CN113735085A - Preparation method of beta-tricalcium phosphate - Google Patents
Preparation method of beta-tricalcium phosphate Download PDFInfo
- Publication number
- CN113735085A CN113735085A CN202111070223.1A CN202111070223A CN113735085A CN 113735085 A CN113735085 A CN 113735085A CN 202111070223 A CN202111070223 A CN 202111070223A CN 113735085 A CN113735085 A CN 113735085A
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- CN
- China
- Prior art keywords
- tricalcium phosphate
- beta
- preparation
- phosphoric acid
- calcium hydroxide
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims abstract description 19
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 18
- 229940078499 tricalcium phosphate Drugs 0.000 claims abstract description 18
- 235000019731 tricalcium phosphate Nutrition 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 13
- 239000002244 precipitate Substances 0.000 claims abstract description 13
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 12
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 12
- 239000011575 calcium Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002243 precursor Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 description 2
- 238000002316 cosmetic surgery Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 229910000150 monocalcium phosphate Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 208000020084 Bone disease Diseases 0.000 description 1
- 206010006956 Calcium deficiency Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000002805 bone matrix Anatomy 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- -1 pH regulator Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000008733 trauma Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
Abstract
The invention provides a preparation method of beta-tricalcium phosphate, which comprises the following steps: 1) preparing reaction raw materials of calcium hydroxide and phosphoric acid; 2) calcium hydroxide with the purity of 96 percent and phosphoric acid with the purity of 85 percent are sequentially added into a reaction kettle as precursor substances according to the Ca/P ratio of 1.5 and are uniformly mixed, and tricalcium phosphate precipitate is obtained after full reaction; 3) and washing and drying the tricalcium phosphate, calcining and cooling to obtain the beta-tricalcium phosphate. The preparation method of the beta-tricalcium phosphate provided by the invention has the advantages of simple preparation method, easiness in operation, mild and controllable conditions, short period, no pollution to the environment, higher biological safety and easiness in industrial mass production.
Description
Technical Field
The invention relates to the crossing field of materials science and biomedicine, in particular to a preparation method of beta-tricalcium phosphate.
Background
The beta-tricalcium phosphate is mainly composed of calcium and phosphorus, has the components similar to inorganic components of bone matrix, has good biocompatibility, bioactivity and biodegradability, is an ideal human hard tissue repair and substitute material, is used as an artificial bone raw material, and is widely applied to orthopedics clinic, plastic and cosmetic surgery, dentistry, bone defect repair, bone fusion and the like caused by trauma, tumor, inflammation, bone diseases and the like. Can be added into food as safe nutrition enhancer to enhance calcium intake, and can be used for preventing or treating calcium deficiency. It can also be used as anticaking agent, pH regulator, and buffer in food.
The preparation method of the beta-tricalcium phosphate comprises an ultrasonic chemical method, a sol-gel method, a W/O microemulsion method, a solid phase synthesis method, a mechanochemical synthesis method and the like. Wherein, the sonochemical method has higher requirements on experimental equipment and is not easy to realize; the sol-gel method and the microemulsion method have complex processes, long preparation time, toxic organic solvent and easy pollution to the environment; the crystal grains synthesized by the solid-phase synthesis method are coarse, the composition is not uniform, and the impure phase exists; the powder prepared by the mechanochemical synthesis method has uneven particle size distribution, is easy to agglomerate and is easy to cause pollution to products.
Therefore, in order to overcome the disadvantages of the prior art, it is necessary to design a method for preparing β -tricalcium phosphate to solve the above problems.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of beta-tricalcium phosphate.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a preparation method of beta-tricalcium phosphate comprises the following steps:
1) preparing reaction raw materials of calcium hydroxide and phosphoric acid;
2) calcium hydroxide with the purity of 96 percent and phosphoric acid with the purity of 85 percent are sequentially added into a reaction kettle as precursor substances according to the Ca/P ratio of 1.5 and are uniformly mixed, and tricalcium phosphate precipitate is obtained after full reaction;
3) and washing and drying the tricalcium phosphate, calcining and cooling to obtain the beta-tricalcium phosphate.
The preferable technical scheme is as follows: in the step 2), calcium hydroxide and phosphoric acid are put into the reaction kettle and then stirred, the stirring speed is 200rpm, and the stirring time is 2 hours.
The preferable technical scheme is as follows: and in the step 3), the tricalcium phosphate precipitate is kept stand and dried for evening after being washed.
The preferable technical scheme is as follows: in the step 3), the tricalcium phosphate precipitate is calcined at the sintering temperature of 900-1300 ℃ for 2 hours to obtain beta-tricalcium phosphate.
The preferable technical scheme is as follows: and grinding and screening the beta-tricalcium phosphate according to the application to obtain a final product.
Due to the application of the technical scheme, the invention has the beneficial effects that:
the preparation method of the beta-tricalcium phosphate provided by the invention has the advantages of simple preparation method, easiness in operation, mild and controllable conditions, short period, no pollution to the environment, higher biological safety and easiness in industrial mass production.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
In the description of the present invention, it should be further noted that, unless otherwise specifically stated or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may include, for example, a fixed connection, a detachable connection, an integral connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection via an intermediate medium, and a communication between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example (b):
the invention provides a preparation method of beta-tricalcium phosphate, which comprises the following steps:
1) preparing reaction raw materials of calcium hydroxide and phosphoric acid;
2) calcium hydroxide with the purity of 96 percent and phosphoric acid with the purity of 85 percent are sequentially added into a reaction kettle as precursor substances according to the Ca/P ratio of 1.5 and are uniformly mixed, and tricalcium phosphate precipitate is obtained after full reaction;
3) and washing tricalcium phosphate, drying, calcining and cooling to obtain beta-tricalcium phosphate.
