of boric acid, boric anhydride or a p  boric acid ester at elevated temperature.  The phospho-sulphurized polymer may be neutralized with a basic alkaline earth metal compound in the presence of the boron compound, water and an alkanol of 1 to 3 carbon atoms.  Alternatively, the phosphosulphurized polymer may be hydrolysed at 200 DEG  to 500 DEG F., e.g. by introducing steam through the mass, the hydrolysed product neutralized with a basic alkaline earth compound, in the presence of said boron compound, water, an alkanol of 1 to 3 carbon atoms, or a mixture of such an alkanol and phenol or an alkylated phenol having 5 to 12 carbon atoms in the alkyl group or groups, at the reflux temperature of the alkanol, e.g. 155 DEG -185 DEG F.  The basic alkaline earth metal compound may be the oxide, hydroxide, carbonate or sulphide of calcium, barium, strontium or magnesium, barium oxide being preferred.  To facilitate handling, a slurry of the hydrolysed or unhydrolysed phospho-sulphurized reaction product in a lubricating oil, or any normally liquid hydrocarbon or oil may be used.  The products have an alkaline earth to phosphorus ratio of from 2:1 to 15:1.  Examples describe the reaction of polybutenes having a molecular weight of 750-800 with P2S5 at 450 DEG F. for 5-5 1/2 hours and the neutralization of the product, with or without a step of hydrolysis, with barium or calcium oxide in the presence of boric acid, water and methanol or a mixture of methanol and nonyl phenol at reflux temperature.ALSO:An oil-soluble, alkaline earth metal and boron-containing complex is obtained by reacting the phosphorus and sulphur-containing reaction product of a phosphorus sulphide and a normally non-gaseous hydrocarbon with a basic alkaline earth metal compound in the presence of boric acid, boric anhydride or a boric acid ester at elevated temperature.  The phospho-sulphurized reaction product may be hydrolysed after it is prepared or it may be used without being subject to hydrolysis. If the unhydrolysed reaction product is used, the said product and the hydrocarbon are neutralised with a basic alkaline earth metal compound, in the presence of the boron compound, water and an alkanol of 1 to 3 carbon atoms.  If a hydrolyzed product is to be used, the said reaction product is hydrolyzed at 200 DEG F.-500 DEG F., e.g. by introducing steam through the mass, and the hydrolyzed product is neutralized with a basic alkaline earth compound, in the presence of said boron compound, water, an alkanol of 1 to 3 carbon atoms, or a mixture of such an alkanol and phenol or an alkylated phenol having 5 to 12 carbon atoms in the alkyl group or groups, at the reflux temperature of the alkanol, e.g. 155-185 DEG F. The basic alkaline earth metal compound may be the oxide, hydroxide, carbonate or sulphide of calcium, barium, strontium or magnesium, barium oxide being preferred.  To facilitate handling, a slurry of the hydrolyzed or unhydrolyzed reaction product in a lubricating oil may be used or any normally liquid hydrocarbon or oil may be used.  The products have an alkaline earth to phosphorus ratio of from 2:1 to 15:1.  Examples of suitable hydrocarbons for the preparation of the phosphosulphurized products are given, polybutenes of molecular weight 750-800 being preferred.  The hydrocarbon is reacted with P2S5 or other phosphorus sulphide at 150 DEG F. to 600 DEG F., using 1 to 50% of the sulphide, for 1 to 10 hours.