Method of preparing calcium phosphate

Claim 1

A method of preparing calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 30° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing about 10% by weight of the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted, at 80° C.; (e) pulverizing the dried slurry to obtain a powdery substance; and (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the calcination period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° C.

Claim 2

A method of preparing calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 30° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing about 10% by weight of the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted, at 80° C.; (e) pulverizing the dried slurry to obtain a powdery substance; and (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the calcination period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° C.

Claim 11

A method of preparing a sintered body of calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 30° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing about 10% by weight of the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted, at 80° C.; (e) pulverizing the dried slurry to obtain a powdery substance; (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° c.; (g) molding the calcium phosphate into a desired shape, and (h) sintering the molded calcium phosphate to obtain a sintered body of the calcium phosphate.

Claim 12

A method of preparing a sintered body of calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 30° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing about 10% by weight of the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted, at 80° C.; (e) pulverizing the dried slurry to obtain a powdery substance; (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° c.; (g) molding the calcium phosphate into a desired shape, and (h) sintering the molded calcium phosphate to obtain a sintered body of the calcium phosphate.

Claim 17

A method of preparing calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 30° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted; (e) pulverizing the dried slurry to obtain a powdery substance; and (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the calcination period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° C.

Claim 18

A method of preparing calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 30° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted; (e) pulverizing the dried slurry to obtain a powdery substance; and (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the calcination period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° C.

Claim 21

A method of preparing a sintered body of calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 90+° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted; (e) pulverizing the dried slurry to obtain a powdery substance; (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the calcination period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° C.; (g) molding the calcium phosphate into a desired shape, and (h) sintering the molded calcium phosphate to obtain a sintered body of the calcium phosphate.

Claim 22

A method of preparing a sintered body of calcium phosphate comprising: (a) weighing powdery materials comprising powdery calcium carbonate and powdery calcium monohydrogenphosphate or a powdery dihydrate thereof such that a Ca/P ratio of the powdery materials is 1.45 to 1.67; (b) adding water at a temperature of not lower than 90+° C. to the weighed powdery materials from step (a) to prepare an aqueous slurry containing the powdery materials; (c) subjecting the aqueous slurry to a rotational attrition by using a ball mill to carry out a mechanochemical reaction of said calcium carbonate with said calcium monohydrogenphosphate or a dehydrate thereof; (d) drying the aqueous slurry, thus mechanochemically reacted; (e) pulverizing the dried slurry to obtain a powdery substance; (f) calcining the powdery substance under conditions of calcination temperature and calcination period of time to obtain a biologically safe calcium phosphate free from all of hemolysis, antigenicity and cytotoxicity, said calcining being carried out at a calcination temperature of 720° to 1,150° C. for a calcination period of time of 1 to 10 hours, said calcining being carried out for a calcination period of time of at least one hour when said calcining is carried out at 1,150° C. and the calcination period of time being related to the calcination temperature such that the calcination period of time is increased with a decrease in said calcination temperature, said calcining being carried out for a calcination period of time of at least 3 hours when said calcining is carried out 1000° C., said calcining being carried out for a calcination period of time of at least 8 hours when said calcining is carried out at 900° C. and said calcining being carried out for a calcination period of time of at least 10 hours when said calcining is carried out at 720° C.; (g) molding the calcium phosphate into a desired shape, and (h) sintering the molded calcium phosphate to obtain a sintered body of the calcium phosphate.