CN110562945A - Alpha-tricalcium phosphate and preparation method thereof - Google Patents
Alpha-tricalcium phosphate and preparation method thereof Download PDFInfo
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Abstract
the invention relates to the technical field of bone repair materials, and discloses a preparation method of alpha-tricalcium phosphate. The problem of easy agglomeration in the sintering process of the alpha-tricalcium phosphate comprises the following steps: 1) mixing calcium hydrogen phosphate and calcium carbonate by a solid-phase reaction method, grinding for 20-40min, heating to 850-920 ℃, calcining, cooling, and sieving by a 10-200 mu m sieve to obtain powder A; 2) adding zirconium dioxide powder into the powder A obtained in the step 1), wherein the particle size of the zirconium dioxide powder is larger than that of the powder A, uniformly mixing, heating to 1125-1500 ℃, keeping the temperature for 2-5h, taking out, and cooling; 3) sieving to obtain alpha-tricalcium phosphate powder; the method can reduce the agglomeration of the alpha-tricalcium phosphate and maintain the original size structure of the powder; the grinding step of the sintered alpha-tricalcium phosphate is avoided; the preparation process is simple; the zirconium dioxide can be recycled.
Description
Technical Field
The invention relates to the technical field of bone repair materials, in particular to alpha-tricalcium phosphate and a preparation method thereof.
Background
The calcium phosphate ceramic mainly comprises 3 crystal phases of calcium phosphate biological ceramic materials such as hydroxyapatite (HA for short), alpha-tricalcium phosphate (alpha-TCP for short), beta-tricalcium phosphate (beta-TCP for short) and the like.
Tricalcium phosphate HAs an alpha phase and a beta phase, the beta phase is a low-temperature phase, the alpha phase is a high-temperature phase, alpha-TCP is a monoclinic system, the beta-TCP is a hexagonal system, the beta phase is converted into the alpha phase at 1125 ℃, the alpha-TCP HAs good comprehensive performance, the bioactivity is better than HA, the biocompatibility is better than that of the beta-TCP, the biodegradation rate is higher than that of the beta-TCP, so that more and more attention is attracted, and the tricalcium phosphate becomes one of the research hotspots of the current calcium phosphate biological ceramic material.
patent CN201610946615.2 discloses a method for preparing porous α -TCP microspheres with antibacterial function, which agglomerate after sintering, thus requiring grinding of the product. With the increase of the calcination temperature, agglomeration occurs among the alpha-TCP particles, the particle size of the particles gradually increases, the unevenness of the particles gradually increases, and the sintering agglomeration is more easily formed as the sintering temperature is higher, so that the problem of agglomeration is particularly important to solve in the process of preparing the superfine powder.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide alpha-tricalcium phosphate and a preparation method thereof so as to solve the problem that the existing alpha-tricalcium phosphate is easy to agglomerate in the sintering process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
A preparation method of alpha-tricalcium phosphate is characterized by comprising the following steps:
1) Mixing calcium hydrogen phosphate and calcium carbonate by a solid-phase reaction method, grinding for 20-40min, heating to 850-920 ℃, calcining, cooling, and sieving by a 10-200 mu m sieve to obtain powder A;
2) adding zirconium dioxide powder into the powder A obtained in the step 1), wherein the particle size of the zirconium dioxide powder is larger than that of the powder A, uniformly mixing, heating to 1125-1500 ℃, keeping the temperature for 2-5h, taking out, and cooling;
3) Sieving to obtain alpha-tricalcium phosphate powder;
The inventor of the application unexpectedly finds that the zirconium dioxide with a certain particle size is added, so that sintering agglomeration in the preparation process of the alpha-tricalcium phosphate can be avoided, and the original size structure of the powder is kept;
Zirconium dioxide (chemical formula: ZrO 2) is the main oxide of zirconium, and has a melting point of 2680 ℃ and a boiling point of 4300 ℃. The diamond is white odorless and tasteless crystal under normal conditions, and has the properties of high melting point, high resistivity, high refractive index and low thermal expansion coefficient, so that the diamond is an important high-temperature resistant material, a ceramic insulating material and a ceramic opacifier and is also a main raw material of artificial drilling.
The invention mixes the calcined and sieved powder with zirconium dioxide, then converts alpha-tricalcium phosphate by high temperature, and then sieves the product to obtain alpha-tricalcium phosphate with certain particle size. The prepared product does not agglomerate, does not need to be ground, can be obtained only by sieving, and has simple preparation method.
The principle of the scheme is that zirconia is possibly added to block agglomeration of tricalcium phosphate, and the contact bonding force of tricalcium phosphate and zirconia is greater than that of tricalcium phosphate, so that sintered tricalcium phosphate is not agglomerated.
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, in step 2), the zirconia has a particle size of 200 to 1000 μm, and the powder a has a particle size of 10 to 200 μm.