Further, in the step 2), calcium hydroxide and phosphoric acid are put into the reaction kettle and then stirred, the stirring speed is 200rpm, and the stirring time is 2 hours, so as to ensure full reaction.
Further, in step 3), the tricalcium phosphate precipitate is washed and then left to dry evening.
Further, in step 3), the tricalcium phosphate precipitate was calcined at a sintering temperature of 900-.
Further, the beta-tricalcium phosphate is ground and sieved according to the application to obtain the final product.
Wherein, step 2):
1. the fine particles may be made large by the sintering process.
2.H3PO4And Ca (OH)2Reaction to form
This is a stepwise reaction, since the phosphoric acid is ionized stepwise, according to H3PO4And Ca (OH)2The amount of the substance (c) determines the product.
(1) If phosphoric acid is in excess, 2H3PO4+Ca(OH)2＝Ca(H2PO4)2+H20；
(2) If there is Ca (OH)2And then: ca (OH)2+Ca(H2PO4)2＝2CaHPO4(precipitate) + H2O;
(3) if Ca (OH)2And if the amount is excessive, the method comprises the following steps: ca (OH)2+2CaHPO4＝Ca3(PO4)2(precipitate) + H2O.
3. For CaHPO4·2H2O-CaCO3The precipitate is heated (heating temperature 100-. Then gradually heated to 1000 ℃.
4. The temperature is raised to 900 ℃ and 1300 ℃ to reach the generation condition of the beta-tricalcium phosphate.
Therefore, the invention has the following advantages:
the preparation method of the beta-tricalcium phosphate provided by the invention has the advantages of simple preparation method, easiness in operation, mild and controllable conditions, short period, no pollution to the environment, higher biological safety and easiness in industrial mass production.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (5)
1. The preparation method of the beta-tricalcium phosphate is characterized by comprising the following steps:
1) preparing reaction raw materials of calcium hydroxide and phosphoric acid;
2) calcium hydroxide with the purity of 96 percent and phosphoric acid with the purity of 85 percent are sequentially added into a reaction kettle as precursor substances according to the Ca/P ratio of 1.5 and are uniformly mixed, and tricalcium phosphate precipitate is obtained after full reaction;
3) and washing and drying the tricalcium phosphate, calcining and cooling to obtain the beta-tricalcium phosphate.
2. The method of claim 1, wherein the tricalcium phosphate is prepared by: in the step 2), calcium hydroxide and phosphoric acid are put into the reaction kettle and then stirred, the stirring speed is 200rpm, and the stirring time is 2 hours.
3. The method of claim 1, wherein the tricalcium phosphate is prepared by: and in the step 3), the tricalcium phosphate precipitate is kept stand and dried for evening after being washed.
4. The method of claim 1, wherein the tricalcium phosphate is prepared by: in the step 3), the tricalcium phosphate precipitate is calcined at the sintering temperature of 900-1300 ℃ for 2 hours to obtain beta-tricalcium phosphate.
5. The method of claim 1, wherein the tricalcium phosphate is prepared by: and grinding and screening the beta-tricalcium phosphate according to the application to obtain a final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111070223.1A CN113735085A (en) | 2021-09-13 | 2021-09-13 | Preparation method of beta-tricalcium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111070223.1A CN113735085A (en) | 2021-09-13 | 2021-09-13 | Preparation method of beta-tricalcium phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113735085A true CN113735085A (en) | 2021-12-03 |
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ID=78738550
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111070223.1A Pending CN113735085A (en) | 2021-09-13 | 2021-09-13 | Preparation method of beta-tricalcium phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113735085A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654236A (en) * | 2009-09-04 | 2010-02-24 | 广东光华化学厂有限公司 | Preparation method of food additive grade tricalcium phosphate |
| CN104016325A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for tricalcium phosphate |
| CN109052357A (en) * | 2018-08-30 | 2018-12-21 | 南昌航空大学 | A kind of preparation method of rodlike beta-tricalcium phosphate crystal |
| WO2019132843A1 (en) * | 2017-12-27 | 2019-07-04 | Yildiz Teknik Universitesi | Production of beta-tri-calcium phosphate (beta-tcp) with high purity |
| CN113080204A (en) * | 2021-03-10 | 2021-07-09 | 蒙娜丽莎集团股份有限公司 | Silver-loaded calcium phosphate with lasting antibacterial function and wet synthesis method thereof |
-
2021
- 2021-09-13 CN CN202111070223.1A patent/CN113735085A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654236A (en) * | 2009-09-04 | 2010-02-24 | 广东光华化学厂有限公司 | Preparation method of food additive grade tricalcium phosphate |
| CN104016325A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for tricalcium phosphate |
| WO2019132843A1 (en) * | 2017-12-27 | 2019-07-04 | Yildiz Teknik Universitesi | Production of beta-tri-calcium phosphate (beta-tcp) with high purity |
| CN109052357A (en) * | 2018-08-30 | 2018-12-21 | 南昌航空大学 | A kind of preparation method of rodlike beta-tricalcium phosphate crystal |
| CN113080204A (en) * | 2021-03-10 | 2021-07-09 | 蒙娜丽莎集团股份有限公司 | Silver-loaded calcium phosphate with lasting antibacterial function and wet synthesis method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
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| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20211203 |