CN1338425A - 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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- CN1338425A CN1338425A CN 01141965 CN01141965A CN1338425A CN 1338425 A CN1338425 A CN 1338425A CN 01141965 CN01141965 CN 01141965 CN 01141965 A CN01141965 A CN 01141965A CN 1338425 A CN1338425 A CN 1338425A
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- calcium phosphate
- salt
- bone
- tcp
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Abstract
An alpha-calcium phosphate as the basic material of bone-repairing biologic material is prepared from calcium phosphate and calcium carbonate through proportional mixing, adding compound mineralizing agent, wet grinding, drying, sieving, high-temp calcining, and naturally cooling. Said mineralizing agent is the fluoric alkali-earth metal salts or alkali metal salts (potassium fluoride or calcium fluoride). Its advantages include high purity and better biologic compatibility and 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 (H2PO
4)
2.H
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 patent one 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.
Specific 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
3), 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 (2)
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, obtaining purity reaches α more than 99.2%-TCP bone 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 ℃.
2. according to the preparation method of the described alpha-calcium phosphate as basic material of bone reparing biological material of claim one, it is characterized in that: fluorine-containing alkaline-earth metal or an alkali metal salt are Potassium monofluoride, Calcium Fluoride (Fluorspan), Sodium Fluoride.
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 true CN1338425A (en) | 2002-03-06 |
| CN1137044C 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 (3)
| 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 |
| 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 |
| CN114569732A (en) * | 2022-01-24 | 2022-06-03 | 国家纳米科学中心 | Nano medicine and its preparing method and use |
-
2001
- 2001-09-26 CN CNB011419652A patent/CN1137044C/en not_active Expired - Fee Related
Cited By (4)
| 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 |
| 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 |
| CN114569732A (en) * | 2022-01-24 | 2022-06-03 | 国家纳米科学中心 | Nano medicine and its preparing method and use |
| CN114569732B (en) * | 2022-01-24 | 2023-09-01 | 国家纳米科学中心 | Nanometer medicine and its prepn and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1137044C (en) | 2004-02-04 |
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