Preferably, the zirconium dioxide has a particle size of 500 μm;
Preferably, the particle size of the powder a is 150 μm;
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, the mass ratio of powder a to zirconium dioxide is: 1:0.5-2.
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, the mass ratio of powder a to zirconium dioxide is: 1:0.7.
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, in step 2), dispersing agent activated carbon is further added, and the mass ratio of the powder a, zirconium dioxide and dispersing agent activated carbon is: 1:(0.5-2): (0.1-0.5), preferably, the mass ratio of the powder A to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1:0.3.
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, in the step 1), the mass ratio of calcium hydrogen phosphate to calcium carbonate is: (2-2.5) 1, preferably, the mass ratio of calcium hydrophosphate to calcium carbonate added is as follows: 2:1.
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, in the step 1), the calcium hydrogen phosphate and calcium carbonate are mixed at a volume ratio of 1:0.5-2 with alcohol, and ball milled in a ball mill at a speed of 100-200 rpm.
As a preferred embodiment of the method for preparing α -tricalcium phosphate of the present invention, in the step 1), the mass ratio of calcium hydrogen phosphate to calcium carbonate is: 2:1, wherein the grinding is to grind the mixed calcium hydrophosphate, calcium carbonate and alcohol in a volume ratio of 1:2 in a ball mill at a speed of 200 rpm for 30min, heat up to 900 ℃, calcine, cool and pass through a 150-micron sieve;
In the step 2), the particle size of the zirconium dioxide is 300 μm, the particle size of the powder a is 50 μm, and the mass ratio of the powder a to the zirconium dioxide is as follows: 1:0.7, uniformly mixing, heating to 1350 ℃, preserving heat for 4 hours, and cooling.
The invention also provides the alpha-tricalcium phosphate prepared by the preparation method.
The invention also provides application of the alpha-tricalcium phosphate in preparing bone cement products.
Compared with the prior art, the invention has the beneficial effects that:
1) Sintering is not agglomerated, and the original size structure of the powder is maintained;
2) The grinding step of the sintered alpha-tricalcium phosphate is avoided;
3) The preparation process is simple;
4) The zirconium dioxide can be recycled.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
As an example of the preparation method of α -tricalcium phosphate according to the present invention, the preparation method of α -tricalcium phosphate described in this example includes the following steps:
1) calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)42H 2O) with a molar ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling for 40min in a ball mill at the speed of 200 rpm, calcining for 1 h in a muffle furnace at 900 ℃, cooling along with the furnace, and sieving the cooled powder through a sieve with the diameter of 10 mu m to obtain powder A.
2) zirconium dioxide with the average particle diameter of 200 mu m is added into the powder A, and the mass ratio of the powder to the zirconium dioxide is as follows: 1:0.5, uniformly mixing the powder with the alpha-tricalcium phosphate, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 5 hours, taking out, rapidly cooling to room temperature in air, and sieving by a sieve of 10 mu m to obtain the yield of the alpha-tricalcium phosphate of 83 percent.
Example 2
as an example of the preparation method of α -tricalcium phosphate according to the present invention, the preparation method of α -tricalcium phosphate described in this example includes the following steps:
1) calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2O) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder with a 150 mu m sieve to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m is added into the powder A, and the mass ratio of the powder to the zirconium dioxide is as follows: 1:1, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at a heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in air, and sieving by a sieve of 150 mu m to obtain the alpha-tricalcium phosphate with the yield of 90%.
Example 3
As an example of the preparation method of α -tricalcium phosphate according to the present invention, the preparation method of α -tricalcium phosphate described in this example includes the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2O) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling for 20 min in a ball mill at the speed of 200 rpm, calcining for 1 h in a muffle furnace at 900 ℃, cooling along with the furnace, and sieving the cooled powder through a 200-micron sieve to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 1000 μm is added into the powder A, and the mass ratio of the powder to the zirconium dioxide is as follows: 1:2, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at a heating rate of 5 ℃/min, keeping the temperature for 2h, taking out, rapidly cooling to room temperature in air, sieving by a 200 mu m sieve, and obtaining the yield of the alpha-tricalcium phosphate of 81%.
Example 4
As an example of the preparation method of α -tricalcium phosphate according to the present invention, the preparation method of α -tricalcium phosphate described in this example includes the following steps:
1) calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2O) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m and dispersant activated carbon with the average particle diameter of 500 mu m are added into the powder A, and the mass ratio of the powder to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1: 0.1, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 4 hours, taking out, rapidly cooling to room temperature in the air, and sieving by a sieve of 150 mu m to obtain the yield of the alpha-tricalcium phosphate of 92 percent.
