# US 4,141,744 A · Cellular inorganic resin cements, and process and compositions for forming them > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 4,141,744 A - Document ID: US4141744A - Status: Granted - Kind: A - Application number: 05/857,310 - Filed: 1977-12-05 - Granted: 1979-02-27 - Earliest claimed: 1976-07-19 - Assignees: Arthur D. Little, Inc. - Inventors: William L. Prior; Richard S. Lindstrom - Web page: https://patentgrep.com/patent/US4141744A ## CPC - C04B 28/30: containing magnesium cements {or similar cements}(magnesium oxide cements C04B28/10) - C04B 28/32: Magnesium oxychloride cements, e.g. Sorel cement - C04B 2111/275: {Making materials water insoluble} - C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE ## Abstract Process and composition for forming cellular inorganic plastic cements of magnesium oxychlorides and magnesium oxysulfates. A water slurry containing a magnesium salt, magnesium oxide and a water-soluble phosphate is formed and to it are added an anionic water-repellent surfactant and a blowing agent capable of providing a gaseous component in the strongly alkaline environment either through decomposition or reaction or through vaporization. Inorganic filler material may be added to impart strength, the maximum flexural strength being attained when at least about one-half of the filler comprises microfibers. The resulting cellular product is nonflammable and exhibits essentially zero flame spread, zero smoke density and zero fuel contribution. The cellular products are further characterized as being formed of substantially uniformly sized cells and having densities over a wide range. ## Claims ### Claim 1 A process for forming a cellular inorganic resin cement, comprising the steps of (a) forming a reactant water slurry of a magnesium salt selected from magnesium chloride hexahydrate and magnesium sulfate heptahydrate, a water-soluble phosphate and reactive magnesium oxide, the amount of said magnesium salt ranging from about 50% to about 75% by weight of the total weight of said water and said magnesium salt, said slurry having a viscosity ranging between about 700 and 15,000 centipoises; (b) blending into said slurry at least 0.5% by slurry weight of an anionic water-repellent surfactant; (c) uniformly dispersing throughout said slurry a blowing agent, capable of providing a gaseous component either through decomposition or reaction or through vaporization at a temperature below that at which said inorganic resin cement is cured, in an amount required to form said cellular inorganic resin cement with a predetermined density, thereby to provide a foaming composition capable of attaining said predetermined density and final cell structure before said foaming composition gels to form said inorganic resin cement; and (d) curing said foaming composition under conditions to retain essentially all of its water content. ### Claim 2 (depends on 1) A process in accordance with claim 1 wherein the molar ratio of said magnesium chloride hexahydrate to said magnesium oxide is between about 1 to 3 and about 1 to 8 and of said magnesium sulfate heptahydrate to said magnesium oxide is between about 1 to 3 and about 1 to 14. ### Claim 3 (depends on 1) A process in accordance with claim 1 wherein the amount of said magnesium salt in said slurry ranges from about 60% to about 75% by weight of the total weight of said water and said magnesium salt. ### Claim 4 (depends on 1) A process in accordance with claim 1 wherein said magnesium salt is magnesium chloride hexahydrate and the molar ratio of said magnesium salt to said magnesium oxide is about 1 to 5. ### Claim 5 (depends on 1) A process in accordance with claim 1 wherein the viscosity of said slurry is between about 700 and 2500 centipoises. ### Claim 6 (depends on 1) A process in accordance with claim 1 wherein the amount of said surfactant ranges between about 0.5% and about 3% by slurry weight. ### Claim 7 (depends on 5) A process in accordance with claim 5 wherein said surfactant is stearic acid or an inorganic salt thereof. ### Claim 8 (depends on 1) A process in accordance with claim 1 wherein said blowing agent decomposes in the strongly alkaline slurry to provide said gaseous component. ### Claim 9 (depends on 8) A process in accordance with claim 8 wherein said blowing agent is hydrogen peroxide in an amount up to about 2.5% (100% concentration basis) by said slurry weight. ### Claim 10 (depends on 9) A process in accordance with claim 9 including the step of blending into said slurry, prior to the addition of said hydrogen peroxide, a catalyst for the decomposition of said hydrogen peroxide. ### Claim 11 (depends on 1) A process in accordance with claim 1 wherein said blowing agent is a liquid which vaporizes above ambient temperature to provide said gaseous component. ### Claim 12 (depends on 11) A process in accordance with claim 11 wherein said liquid blowing agent is trichlorofluoromethane in an amount