# US RE31,307 E · Method for preparing clay-based grease compositions > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US RE31,307 E - Document ID: USRE31307E - Status: Granted - Kind: E - Application number: 06/192,060 - Filed: 1980-09-29 - Granted: 1983-07-12 - Earliest claimed: 1976-08-03 - Assignees: Shell Internationale Research Maatschap IIJ B.V. - Inventors: Kenneth A. MacKenzie; Abraham Verhoeff - Web page: https://patentgrep.com/patent/USRE31307E ## Abstract An improved method for preparing clay-based grease compositions is described whereby a clay containing pre-grease is prepared and a water separated from the clay-bearing pre-grease prior to the addition of an epoxide which is cured, e.g., simultaneously with the dehydration of the pre-grease. The grease compositions prepared in this manner show improved water resistance over those wherein the epoxide is added prior to separation of the water phase and the grease is also more responsive to the addition of conventional grease additives such as extreme pressure additives, anti-corrosion additives and anti-oxidants. ## Claims ### Claim 1 In the method for preparing a clay-bearing grease which comprises mixing an aqueous clay hydrogel and a conjugate acid surfactant formed from an acid and an organic amine, which mixture is combined, with mixing, with a major proportion of a lubricating oil to result in a pre-grease phase containing the oil, clay and surfactant and a water phase; followed by separating the pre-grease phase from the water phase; the improvement which comprises: (a) mixing with the pre-grease, from about 0.1 to about 20 weight percent of an epoxide, based upon the weight of the pre-grease before or after a dehydration step; (b) heating the mixture [to a temperature not greater than 250.degree. F.] to cure the epoxide; and (c) milling the dried and cured mixture to form a clay-bearing grease. ### Claim 2 (depends on 1) The method of claim 1, wherein the curing and dehydration step is performed by vacuum distillation. ### Claim 3 (depends on 1) The method of claim 1, wherein the epoxide is a polyglycidyl polyether. ### Claim 4 (depends on 3) The method of claim 3, wherein the polyglycidyl polyether is the diglycidyl ether of a diphenylol propane. ### Claim 5 (depends on 1) The method of claim 1, wherein the mixing of conjugate acid surfactant clay hydrogel and lubricating oil is accomplished by means of turbulent pipeline flow. ### Claim 6 (depends on 1) The method of claim 1, wherein the clay hydrogel is formed from a bentonitic clay. ### Claim 7 (depends on 1) The method of claim 1, wherein the clay is hectorite clay. ### Claim 8 (depends on 1) The method of claim 1, wherein the acid used in the formation of the conjugate acid surfactant is phosphoric acid. ### Claim 9 (depends on 1) The method of claim 1, in which the acid used in the formation of the conjugate acid surfactant is a C.sub.1 -- to C.sub.4 -- aliphatic monocarboxylic acid. ### Claim 10 (depends on 1) The method of claim 1, wherein the conjugate acid surfactant is formed from a compound selected from the group comprising: reaction products of fatty acids and polyalkylene polyamines, and fatty polyamines. ### Claim 11 (depends on 1) The method of claim 1, wherein the concentration of the conjugate acid surfactant is from 10% w to 150% w of the stoichiometric amount needed to counteract the anionic charges on the clay. ### Claim 12 (depends on 1) The method of claim 1, wherein the clay is titrated with the conjugate acid surfactant to a zero electrometric potential. ### Claim 13 (depends on 1) The method of claim 1, wherein antioxidants, high pressure additives and anti-corrosion additives are added in amounts of from 0.1 to 20% by weight of each additive, based upon the weight of the final grease, the total amount of addivites being a minor portion of the grease. ### Claim 14 In the method for preparing a clay-bearing grease which comprises mixing an aqueous clay hydrogel and a conjugate acid surfactant formed from an acid and an organic amine, which mixture is combined, with mixing, with a major proportion of a lubricating oil to result in a pre-grease phase containing the oil, clay and surfactant and a water phase; followed by separating the pre-grease phase from the water phase; the improvement which comprises: (a) mixing with the pre-grease, from about 0.1 to about 20 weight percent of a polyepoxide, based upon the weight of the pre-grease; (b) heating the mixture to a temperature not greater than 250.degree. F. to simultaneously cure the polyepoxide and dehydrate the mixture; and (c) milling the dried and cured mixture to form a clay-bearing grease. ### Claim 15 A clay-bearing grease composition prepared by the method which comprises: (a) forming a clay hydrogel of clay of sufficient ion exchange capacity and water; (b) intimately mixing therewith a conjugate acid surfactant formed from an acid and an organic amine compound; (c) intimately mixing with the mixture formed in step (b) a major proportion of lubricating oil whereby a water phase and pre-grease phase comprising curds of oil, clay, surfactant and minor amounts of water are formed; (d) separating the water phase from the wet pre-grease phase; (e) mixing and reacting with the amine groups of the amine in the pre-grease from about 0.1 to about 20 weight percent of an epoxide, based upon the weight of the pre-grease; (f) heating the mixture [to a temperature not greater than 250.degree.] to cure the epoxide; and (g) milling the dried and cured mixture to form the clay-bearing grease. ### Claim 16 (depends on 15) The grease of claim 15 wherein the clay is a bentonitic clay. ### Claim 17 (depends on 15) The grease of claim 15 wherein the clay is a hectorite clay. ### Claim 18 (depends on 15) The grease of claim 15 wherein the epoxide is a monoepoxide or polyepoxide having epoxy equivalent values of from 1.5 to about 4. ### Claim 19 In the method for preparing a clay-bearing grease which comprises mixing an aqueous clay hydrogel and a conjugate acid surfactant formed from an acid and an organic amine, which mixture is combined, with mixing, with a major proportion of a lubricating oil to result in a pre-grease phase containing the oil, clay and surfactant and a water phase; followed by separating the pre-grease phase from the water phase; the improvement which comprises: (a) mixing with the pre-grease, from about 0.1 to about 20 weight percent of an epoxide, based upon the weight of the pre-grease; (b) heating the mixture to a temperature not greater than 250.degree. F. to dehydrate the pre-grease and cure the epoxide; and (c) milling the dried and cured mixture to form a clay-bearing grease.