Preparation method of biphasic calcium phosphate composite powder synthesized by high-temperature solid-state reaction

A high-temperature solid-state reaction, biphasic calcium phosphate technology, applied in the direction of prosthesis, tissue regeneration, medical science, etc., can solve the problem of inability to effectively control the grain size and crystallinity of HA and β-TCP, unsuitable for mass production, very difficult Difficult two-phase structure and other problems, to achieve the effect of low raw material cost, controllable grain size and crystallinity, and uniform distribution of two phases

Active Publication Date: 2020-02-07
SUZHOU DINGAN ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method involves the formation of sol and gel and the calcination process of gel, which is not only complicated in process, but also has polluting gas emissions. The reaction uses ester as a raw material and requires higher cost, so it is not suitable for industrialized mass production.
[0008] (5) Calcium-deficient hydroxyapatite (CDHA) is synthesized by a liquid phase method, and then calcined at about 700°C to partially decompose it to obtain a two-phase composite powder of HA and β-TCP, but this The CDHA used in the process method is usually produced by the liquid phase method. Therefore, it not only has the inherent environmental protection problems of the liquid phase method, but also it is difficult to obtain a large range of HA / β-TCP phase ratio and stable content through the control of process parameters during the calcination process. , uniformly distributed two-phase structure, and cannot effectively control the grain size and crystallinity of each phase of HA and β-TCP

Method used

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  • Preparation method of biphasic calcium phosphate composite powder synthesized by high-temperature solid-state reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] BCP (99wt% β-TCP+1wt% HA)

[0056] Weigh 200.78g calcium carbonate and 688.36g dibasic calcium phosphate dihydrate respectively, add 250ml ethanol and ball mill for 25h, the mass ratio of raw material and ball milling medium is 1:4, the ball mill speed is 450rpm to obtain a uniform mixed slurry, and then dry and crush. Place the dried and crushed mixed powder in a corundum crucible, and move it into a muffle furnace for calcination. When the temperature is raised to 700℃, the deionized water is introduced at a rate of 0.2ml / min, and it is calcined at 900℃ for 5 hours. After the furnace is cooled down, the desired product is obtained. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis results show that the product is BCP (99wt%β-TCP+1wt%HA) composite powder with a grain size of 0.1-2μm and a crystallinity of more than 75%.

Embodiment 2

[0058] BCP (1wt% β-TCP+99wt% HA)

[0059] Weigh 266.2g calcium carbonate and 688.4g dibasic calcium phosphate dihydrate, the mass ratio of raw material and ball milling medium is 1:4, add 500ml deionized water and ball mill for 18h, the speed of the ball mill is 350rpm to obtain a uniform mixed slurry, and then dry Shattered. Place the dried and crushed mixed powder into the device for calcination. When the temperature is raised to 700°C, deionized water is introduced at a rate of 1ml / min, and finally the temperature is raised to 1200°C and kept for 3h, and the temperature is reduced to 800 at a rate of 5°C / min. Stop passing the deionized water after temperature, and obtain the required BCP (1wt% β-TCP+99wt% HA) composite powder after natural cooling. XRD and SEM analysis results show that the product has a crystal grain size of 2-15 μm and a crystallinity of over 85%.

Embodiment 3

[0061] BCP (10wt% β-TCP+90wt% HA)

[0062] Weigh 391.15g calcium carbonate and 1036.50g dibasic calcium phosphate dihydrate, the mass ratio of raw material and ball milling medium is 1:3, add 520ml deionized water and ethanol mixed ball mill solvent and ball mill for 4h, the ball mill speed is 350rpm, to obtain a uniform mixed slurry Material, and then dried and crushed. Place the dried and crushed mixed powder in the device for calcination. When the temperature is raised to 700°C, deionized water is introduced at a rate of 3ml / min, and finally the temperature is raised to 1150°C and kept for 8h, and the temperature is reduced to 800 at a rate of 4°C / min. Stop passing in deionized water after ℃, and obtain the required BCP (10wt% β-TCP+90wt% HA) composite powder after natural cooling. XRD and SEM analysis results show that the crystal grain size of the product is 10-27 μm, and the crystallinity is about 80%.

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Abstract

The invention discloses biphase calcium phosphate (BCP) composite powder synthesized by a high-temperature solid phase reaction. BCP powder is biphase composite powder prepared from hydroxyapatite (HA) and beta-tricalcium phosphate (beta-TCP), in which the molar ratio Ca / P of calcium to phosphorus is 1.5 to 1.67, wherein the value ranges of the relative mass percent of HA and beta-TCP two phases are each 1 to 99 percent; the sizes of crystalline grains of the HA and beta-TCP two phases are 20nm to 300 microns; the crystallinity is 50 to 100 percent. The invention also discloses a preparation method of the BCP composite powder synthesized by the high-temperature solid phase reaction. The BCP composite powder is prepared through the high-temperature solid phase reaction of a calcium-containing solid compound and a calcium-phosphorus solid containing compound. The BCP composite powder has the advantages that a reaction period is short; the costs of raw materials are low; the equipment investment is low; no waste gas and waste water are discharged; further, the proportion of the HA and beta-TCP two phase in the BCP powder is easily regulated and controlled at the same time; the two phases are distributed uniformly; the sizes of the crystal grains and the crystallinity are controllable; finally; the production requirement that the compression strength of BCP biphase composite ceramic is improved or a degradation speed is regulated and controlled is met.

Description

Technical field [0001] The invention relates to the technical field of bioactive materials and orthopedic implants, in particular to a method for preparing hydroxyapatite and β-tricalcium phosphate dual-phase composite powder synthesized by high-temperature solid-phase reaction. Background technique [0002] Bone transplantation is the main method to treat bone defects. Autologous bone transplantation, as the gold standard of bone transplantation, has achieved good results in clinical practice, but its sources are limited, and there are surgical complications of bone removal. The source of allogeneic demineralized bone is limited and there is immunogenicity, unstable osteoinduction, long-term absorption, and risk of infection during the perioperative period and later. Hydroxyapatite (HA) has excellent biocompatibility, can conduct bone regeneration faster, and can directly bond with bone without passing through an intermediate medium. However, the hydroxyapatite obtained by the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/447C04B35/626A61L27/42A61L27/10A61L27/58A61L27/50
CPCA61L27/10A61L27/425A61L27/50A61L27/58A61L2430/02C04B35/447C04B35/6261C04B35/62645C04B2235/3212
Inventor 徐传艳朱阳光李亚东李亚军
Owner SUZHOU DINGAN ELECTRONICS TECH
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