up to about 8% by said slurry weight. ### Claim 13 (depends on 1) A process in accordance with claim 1 wherein said curing of said foaming composition is carried out at a temperature between ambient and about 250.degree. C. ### Claim 14 (depends on 1) A process in accordance with claim 1 including the step of adding to said slurry a nucleating agent in an amount up to about 0.5% by said slurry weight. ### Claim 15 (depends on 1) A process in accordance with claim 1 including the step of forming said foaming composition into a predetermined configuration prior to said curing. ### Claim 16 (depends on 1) A process in accordance with claim 1 wherein said forming comprises molding with or without added heat and with or without added pressure. ### Claim 17 (depends on 1) A process in accordance with claim 1 including the step of incorporating a filler component into said cellular inorganic resin prior to said curing, the amount of said filler component being up to about 40% by weight of said cellular inorganic resin and less than that which will cause the collapse of said cellular inorganic resin. ### Claim 18 (depends on 17) A process in accordance with claim 17 wherein said filler component comprises at least in part microfibers up to about one-fourth inch in length. ### Claim 19 (depends on 18) A process in accordance with claim 18 wherein said microfibers comprise milled glass fibers. ### Claim 20 (depends on 18) A process in accordance with claim 18 wherein said microfibers comprise asbestos mine tailings. ### Claim 21 (depends on 18) A process in accordance with claim 18 wherein said microfibers comprise wollastonite fibers. ### Claim 22 (depends on 17) A process in accordance with claim 17 wherein said filler component comprises at least in part glass fibers longer than one-fourth inch. ### Claim 23 (depends on 22) A process in accordance with claim 22 wherein said glass fibers are in the form of a glass fiber mat. ### Claim 24 (depends on 17) A process in accordance with claim 17 wherein said filler component comprises at least in part a finely divided particulate material. ### Claim 25 (depends on 24) A process in accordance with claim 24 wherein said finely divided particulate material comprises mica, talc, perlite, vermiculite, polystyrene beads, glass microballoons or mixtures thereof. ### Claim 26 (depends on 17) A process in accordance with claim 17 wherein said step of incorporating said filler component comprises adding at least a portion of said filler component to said slurry, the amount of said filler component added to said slurry being no greater than that which raises the viscosity of said slurry to about 100,000 centipoises. ### Claim 27 (depends on 26) A process in accordance with claim 26 wherein said filler component is added to said slurry prior to dispersing said blowing agent throughout said slurry. ### Claim 28 (depends on 26) A process in accordance with claim 26 wherein said filler component is dispersed throughout said slurry with said blowing agent. ### Claim 29 (depends on 26) A process in accordance with claim 26 wherein said filler component comprises at least 50% by weight of microfibers ranging in length between about 1/32 inch and 1/4 inch. ### Claim 30 (depends on 26) A process in accordance with claim 26 wherein said filler component comprises at least in part fibers longer than one-fourth inch or particulate material. ### Claim 31 (depends on 26) A process in accordance with claim 26 including the steps of forming said foaming composition into a predetermined configuration and adding at least a portion of said filler component to said foaming composition during said forming of said predetermined configuration. ### Claim 32 (depends on 31) A process in accordance with claim 31 wherein said filler component added during said forming comprises microfibers ranging in length between about 1/32 inch and 1/4 inch. ### Claim 33 (depends on 31) A process in accordance with claim 31 wherein said filler component added during said forming comprises fibers longer than one-fourth inch or particulate material. ### Claim 34 (depends on 33) A process in accordance with claim 33 wherein said fibers added during said forming are glass and are provided as a glass fiber mat and said forming said predetermined configuration includes laminating said glass fiber mat with said foaming composition. ### Claim 35 (depends on 31) A process in accordance with claim 31 wherein said step of forming said predetermined configuration comprises molding said foaming composition within a mold cavity, said molding being performed with or without added heat and with or without added pressure. ### Claim 36 (depends on 35) A process in accordance with claim 35 including the step of lining said mold cavity with a mixture of a filler component and said reactant slurry without a blowing agent. ### Claim 37 (depends on 36) A process in accordance with claim 36 wherein said filler component in said