Patent GB-1025008-A (GB)
Title: Phosphorus sulphide-hydrocarbon products, high barium-content carbonated salts thereof, and methods for preparing the same
IPC: C07F9/04
Filed: 1963-12-17
Abstract: Lubricating oil additives are formed by subjecting a phosphorus sulphide-hydrocarbon reaction product to the action of an oxygen-containing gas at 100 DEG  to 200 DEG  C., and then forming a high barium-content salt by any suitable prior art process.  For the preferred process for forming the high barium-content salt (see Division C3).  The phosphorus sulphide-hydrocarbon reaction product is normally obtained by reacting a homo- or co-polymer of a monoolefine, although non-polymeric hydrocarbons may also be used, with a phosphorus sulphide and the oxygen-containing gas may be air. In the preferred preparation of the barium salt the air-treated phosphorus sulphide-hydrocarbon reaction product is dissolved in a hydrocarbon solvent which is advantageously a mineral oil which need not be removed from the final product, the oil solution of the product thus obtained being directly blendable with a base lubricating oil.  Suitable blends comprise a major proportion of a lubricating oil and from 0.1 to 30% by weight on an oil free basis, of the high barium content salt.ALSO:Phosphorus sulphide-hydrocarbon reaction products are subjected to the action of an oxygen-containing gas at 100 DEG  to 200 DEG  C. to produce a product suitable for conversion to a barium salt.  The phosphorus sulphide - hydrocarbon reaction product may be prepared by reacting the hydrocarbon with a phosphorus sulphide in a non-oxidizing atmosphere.  The oxygen-containing gas may be air and it is preferably introduced into the stirred reaction mass at a temperature of 150 DEG  C.  The air treatment is generally carried out for 1 to 5 hours.ALSO:A lubricating oil additive which is a high barium-content salt of a phosphorus sulphide-polyolefine reaction product is prepared by (1) subjecting a phosphorus sulphide-polyolefine reaction product to the action of an oxygencontaining gas at 100 to 200 DEG  C., (2) preparing a hydrocarbon solution of said oxygen treated phosphorus sulphide-polyolefine reaction product, (3) forming a reaction mixture of (a) the oxygen treated polyolefine solution and (b) a methanol solution of barium methylate containing from 20 to 40 mols of methanol per mol of barium, in an amount to supply to said reaction mixture an excess of barium methylate over that required to form a normal barium salt of said phosphorus sulphide-polyolefine reaction product and (c) water, in an amount to supply to said reaction mixture from 2 to 4 mols of water per mol of barium supplied by the barium methylate solution, (4) heating the reaction mixture at a temperature of from 65 DEG  to 200 DEG  C. and distilling off alcohol and water therefrom, whereby a basic barium salt of the phosphorus sulphide-polyolefine reaction product is formed, (5) intimately contacting the reaction mixture with carbon dioxide gas while maintaining said mixture at a temperature of 90 DEG  to 200 DEG  C. to incorporate into said basic barium salt 0.3 parts by weight of carbon dioxide per part of basic barium present in said salt, (6) lowering the temperature of the reaction mixture to a level below 65 DEG  C., (7) adding additional methanol solution of barium methylate and water to the reaction mixture in an amount to supply from 0.25 to 4 parts by weight of barium per part of phosphorus supplied to the reaction mixture in step 3 by the phosphorus sulphide-polyolefine reaction product, the mol proportions of methanol and water to barium being the same as in step (3), (8) again heating the reaction mixture at a temperature of from 65 DEG  to 200 DEG  C. and distilling off alcohol and water therefrom and (9) filtering the reaction mixture to recover a hydrocarbon solution of the high barium content salt of the phosphorus sulphide-polyolefine reaction product.  In step (1) the oxygen-containing gas may be air and the preferred temperature is 150 DEG  C. and the air is preferably introduced at the rate of 0.15 to 2.00 litres per minute per kilogram of phospho-sulphurized hydrocarbon being treated.