CN1137044C - Process for preparing alpha-calcium phosphate as basic material of bone reparing biological material - Google Patents
Process for preparing alpha-calcium phosphate as basic material of bone reparing biological material Download PDFInfo
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- CN1137044C CN1137044C CNB011419652A CN01141965A CN1137044C CN 1137044 C CN1137044 C CN 1137044C CN B011419652 A CNB011419652 A CN B011419652A CN 01141965 A CN01141965 A CN 01141965A CN 1137044 C CN1137044 C CN 1137044C
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- calcium phosphate
- alpha
- tcp
- present
- calcium
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Abstract
The present invention discloses a preparation method of alpha-calcium phosphate of base material of bone repair biologic material. The present invention has the method that a composite mineralizing agent is added into the mixture of calcium phosphate and calcium carbonate, the mixture is ground by a wet method, the obtained powder is dried, sieved and calcined at a high temperature and is naturally cooled to room temperature with a stove, and alpha-TCP bone repair basic material whose purity reaches more than 99.2% is obtained. The present invention is characterized in that the calcium phosphate and the calcium carbonate are mixed according to the ratio of 2:1, and 0.5 to 3 wt% of alkali earth metal or alkali metal salt mineralizing agent containing fluorine ions, such as, potassium fluoride, calcium fluoride, etc. is added. The alpha-TCP prepared by the present invention has high purity, good biocompatible polymer and good mechanical performance.
Description
Technical field
The present invention relates to a kind of preparation method of alpha-calcium phosphate as basic material of bone reparing biological material, belong to the technology of preparing of bone renovating material.
Background technology
With α-TCP respectively with CaHPO
42H
2O, CaHPO
4, Ca (H
2PO
4)
2H
2O, CaCO
3Deng mixing, be in harmonious proportion with water or solvent again, obtained multiple α-TCP bone cement, and be successfully applied to clinical.Wherein the purity of alpha-calcium phosphate substrate material is directly to influence the microstructure of self cure time, hydrated reaction product and material of bone cement and the important factor of mechanical property.At present the preparation method of alpha-calcium phosphate is to be raw material with calcium phosphate salt and lime carbonate, adopts solid reaction process, and high temperature is incubated for a long time, is quickly cooled to room temperature preparation again and forms.Present method becomes cryostatic stabilization phase β-TC mutually for preventing high-temperature stable phase α-TCP in process of cooling, its gordian technique is control calcining temperature and speed of cooling.But this technology is difficult to grasp, and needs corresponding support equipment, causes prepared α-TCP purity not high, the production cost height.
The synthetic calcium phosphate composite material (Reaction tricalciumphosphate composition, Fulmer, et al., U.S.Pat.886239,1997) of the patent-reaction of application such as U.S. mark Fu Ermo is with CaPHO
4And CaCO
3Be raw material, under certain water vapor pressure, solid phase in 1400 ℃ of calcinings 4 hours, be quickly cooled in 30 seconds about 700 ℃, then continue to be cooled to room temperature, make stable alpha-TCP product,, will be mingled with a little hydroxyapatite in the product if speed of cooling is fast inadequately.Spain Khairoun I. etc. studies α-TCP material and bone cement thereof, as with CaHPO
4And CaCO
3Be raw material,, be chilled to room temperature and obtain α-TCP in 1300 ℃ of calcinings 6 hours, with α-TCP be base starting material to prepare setting time be 10～30 minutes, ultimate compression strength is the bone cement of 20～40MPa.Japan Mei Jinyi first-class has been invented a kind of α-TCP material (Japanese Patent, 95190275) that is applicable to that bone is repaired.The domestic Zhang Xingdong of Sichuan University etc. utilizes high temperature solid state reaction, and process for cooling is prepared α-TCP fast, and the ultimate compression strength of its corresponding α-TCP bone cement can reach 15MPa.So far the preparation technology of bone reparation substrate material α-TCP is basic identical, never break through, so α-TCP costs an arm and a leg.