mixture lining said mold cavity comprises fibers greater than one-fourth inch in length. ### Claim 38 (depends on 31) A process in accordance with claim 31 including the step of applying a surface finish to said predetermined configuration subsequent to curing said cellular inorganic resin cement. ### Claim 39 A composition for forming a cellular inorganic resin cement, comprising in combination (a) a reactant water slurry of a magnesium salt selected from magnesium chloride hexahydrate and magnesium sulfate heptahydrate, reactive magnesium oxide and at least one water-soluble phosphate, said slurry having a viscosity ranging between about 700 and 15,000 centipoises and being one in which the solids concentration of said magnesium salt ranges between about 50% and about 70% by weight of the total weight of water of said slurry and said magnesium salt; (b) an anionic, water-repellent surfactant present in said slurry in an amount between about 0.5% and about 3% by slurry weight; and (c) a blowing agent, capable of providing a gaseous component either through decomposition or reaction or through vaporization in the strongly alkaline environment of said slurry, uniformly dispersed throughout said slurry and present in an amount required to form said cellular inorganic resin cement with a predetermined density, thereby to provide a foaming composition capable of attaining said predetermined density and final cell structure before said foaming composition gels to form said cellular inorganic resin cement and from which essentially no water is removed upon curing. ### Claim 40 (depends on 39) A composition in accordance with claim 39 wherein the molar ratio of said magnesium chloride hexahydrate to said magnesium oxide ranges between about 1 to 3 and about 1 to 8 and of said magnesium sulfate heptahydrate to said magnesium oxide between about 1 to 3 and about 1 to 14. ### Claim 41 (depends on 39) A composition in accordance with claim 39 wherein the amount of said magnesium salt in said slurry ranges from about 60% to about 75% by weight of the total weight of said water and said magnesium salt. ### Claim 42 (depends on 39) A composition in accordance with claim 39 wherein said magnesium salt is magnesium chloride hexahydrate and the molar ratio of said magnesium salt to said magnesium oxide is about 1 to 5. ### Claim 43 (depends on 39) A composition in accordance with claim 39 wherein the viscosity of said slurry is between about 700 and 2500 centipoises. ### Claim 44 (depends on 39) A composition in accordance with claim 39 wherein the amount of said surfactant ranges between about 0.5% and about 3% by slurry weight. ### Claim 45 (depends on 44) A composition in accordance with claim 44 wherein said surfactant is stearic acid or an inorganic salt thereof. ### Claim 46 (depends on 39) A composition in accordance with claim 39 wherein said blowing agent decomposes in the strongly alkaline slurry to provide said gaseous component. ### Claim 47 (depends on 46) A composition in accordance with claim 46 wherein said blowing agent is hydrogen peroxide in an amount up to about 2.5% (100% concentration basis) by said slurry weight. ### Claim 48 (depends on 47) A composition in accordance with claim 47 including a catalyst for the decomposition of said hydrogen peroxide. ### Claim 49 (depends on 48) A composition in accordance with claim 48 wherein said decomposition catalyst is potassium permanganate in an amount up to about 0.5% by said slurry weight. ### Claim 50 (depends on 39) A composition in accordance with claim 39 wherein said blowing agent is a liquid which vaporizes above ambient temperature to provide said gaseous component. ### Claim 51 (depends on 50) A composition in accordance with claim 50 wherein said liquid blowing agent is trichlorofluoromethane in an amount up to about 8% by said slurry weight. ### Claim 52 (depends on 39) A composition in accordance with claim 39 including a nucleating agent in an amount up to about 0.5% by said slurry weight. ### Claim 53 (depends on 39) A composition in accordance with claim 39 including a filler component present in an amount up to about 40% by said slurry weight, and less than that which will cause the collapse of the cellular inorganic resin formed from said composition, said composition being further characterized as having a viscosity no greater than about 100,000 centipoises. ### Claim 54 (depends on 53) A composition in accordance with claim 53 wherein said filler component comprises at least 50% by weight of microfibers ranging in length between about 1/32 inch and 1/4 inch. ### Claim 55 (depends on 54) A composition in accordance with claim 54 wherein said microfibers comprise milled glass fibers. ### Claim 56 (depends on 55) A composition in accordance with claim 55 wherein said milled glass fibers are water-bonded. ### Claim 57 (depends on 54) A composition in accordance with claim 54 wherein said microfibers comprise mineral fibers. ### Claim 