# US 9,040,156 B2 · Whitlockite and method for manufacturing the same > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,040,156 B2 - Document ID: US9040156B2 - Status: Granted - Kind: B2 - Application number: 13/645,508 - Filed: 2012-10-04 - Published: 2014-02-13 - Granted: 2015-05-26 - Earliest claimed: 2012-08-10 - Assignees: Snu R&Db Foundation - Applicants: Snu R&Db Foundation - Inventors: Kug Sun Hong; Ki Tae Nam; Hae Lin Jang; Hyun Seung Ryu; Kyoung Suk Jin - Web page: https://patentgrep.com/patent/US9040156B2 ## CPC - C01B 25/32: Phosphates of magnesium, calcium, strontium, or barium - C01B 25/322: {Preparation by neutralisation of orthophosphoric acid} - Y10S 977/773: Nanoparticle, i.e. structure having three dimensions of 100 nm or less - Y10T 428/2982: Particulate matter [e.g., sphere, flake, etc.] - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract This invention relates to whitlockite and a method for manufacturing the same. The method includes adding, to water, a calcium ion supplying material and a cation supplying material containing a cation (X) other than the calcium ion to prepare a cation aqueous solution, adding a phosphoric acid supplying material to the cation aqueous solution, and aging the cation aqueous solution including the phosphoric acid supplying material. As a result, whitlockite having high purity and high crystallinity can be mass produced using a simple process. ## Claims ### Claim 1 A method for manufacturing whitlockite, the method comprising: adding, to water, a calcium ion supplying material and a cation supplying material containing a cation (X) other than a calcium ion to prepare a cation aqueous solution; adding a phosphoric acid supplying material to the cation aqueous solution; and aging the cation aqueous solution including the phosphoric acid supplying material, wherein a temperature of the water is equal to or lower than a boiling point, wherein the phosphoric acid supplying material is added in a dropwise manner, wherein a pH of the cation aqueous solution is gradually decreased depending on addition of the phosphoric acid supplying material, and the cation aqueous solution including the phosphoric acid supplying material added thereto is aged in an acidic environment. ### Claim 2 (depends on 1) The method of claim 1, wherein, in the cation aqueous solution, the cation (X) is contained in an amount of 10˜50 mol % based on a total amount of cations (Ca+X). ### Claim 3 (depends on 2) The method of claim 2, wherein the phosphoric acid supplying material is added to bring a molar ratio of anion to cation (anion/cation=P/(Ca+X)) to 0.6 or greater. ### Claim 4 (depends on 3) The method of claim 3, wherein an amount of the cation (X) and the molar ratio of anion to cation are selected within a range that suppresses formation of a byproduct other than the whitlockite in view of a correlation therebetween. ### Claim 5 (depends on 1) The method of claim 1, wherein the calcium ion supplying material includes one or more chosen from calcium hydroxide, calcium acetate, calcium carbonate, and calcium nitrate. ### Claim 6 (depends on 1) The method of claim 1, wherein the cation (X) includes one or more chosen from Mg, Co, Sb, Fe, Mn, Y, Eu, Cd, Nd, Na, La, Sr, Pb, Ba and K. ### Claim 7 (depends on 1) The method of claim 1, wherein the cation supplying material includes one or more chosen from a hydroxide compound (X-hydroxide), an acetate compound (X-acetate), a carbonate compound (X-carbonate), and a nitrate compound (X-nitrate). ### Claim 8 (depends on 1) The method of claim 1, wherein the phosphoric acid supplying material includes one or more chosen from diammonium hydrogen phosphate, ammonium phosphate, and phosphoric acid. ### Claim 9 (depends on 1) The method of claim 1, wherein the phosphoric acid supplying material is added in a dropwise manner. ### Claim 10 (depends on 9) The method of claim 9, wherein a pH of the cation aqueous solution is gradually decreased depending on addition of the phosphoric acid supplying material, and the cation aqueous solution including the phosphoric acid supplying material added thereto is aged in an acidic environment. ### Claim 11 (depends on 1) The method of claim 1, wherein the cation supplying material is magnesium hydroxide, an amount of magnesium (Mg) in the cation aqueous solution is 10˜35 mol % based on the total amount of cations (Ca+Mg), and the phosphoric acid supplying material is added to bring the molar ratio of anion to cation (anion/cation=P/(Ca+Mg)) to 0.8 or greater. ### Claim 12 (depends on 1) The method of claim 1, wherein the cation supplying material is magnesium nitrate, and the phosphoric acid supplying material is added to bring the molar ratio of anion to cation (anion/cation=P/(Ca+Mg)) to 0.6 or greater. ### Claim 13 (depends on 1) The method of claim 1, further comprising adding an oxidant to the water or the cation aqueous solution before adding the phosphoric acid supplying material. ### Claim 14 (depends on 13) The method of claim 13, wherein the oxidant is hydrogen peroxide. ### Claim 15 (depends on 1) The method of claim 1, further comprising drying the aged aqueous solution thus forming whitlockite powder. ### Claim 16 (depends on 1) The method of claim 1, wherein a temperature of the water is equal to or lower than a boiling point. ### Claim 17 A whitlockite, wherein the whitlockite is manufactured by a manufacturing method comprising: adding, to water, a calcium ion supplying material and a cation supplying material containing a cation (X) other than a calcium ion to prepare a cation aqueous solution; adding a phosphoric acid supplying material to the cation aqueous solution; and aging the cation aqueous solution including the phosphoric acid supplying material, wherein a temperature of the water is equal to or lower than a boiling point, wherein the phosphoric acid supplying material is added in a dropwise manner, wherein a pH of the cation aqueous solution is gradually decreased depending on addition of the phosphoric acid supplying material, and the cation aqueous solution including the phosphoric acid supplying material added thereto is aged inan acidic environment. ### Claim 18 (depends on 17) The whitlockite of claim 17, wherein the whitlockite has a chemical formula represented by Ca20-yXy(HPO4)2(PO4)12, and a ratio of Ca:X:P is (1.28±0.2):(0.14±0.02):1. ### Claim 19 (depends on 17) The whitlockite of claim 17, wherein the manufacturing method further comprises drying the aged aqueous solution thus forming whitlockite powder. ### Claim 20 (depends on 19) The whitlockite of claim 19, wherein the whitlockite powder has a particle size of 100 nm or less.