Patent GB-882529-A (GB)
Title: Phosphorus-and sulphur-containing lubricant additives and their preparation
IPC: C07F9/04
Filed: 1959-03-06
Abstract: Lubricant compositions comprise an additive prepared by heating a mixture of (1) a terpene hydrocarbon, (2) a monohydric saturated aliphatic or cycloaliphatic alcohol containing up to 18 carbon atoms and having at least one hydrogen on the carbon atom to which the hydroxyl group is attached, or a mixture of such alcohols, and (3) phosphorus pentasulphide (or elemental phosphorus and sulphur in the corresponding proportions), there being used a total of 1 to 2,5 moles of hydrocarbon and 1 to 3 moles of alcohol or alcohols per mole of sulphide, to a temperature in the range of about 70 DEG  to about 150 DEG  C., at which an acidic reaction product is formed; and then heating said product to a temperature in the range of about 60 DEG to about 150 DEG  C. with an amount of a basic inorganic compound of a metal above hydrogen in the electromotive series sufficient to neutralize said product.  The neutralizing agent may be an oxide, hydroxide, carbonate, bicarbonate or sulphide of lithium, rubidium, potassium, barium, strontium, calcium, sodium, magnesium, beryllium, aluminium, manganese, zinc, chromium, iron, cadmium, cobalt, nickel, tin or lead.  Zinc is preferred.  Compounds of the less basic metals may be made by double decomposition between a salt of such metal and a compound according to the invention with a more basic metal.  The phosphorus pentasulphide may be added to the heated mixture of terpene and alcohol in portions.  In a preferred embodiment, the terpene and alcohol are concurrently introduced into a slurry of phosphorus pentasulphide in an inert organic medium at about 90 DEG -150 DEG C.  Suitable media include the less reactive hydrocarbons stripped from previous terpene-P2S5-alcohol reactions, hydrocarbon solvents, mineral oils and synthetic lubricants. After the reaction an additional 0,1 to about 0,8 mole per mole of P2S5 used of the same or a different alcohol may be introduced and the mixture heated further prior to neutralization.  The intermediate acidic product may be treated with elemental sulphur prior to neutralization.  The additives may be added to mineral oils or synthetic ester lubricants, generally in amount to give about 0,01 to about 0,5% by weight of phosphorus.  A 4, 41-methylenebis-(2, 6-dialkylphenol) may be included.  Thickeners, other inhibitors, detergent-dispersants, pour point depressants, viscosity index improvers, antifoam agents, rust inhibitors, oiliness or film strength agents or dyes may also be present.ALSO:Phosphorus pentasulphide reaction products useful as lubricant additives are prepared by heating a mixture of (1) a terpene hydrocarbon, (2) a monohydric saturated aliphatic or cycloaliphatic alcohol containing up to 18 carbon atoms and having at least one hydrogen on the carbon atom to which the hydroxyl group is attached, or a mixture of such alcohols, and (3) phosphorus pentasulphide (or elemental phosphorus and sulphur in the corresponding proportions), there being used a total of 1 to 2.5 moles of hydrocarbon and 1 to 3 moles of alcohol or alcohols per mole of sulphide, to a temperature in the range of about 70 DEG C. to about 150 DEG C., at which an acidic reaction product is formed; and then heating said product to a temperature in the range of about 60 DEG C. to about 150 DEG C. with an amount of a basic inorganic compound of a metal above hydrogen in the electromotive series sufficient to neutralise said product.  The neutralising agent may be an oxide, hydroxide, carbonate, bicarbonate or sulphide of lithium, rubidium, potassium, barium, strontium, calcium, sodium, magnesium, beryllium, aluminium, manganese, zinc, chromium, iron, cadmium, cobalt, nickel, tin or lead.  Zinc is preferred. Compounds of the less basic metals may be made by double decomposition between a salt of such metal and a compound according to the invention with a more basic metal.  The phosphorus pentasulphide may be added to the heated mixture of terpene and alcohol in portions.  In a preferred embodiment, the terpene and alcohol are concurrently introduced into a slurry of phosphorus pentasulphide in an inert organic medium at about 90 DEG C.-150 DEG C.  Suitable media include the less reactive hydrocarbons stripped from previous terpene-P2S5-alcohol reactions, hydrocarbon solvents, mineral oils and synthetic lubricants.  After the reaction an additional 0.1 to about 0.8 mole per mole of P2S5 used of the same or a different alcohol may be introduced and the mixture heated further prior to neutralisation.  The intermediate acidic product may be treated with elemental sulphur prior to neutralisation.  The products are used as lubricant additives (see Group III).