Summary of the invention
The object of the invention is to provide a kind of bone to repair the preparation method of alpha-calcium phosphate as basic material.This method preparation process condition is easily controlled, and prepared α-TCP purity height has excellent biological compatibility and mechanical property,
The present invention is realized by following technical proposals.Add composite mineralizer in calcium phosphate salt and carbonate salt mixture, the powder after the wet grinding is through comprising drying, sieve, high-temperature calcination, naturally cooling to the process of room temperature with stove, obtains α-TCP bone that purity reaches more than 99.2% and repairs base material.It is characterized by, the composite mineralizer of employing is fluorine-containing (F
-) ionic alkaline earth salt or an alkali metal salt.Its add-on is for being the mineralizer that adds 0.5-3.0wt% in 2: 1 the mixture in calcium phosphate salt and carbonate salt mol ratio, and the dried powder calcination temperature of wet-milling is 1250-1480 ℃.
Above-mentioned fluorine-containing alkaline-earth metal or an alkali metal salt are Potassium monofluoride, Calcium Fluoride (Fluorspan), Sodium Fluoride.
Embodiment
Embodiment 1:
Accurately take by weighing 171.1 gram dicalcium phosphate dihydrate (CaHPO
42H
2O) and 50.0 gram lime carbonate (CaCO
3), add 1.4 gram CaF
2With 0.8 gram KF composite mineralizer, this compound is inserted in the ball grinder, and mill is situated between and medium is respectively zirconia ball and dehydrated alcohol, and material: ball: the medium-weight ratio is 1: 2: 1.7, behind the ball milling 4 hours, dry under 80 ℃ of temperature, dried powder is sieved, in 1300 ℃ of calcinings, and be incubated 2 hours, then naturally cool to room temperature, can obtain purity and can reach α-TCP material of 99.2%, grind, seal up for safekeeping made α-TCP material stand-by with stove.Embodiment 2:
Accurately take by weighing 342.2 gram dicalcium phosphate dihydrate (CaHPO
42H
2O) and 100 gram lime carbonate (CaCO
2), add 2.0 gram CaF
2With 1.8 gram NaF composite mineralizers, this compound is inserted in the ball grinder, and mill is situated between and medium is respectively agate ball and dehydrated alcohol, and material: ball: the medium-weight ratio is 1: 3: 1.7, behind the ball milling 8 hours, dry under 80 ℃ of temperature, dried powder is sieved, in 1420 ℃ of calcinings, and be incubated 2 hours, then naturally cool to room temperature, can obtain purity and can reach α-TCP material of 99.2%, grind, seal up for safekeeping made α-TCP material stand-by with stove.
Claims (1)
1. the preparation method of an alpha-calcium phosphate as basic material of bone reparing biological material, this method adds composite mineralizer in calcium phosphate salt and carbonate salt mixture, powder after the wet grinding is through comprising drying, sieve, high-temperature calcination, naturally cool to the process of room temperature with stove, obtain the alpha-calcium phosphate bone that purity reaches more than 99.2% and repair base material, it is characterized by: the composite mineralizer of employing is a Potassium monofluoride, Calcium Fluoride (Fluorspan), Sodium Fluoride, its add-on is for being the mineralizer that adds 0.5-3.0wt% in 2: 1 the mixture in calcium phosphate and carbonate salt mol ratio, and the dried powder calcination temperature of wet-milling is 1250-1480 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011419652A CN1137044C (en) | 2001-09-26 | 2001-09-26 | Process for preparing alpha-calcium phosphate as basic material of bone reparing biological material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011419652A CN1137044C (en) | 2001-09-26 | 2001-09-26 | Process for preparing alpha-calcium phosphate as basic material of bone reparing biological material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1338425A CN1338425A (en) | 2002-03-06 |
| CN1137044C true CN1137044C (en) | 2004-02-04 |
Family
ID=4676518
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011419652A Expired - Fee Related CN1137044C (en) | 2001-09-26 | 2001-09-26 | Process for preparing alpha-calcium phosphate as basic material of bone reparing biological material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1137044C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110562945A (en) * | 2019-10-17 | 2019-12-13 | 广州润虹医药科技股份有限公司 | Alpha-tricalcium phosphate and preparation method thereof |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100357178C (en) * | 2005-09-27 | 2007-12-26 | 华南理工大学 | Carbonic acid type high activity partially crystallized calcium phosphate and its prepn |
| CN114569732B (en) * | 2022-01-24 | 2023-09-01 | 国家纳米科学中心 | Nanometer medicine and its prepn and application |
-
2001
- 2001-09-26 CN CNB011419652A patent/CN1137044C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110562945A (en) * | 2019-10-17 | 2019-12-13 | 广州润虹医药科技股份有限公司 | Alpha-tricalcium phosphate and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1338425A (en) | 2002-03-06 |
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