Example 5
As an example of the preparation method of α -tricalcium phosphate according to the present invention, the preparation method of α -tricalcium phosphate described in this example includes the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2o) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m and dispersant activated carbon with the average particle diameter of 500 mu m are added into the powder A, and the mass ratio of the powder to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1:0.3, mixing the powder evenly, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in the air, sieving by a sieve of 150 mu m, and obtaining the yield of the alpha-tricalcium phosphate of 94%.
Example 6
As an example of the preparation method of α -tricalcium phosphate according to the present invention, the preparation method of α -tricalcium phosphate described in this example includes the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2o) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m and dispersant activated carbon with the average particle diameter of 500 mu m are added into the powder A, and the mass ratio of the powder to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1: 0.5, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in the air, and sieving by a sieve of 150 mu m to obtain the alpha-tricalcium phosphate with the yield of 90 percent.
Comparative example 1
the preparation method of the alpha-tricalcium phosphate described in the comparative example comprises the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2o) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m is added into the powder A, and the mass ratio of the powder to the zirconium dioxide is as follows: 1:3, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at a heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in air, and sieving by a sieve of 150 mu m to obtain the alpha-tricalcium phosphate with the yield of 42%.
This comparative example is substantially the same as example 2, except that the mass ratio of powder to zirconium dioxide is: 1:1.
Comparative example 2
The preparation method of the alpha-tricalcium phosphate described in the comparative example comprises the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2o) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m is added into the powder A, and the mass ratio of the powder to the zirconium dioxide is as follows: 1:0.3, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 4 hours, taking out, rapidly cooling to room temperature in the air, and sieving by a sieve of 150 mu m to obtain the alpha-tricalcium phosphate with the yield of 36 percent.
This comparative example is substantially the same as example 2, except that the mass ratio of powder to zirconium dioxide is: 1:0.3.
Comparative example 3
the preparation method of the alpha-tricalcium phosphate described in the comparative example comprises the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2O) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) adding alumina with the average particle diameter of 500 mu m into the powder A, wherein the mass ratio of the powder to the alumina is as follows: 1:1, uniformly mixing the powder, heating to 1350 ℃ in a muffle furnace at a heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in air, sieving by a sieve of 150 mu m, and obtaining the yield of the alpha-tricalcium phosphate of 8%.
This comparative example is substantially the same as example 2, except that alumina was added instead of zirconia.
Comparative example 4
The preparation method of the alpha-tricalcium phosphate described in the comparative example comprises the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate (CaHPO)4•2H2O) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) zirconium dioxide with the average particle diameter of 500 mu m and dispersant activated carbon with the average particle diameter of 500 mu m are added into the powder A, and the mass ratio of the powder to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1: 0.05, mixing the powder evenly, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in the air, sieving by a sieve of 150 mu m, and obtaining the yield of the alpha-tricalcium phosphate of 75%.
This comparative example is about the same as example 5 except for the amount of dispersant activated carbon added.
Comparative example 5
The preparation method of the alpha-tricalcium phosphate described in the comparative example comprises the following steps:
1) Calcium carbonate (CaCO)3) And calcium hydrogen phosphate（CaHPO4•2H2O) is calculated by the following ratio of 2:1, adding absolute ethyl alcohol according to the volume ratio of the powder to the alcohol of 1:2, ball-milling in a ball mill at the speed of 200 rpm for 30min, calcining in a muffle furnace at 900 ℃ for 1 h, cooling along with the furnace, and sieving the cooled powder through a sieve of 150 mu m to obtain powder A.
2) Zirconium dioxide with the average particle diameter of 500 mu m and dispersant activated carbon with the average particle diameter of 500 mu m are added into the powder A, and the mass ratio of the powder A to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1: 0.6, mixing the powder evenly, heating to 1350 ℃ in a muffle furnace at the heating rate of 5 ℃/min, keeping the temperature for 4h, taking out, rapidly cooling to room temperature in the air, sieving by a sieve of 150 mu m, and obtaining the yield of the alpha-tricalcium phosphate of 79 percent.
This comparative example is about the same as example 5 except for the amount of dispersant activated carbon added.
the following performance tests were performed on the α -tricalcium phosphates prepared in examples 1 ~ 6 and comparative examples 1 ~ 5.
Powder characteristic analysis:
the particle size of the α -tricalcium phosphate prepared in examples 1 ~ 6 and comparative examples 1 ~ 5 was measured on an WQL (LKY-2) type particle analyzer.
