# US 9,752,014 B2 · Process for the manufacture of nano-scale, primary, coated hydrotalcite and hydrotalcite > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,752,014 B2 - Document ID: US9752014B2 - Status: Granted - Kind: B2 - Application number: 13/976,737 - Filed: 2011-12-21 - Published: 2013-12-12 - Granted: 2017-09-05 - Earliest claimed: 2010-12-27 - Assignees: K+S Aktiengesellschaft - Applicants: Jochen Brod; David Christopher Glende - Inventors: Jochen Brod; David Christopher Glende - Web page: https://patentgrep.com/patent/US9752014B2 ## CPC - C08K 9/02: Ingredients treated with inorganic substances - B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites - C01F 7/785: Hydrotalcite - C09C 1/40: Compounds of aluminium {(C09C1/0009, C09C1/0015, C09C1/0078, C09C1/32 take precedence)} - C09C 1/42: Clays - C01P 2002/22: layered hydroxide-type, e.g. of the hydrotalcite-type - C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer - C01P 2006/12: Surface area - C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09) - B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES - C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00}) - C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS} - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS ## Abstract The invention presented concerns a process for the manufacture of coated, nano-scale, hydrotalcites, where the individual, primary, nano-scale hydrotalcite particles are coated. In order to obtain the corresponding hydrotalcite particles in coated, nano-scale form, the additive precipitation reaction is employed invention-related. Every primary particle indicates its own coating in this case. In a further aspect, the registration is directed toward coated primary, nano-scale, hydrotalcite particles, in particular obtainable in accordance with the invention-related process. A further aspect of the invention is directed toward composites containing nano-scale hydrotalcites, in particular hydrotalcites manufactured in accordance with the invention presented. Finally the registration presented is directed towards compositions containing mixtures of magnesium hydroxide and hydrotalcite. ## Claims ### Claim 1 Coated, primary, nano-scale, hydrotalcite particles obtained by a process, comprising: contacting i) a magnesium saline solution with ii) an aluminum saline solution, to obtain a first reaction mixture, adding sodium carbonate and sodium hydroxide to the first reaction mixture, to obtain a second reaction mixture, and precipitating a coated, primary, nano-scale, hydrotalcite particles from the second reaction mixture, wherein one of the solutions i) or ii) comprises at least one additive selected from the group consisting of A and B, optionally in combination with an additive C, or the contacting of i) and ii) further comprises contacting at least one additive selected from the group consisting of A and B, optionally in combination with an additive C, with the first reaction mixture, wherein the additive A is a growth inhibitor, the additive B is a dispersing agent and the additive C is a diluted fatty acid solution, and wherein the primary hydrotalcite particles are each individually coated. ### Claim 2 (depends on 1) The coated, primary, nano-scale hydrotalcite particles of claim 1, wherein the particles have a BET surface area of ≧50 m2/g. ### Claim 3 (depends on 1) A composite, comprising: the coated, primary, nano-scale hydrotalcite particles of claim 1, as a filling material. ### Claim 4 (depends on 1) A composition, comprising: 1 to 60 mass % MgOH2, and 1 to 20 mass % coated, primary, nano-scale hydrotalcite particles according to claim 1. ### Claim 5 (depends on 1) The coated, primary, nano-scale hydrotalcite particles of claim 1, wherein said additive C is present and is a stearate solution. ### Claim 6 (depends on 1) The coated, primary, nano-scale hydrotalcite particles of claim 1, wherein hydrotalcite of the particles has a formula Mg6Al2(OH)16CO3.4H2O. ### Claim 7 (depends on 3) The composite of claim 3, further comprising a plastic. ### Claim 8 (depends on 3) A process for manufacturing the composite of claim 3, comprising: an extrusion process in which a plastic is mixed with said coated, primary, nano-scale hydrotalcite particles. ### Claim 9 A composite, comprising: a plastic, coated, primary, nano-scale hydrotalcite particles, as a filling material in the plastic, in a content of from 1 to 20 mass % with respect to the composite, and MgOH2 in a content of from 1 to 60 mass % with respect to the composite, wherein the coated, primary, nano-scale hydrotalcite particles are obtained by a process, comprising: contacting i) a magnesium saline solution with ii) an aluminum saline solution, to obtain a first reaction mixture, adding sodium carbonate and sodium hydroxide to the first reaction mixture, to obtain a second reaction mixture, and precipitating a coated, primary, nano-scale, hydrotalcite particles from the second reaction mixture, wherein one of the solutions i) or ii) comprises at least one additive selected from the group consisting of A and B, optionally in combination with an additive C, or wherein the contacting of i) and ii) further comprises contacting at least one additive selected from the group consisting of A and B, optionally in combination with an additive C, with the first reaction mixture, wherein the additive A is a growth inhibitor, the additive B is a dispersing agent, and the additive C is a diluted fatty acid solution, wherein the primary hydrotalcite particles are each individually coated, and wherein the composite has a UL94 V0 fire resistance. ### Claim 10 (depends on 9) The composite of claim 9, wherein hydrotalcite of the coated, primary, nano-scale hydrotalcite particles has a formula Mg6Al2(OH)16CO3.4H2O. ### Claim 11 (depends on 1) A process for manufacturing the coated, primary, nano-scale, hydrotalcite particles of claim 1, the process comprising: contacting i) a magnesium saline solution with ii) an aluminum saline solution, to obtain a first reaction mixture, adding sodium carbonate and sodium hydroxide to the first reaction mixture, to obtain a second reaction mixture, and precipitating coated, primary, nano-scale, hydrotalcite particles from the second reaction mixture, wherein one of the solutions i) or ii) comprises at least one additive selected from the group consisting of A and B, optionally in combination with an additive C, or the contacting of i) and ii) further comprises contacting at least one additive selected from the group consisting of A and B, optionally in combination with an additive C, with the first reaction mixture, wherein the additive A is a growth inhibitor, the additive B is a dispersing agent and the additive C is a diluted fatty acid solution. ### Claim 12 (depends on 11) The process of claim 11, wherein the hydrotalcite comprises Zn2+ as a further bivalent metal. ### Claim 13 (depends on 11) The process of claim 11, wherein the hydrotalcite comprises at least one anion selected from the group consisting of sulfate, chloride, and nitrate. ### Claim 14 (depends on 11) The process of claim 11, wherein the hydrotalcite has a formula Mg6Al2(OH)16CO3.4H2O. ### Claim 15 (depends on 11) The process of claim 11, wherein the contacting is performed at a temperature of 0 to 90° C. ### Claim 16 (depends on 11) The process of claim 11, wherein the first reaction mixture comprises the additive B. ### Claim 17 (depends on 11) The process of claim 11, wherein the first reaction mixture comprises 0.1 to 30 mass % of the additive A, based on a solids content of hydrotalcite in the first reaction mixture, and optionally 0.1 to 10 mass % of the additive C, based on a solids content of hydrotalcite in the first reaction mixture. ### Claim 18 (depends on 11) The process of claim 11, which produces nano-scale hydrotalcite particles where at least 90% of the individual particles have a diameter ≦100 nm. ### Claim 19 (depends on 11) The process of claim 11, wherein said additive C is present and is a stearate solution.