58 (depends on 57) A composition in accordance with claim 57 wherein said mineral fibers are asbestos mine tailings. ### Claim 59 (depends on 57) A composition in accordance with claim 57 wherein said mineral fibers are wollastonite fibers. ### Claim 60 (depends on 53) A composition in accordance with claim 53 wherein said filler component comprises at least in part fibers greater than one-fourth inch in length. ### Claim 61 (depends on 53) A composition in accordance with claim 53 wherein said filler component comprises a finely divided particulate material. ### Claim 62 (depends on 61) A composition in accordance with claim 61 wherein said finely divided particulate material comprises mica, talc, perlite, vermiculite, polystyrene beads, glass microballoons or mixtures thereof. ### Claim 63 A cured cellular inorganic resin cement having essentially uniformly sized cells, a density ranging between about 5 and about 100 pounds per cubic foot and being further characterized as exhibiting essentially zero flame spread, zero smoke density and zero fuel contribution, said inorganic resin cement being the reaction product of reactive magnesium oxide and an aqueous, soluble phosphate-containing gaging solution of a magnesium salt selected from magnesium chloride hexahydrate and magnesium sulfate heptahydrate and having a concentration of said magnesium salt ranging between about 50% and about 75% by weight of said gaging solution, said reaction product being further characterized in that essentially all of the water of said gaging solution and the water of hydration of said magnesium salt are consumed in the reaction and contained in said inorganic resin cement. ### Claim 64 (depends on 63) A cellular inorganic resin cement in accordance with claim 63 wherein said cells have diameters up to about 3mm. ### Claim 65 (depends on 63) A cellular inorganic resin cement in accordance with claim 63 wherein the molar ratio of said magnesium chloride hexahydrate to said magnesium oxide ranges between about 1 to 3 and about 1 to 8 and of said magnesium sulfate heptahydrate to said magnesium oxide between about 1 to 3 and about 1 to 14. ### Claim 66 (depends on 63) A cellular inorganic resin cement in accordance with claim 63 including a filler component present in an amount up to about 40% by weight of said cement. ### Claim 67 (depends on 66) A cellular inorganic resin cement in accordance with claim 66 wherein said filler component comprises at least 50% by weight microfibers up to one-fourth inch long. ### Claim 68 (depends on 67) A cellular inorganic resin cement in accordance with claim 67 wherein said microfibers are glass. ### Claim 69 (depends on 67) A cellular inorganic resin cement in accordance with claim 67 wherein said microfibers are milled glass fibers. ### Claim 70 (depends on 69) A cellular inorganic resin cement in accordance with claim 69 wherein said milled glass fibers are water-bonded. ### Claim 71 (depends on 67) A cellular inorganic resin cement in accordance with claim 67 wherein said microfibers comprise mineral fibers. ### Claim 72 (depends on 71) A cellular inorganic resin cement in accordance with claim 71 wherein said mineral fibers are asbestos mine tailings. ### Claim 73 (depends on 61) A cellular inorganic resin cement in accordance with claim 61 wherein said mineral fibers are wollastonite fibers. ### Claim 74 (depends on 66) A cellular inorganic resin cement in accordance with claim 66 wherein said filler component comprises at least in part long fibers greater than one-fourth inch in length. ### Claim 75 (depends on 74) A cellular inorganic resin cement in accordance with claim 74 wherein said long fibers are glass in the form of a woven or nonwoven mat. ### Claim 76 (depends on 75) A cellular inorganic resin cement in accordance with claim 75 wherein said cellular inorganic resin cement is formed as a cellular cement/glass fiber laminate. ### Claim 77 (depends on 76) A cellular inorganic resin cement in accordance with claim 76 wherein said cellular cement of said laminate contains microfibers distributed therethrough. ### Claim 78 (depends on 66) A cellular inorganic resin cement in accordance with claim 66 further characterized as being formed into a predetermined configuration. ### Claim 79 (depends on 78) A cellular inorganic resin cement in accordance with claim 78 wherein selected surfaces of said predetermined configuration have bonded thereto said inorganic resin cement in noncellular form. ### Claim 80 (depends on 79) A cellular inorganic resin cement in accordance with claim 79 wherein said noncellular inorganic resin cement has a filler component incorporated therein. ### Claim 81 (depends on 80) A cellular inorganic resin cement in accordance with claim 80 wherein said filler component comprises fibers greater than one-fourth inch in length. ### Claim 82 (depends on 78) A cellular inorganic resin cement in accordance with claim 78 including a surface finish.