Watch 1
| Number average particle diameter (μm) | Yield of alpha-tricalcium phosphate | |
| Example 1 | 10 | 83% |
| Example 2 | 150 | 90% |
| Example 3 | 200 | 81% |
| Example 4 | 150 | 92% |
| Example 5 | 150 | 94% |
| Example 6 | 150 | 90% |
| Comparative example 1 | 150 | 42% |
| Comparative example 2 | 150 | 36% |
| Comparative example 3 | 150 | 8% |
| comparative example 4 | 150 | 75% |
| Comparative example 5 | 150 | 79% |
As can be seen from table 1, during the preparation of α -tricalcium phosphate, the addition of zirconium dioxide can avoid sintering agglomeration of α -tricalcium phosphate, while the product is still agglomerated after the addition of aluminum oxide. The yield of the non-agglomerated alpha-tricalcium phosphate is related to the particle size of zirconium dioxide and the mass ratio of the alpha-tricalcium phosphate to the zirconium dioxide, when the particle size of the powder A is 20-200 mu m and the particle size of the zirconium dioxide is 200-1000 mu m, the yield of the original particle size of the alpha-tricalcium phosphate is maintained to be 81% -90%, and meanwhile, the yield of the non-agglomerated alpha-tricalcium phosphate can be improved by adding the dispersing agent activated carbon. The product prepared by the preparation method of the alpha-tricalcium phosphate is not agglomerated, the original size structure of the powder can be maintained, the grinding step increased by agglomeration after the alpha-tricalcium phosphate is sintered is avoided, the preparation process is simple, the preparation of the alpha-tricalcium phosphate is not influenced by the added zirconium dioxide, and the zirconium dioxide can be recycled after being sieved.
finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. a preparation method of alpha-tricalcium phosphate is characterized by comprising the following steps:
1) Mixing calcium hydrogen phosphate and calcium carbonate by a solid-phase reaction method, grinding for 20-40min, heating to 850-920 ℃, calcining, cooling, and sieving by a 10-200 mu m sieve to obtain powder A;
2) Adding zirconium dioxide powder into the powder A obtained in the step 1), wherein the particle size of the zirconium dioxide powder is larger than that of the powder A, uniformly mixing, heating to 1125-1500 ℃, keeping the temperature for 2-5h, taking out, and cooling;
3) Sieving to obtain alpha-tricalcium phosphate powder.
2. the process for preparing α -tricalcium phosphate according to claim 1, wherein in step 2), the zirconia has a particle size of 200 to 1000 μ ι η, preferably 500 μ ι η, and the powder a has a particle size of 10 to 200 μ ι η, preferably 150 μ ι η.
3. The method of preparing α -tricalcium phosphate according to claim 2, wherein the mass ratio of powder a to zirconium dioxide is: 1:0.5-2.
4. the method of claim 3, wherein the powder A and zirconium dioxide are present in a mass ratio of: 1:0.7.
5. The method for preparing α -tricalcium phosphate according to claim 3, wherein dispersing agent activated carbon is further added in step 2), and the mass ratio of the powder A, zirconium dioxide and dispersing agent activated carbon is as follows: 1:(0.5-2): (0.1-0.5), preferably, the mass ratio of the powder A to the zirconium dioxide to the dispersant activated carbon is as follows: 1:1:0.3.
6. the method for preparing α -tricalcium phosphate according to claim 1, wherein in said step 1), the calcium hydrogen phosphate and calcium carbonate are added in a mass ratio of: (2-2.5) 1, preferably, the mass ratio of calcium hydrophosphate to calcium carbonate added is as follows: 2:1.
7. the method for preparing α -tricalcium phosphate according to claim 1, wherein in said step 1), said grinding is performed by mixing calcium hydrogen phosphate with calcium carbonate and alcohol in a volume ratio of 1:0.5-2, and ball milling in a ball mill at a speed of 100-200 rpm.
8. The method of preparing α -tricalcium phosphate according to claim 1, wherein,
in the step 1), the mass ratio of calcium hydrophosphate to calcium carbonate is as follows: 2:1, wherein the grinding is to grind the mixed calcium hydrophosphate, calcium carbonate and alcohol in a volume ratio of 1:2 in a ball mill at a speed of 200 rpm for 30min, heat up to 900 ℃, calcine, cool and pass through a 150-micron sieve;
in the step 2), the particle size of the zirconium dioxide is 300 μm, the particle size of the powder a is 50 μm, and the mass ratio of the powder a to the zirconium dioxide is as follows: 1:0.7, uniformly mixing, heating to 1350 ℃, preserving heat for 4 hours, and cooling.
9. an α -tricalcium phosphate prepared according to the preparation process of any one of claims 1 to 8.
10. use of α -tricalcium phosphate according to claim 9 for the preparation of bone cement, dental filling products.
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| CN115246636B (en) * | 2022-03-30 | 2023-10-24 | 南京大学 | Preparation method of bioactive high calcium polyphosphate |
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Denomination of invention: A kind of a-tricalcium phosphate and preparation method thereof Effective date of registration: 20220922 Granted publication date: 20210219 Pledgee: Agricultural Bank of China Limited Guangzhou Development Zone Branch Pledgor: GUANGZHOU RAINHOME PHARM&TECH Co.,Ltd. Registration number: Y2022980015948 |