Patent GB-822648-A (GB)
Title: Process for the preparation of grease-forming compositions and lubricating grease compositions
IPC: C04B33/13
Filed: 1957-01-25
Abstract: A process for the preparation of grease-forming compositions comprises adding an aniline compound to a fluid clay hydrogel, mechanically separating water, displacing the remaining water with a water-soluble organic liquid, adding a lubricating oil to the resultant organogel in a proportion sufficient to prevent collapse of the gel structure but insufficient to form a grease, evaporating the water-soluble organic liquid, and heating the mixture in an oxidizing atmosphere to oxidize the aniline compound.  The lubricating oil may be a refined, unrefined or semi-refined paraffinic, naphthenic or asphaltic base mineral oil (50 to 4000 SUS/100 DEG  F.) or blend thereof or a synthetic oil such as the esters of phosphorus- and/or silicon-containing and aliphatic dicarboxylic acids, e.g. tritolyl phosphate, tetrakis-(2-ethylhexyl)-silicate, dioctyl phthalate, and bis-(2-ethylhexyl) and bis-(3,5,5 - trimethylhexyl) - sebacates, halocarbon oils, e.g. fluorocarbons, and liquid organosilicone polymers, e.g. dimethyl and methyl phenyl silicone polymers which are extensively described and exemplified.  The aniline compounds include aniline itself and nuclear amino, methyl and hydroxyl substitution products thereof, e.g. the phenylene diamines, amino phenols, toluidines and xylidenes.  When heated in the oxidizing atmosphere, i.e. air with or without added oxygen, the ultimate oxidation product of aniline is aniline black, and although intermediate products such as emeraldine, nigraniline, and pernigraniline are effective it is preferred that at least 50% of the aniline be completely oxidized. The clays are preferably high-based exchange clays such as Wyoming bentonite or hectorite, though low-base exchange clays, e.g. Georgia clay, attapulgite, may be used.  The clay hydrogel is preferably treated with a mineral acid, e.g. H2SO4, HCl, H3PO4. Suitable water-soluble organic liquids include alcohols, ketones and esters, e.g. methyl, ethyl and isopropyl alcohols, acetone, methylethyl ketone and ethyl acetate.  The oil used to prepare greases from these concentrates is preferably the same as that already incorporated therein.  Examples comprise hectorite clay treated with 85% H3PO4, aniline, alcohol as volatile solvent, and a silicone oil.  The compositions were heated in a forced draught oven at 300 DEG  F. for 2 days and then milled with more silicone oil to form greases. Specification 736,270 is referred to.ALSO:A process for the preparation of greaseforming compositions (see Group III) comprises adding an aniline compound to a fluid clay hydrogel, mechanically separating water, displacing the water from the remaining concentrated clay hydrogel with a water-soluble organic liquid, adding a lubricating oil to the organogel in amount sufficient to preserve the gel structure during subsequent evaporation of the organic liquid but insufficient to form a grease structure, evaporating the water-soluble organic liquid and heating in an oxidizing atmosphere to oxidize the aniline compound.  A silicone oil may subsequently be added to form a grease containing 1 to 8% wt. of clay.  In an example 1 kg. of 2% wt. Hectorite clay in an aqueous slurry is acidified with 1.4 g. 85% H3PO4.  40 g. aniline are added, the water removed by filtration, and the filter coke washed with ethanol.  The aniline coated clay is then dispersed in 1000 ml. ethanol and 100 g. commercial silicone oil and the alcohol evaporated off.  The composition is then heated in a forced draught oven at 300 DEG  F. for 2 days to oxidize to aniline.  On milling the resulting composition with 100 g. silicone oil a smooth black grease is obtained.  Specification 736,270, [Group III], is referred to.