Patent GB-728779-A (GB)
Title: Processes for the preparation of partially dehydrated inorganic gel compositions and thickened lubricating oil compositions
Filed: 1952-12-19
Abstract: Polyamino hydroxy compounds are prepared by condensing halohydrins with ammonia or a primary or secondary amine, and the product is converted to a partial amide having between 1/4 and 3/4 of its amino groups in the amide form, by reaction with higher fatty acids or rosin acids, such as stearic acid or acids derived from tall oil or animal or vegetable oils and fats. In an example, epichlorhydrin is condensed with ammonia to form 1,3-diamino-2-hydroxy propane and dimers and higher polymers thereof, and the mixture amidated by reaction with tallow fatty acids.ALSO:Thickened lubricating oil compositions, especially greases, are prepared by heating a mixture of an hydrous inorganic colloid and a surface-active agent at a temperature above 60 DEG  C. for at least 30 minutes, removing a substantial proportion of water as a liquid from the mixture, mixing with a water-immiscible lubricating oil and further dehydrating the composition.  Inorganic colloids referred to natural or synthetic clays such as montmorillonite clays, bentonite and hectorite, and clays containing aluminium, magnesium and beryllium silicates; and inorganic oxides, hydroxides, sulphides, silicates, sulphates, chlorides or mixtures thereof; for example, silica, silica and magnesia or magnesium silicate.  The surface-active agents may be cationic, anionic or non-ionic.  Cationic agents specified are organic ammonium, phosphonium, sulphonium, stibonium and arsonium compounds and amine salts; for example, trimethyl heptadecyl ammonium chloride, dimethyl heptadecyl ammonium chloride, octadecyl heptadecyl ammonium bromide, dimethyl dioctadecyl ammonium bromide, tridodecyl ammonium chloride, heptadecyl ammonium acetate, triphenyl alkyl phosphonium or stibonium halides and dialkyl or diaryl phosphonium &c., sulphonium halides; aliphatic long chain amines such as octadecylamine and polyamines and amido-amines, partial amides of higher fatty acids such as stearic acid, tall oil acids or resin acids, with aliphatic polyamino-hydroxy compounds such as the condensation products of halohydrins such as epichlorohydrin with ammonia or a primary or secondary amine, or the partial amide of the condensation product of acrolein and ammonia.  Anionic agents specified are higher fatty or hydroxy fatty acids such as stearic acid and 12-hydroxy-stearic acid and soaps thereof, such as aluminium or lead 12-hydroxystearate; and calcium naphthenate.  The amount of surface-active agent may be at least 25 per cent. of the weight of inorganic colloid. Lubricating oils referred to are mineral oils, phosphorus esters such as trioctyl phosphate, di (2-ethylhexyl) hexane-phosphonate and bis-1, 3-(dioctyl phosphono) butane, esters of aliphatic dicarboxylic acids such as bis (2-ethylhexyl) sebacate and bis (isooctyl) adipate, polymeric oxyalkylene compounds such as polypropylene oxide and its copolymers with ethylene oxide and polymers of glycols such as trimethylene glycol.  In one example, a silica hydrosol is prepared from sodium silicate solution and sulphuric acid and the gel filtered and washed.  A partial amide of tallow fatty acids and an epichlorohydrinammonia condensation product is added to the hydrogel and the mixture heated for 55 minutes up to 95-97 DEG  C. and then filtered.  The partially dehydrated gel is mixed with mineral lubricating oil, milled and dried and then milled again to obtain a grease structure.  In another example, hectorite clay is dispersed in water to which dimethyl dioctadecyl ammonium bromide is added and the mixture heated at 85 DEG  C. for 30 minutes. The onium clay so formed is separated from the water phase by centrifuging, and then mixed with mineral lubricating oil, dehydrated and subjected to shearing to form a lubricating grease.