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Biphase calcium phosphate (BCP) composite powder synthesized by high-temperature solid phase reaction and preparation method thereof

A high-temperature solid-state reaction, biphasic calcium phosphate technology, applied in prosthetics, medical science, tissue regeneration, etc., can solve the problem of inability to effectively control the grain size and crystallinity of HA and β-TCP, unsuitable for mass production, and pollution Low cost of raw materials, controllable grain size and crystallinity, and low equipment investment

Active Publication Date: 2017-09-19
SUZHOU DINGAN ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Biphase calcium phosphate (BCP) composite powder synthesized by high-temperature solid phase reaction and preparation method thereof

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preparation example Construction

[0034] The present invention also provides a method for preparing a biphasic calcium phosphate composite powder synthesized by a high-temperature solid-state reaction, comprising the following steps:

[0035] S1. Take the measured calcium-containing solid compound and calcium-phosphorus solid compound as raw materials, and the molar ratio of calcium to phosphorus Ca / P in the raw material is 1.5-1.67;

[0036] S2. Using wet ball milling, using ethanol and / or deionized water as the ball milling solvent, and using zirconia or aluminum oxide or tungsten carbide particles as the ball milling medium, the raw materials in step S1 are ball milled and mixed evenly;

[0037] S3. Take out the powder slurry uniformly mixed by ball milling in step S2, put it in a container to dry or put it in a constant temperature box to dry, and then pulverize it into uniform and fine mixed powder;

[0038] S4. Put the mixed powder obtained by crushing in step S3 into a corundum crucible and place it in ...

Embodiment 1

[0055] BCP (99wt% β-TCP+1wt% HA)

[0056] Weigh 200.78g of calcium carbonate and 688.36g of calcium hydrogen phosphate dihydrate, add 250ml of ethanol and ball mill for 25 hours, the mass ratio of raw materials and ball milling medium is 1:4, and the ball mill speed is 450rpm to obtain a uniformly mixed slurry, which is then dried and pulverized. Put the dried and pulverized mixed powder in a corundum crucible, and move it into a muffle furnace for calcination. When the temperature rises to 700°C, pour in deionized water at a rate of 0.2ml / min, and calcine at 900°C for 5 hours. The desired product was obtained after the furnace was cooled down. X-ray diffraction (XRD) and scanning electron microscope (SEM) analysis results showed that the product was 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 of calcium carbonate and 688.4g of calcium hydrogen phosphate dihydrate, the mass ratio of raw materials and ball milling medium is 1:4, add 500ml of deionized water and ball mill for 18 hours, the speed of the ball mill is 350rpm, obtain a uniformly mixed slurry, and then dry smash. Put the dried and pulverized mixed powder into the device for calcination. When the temperature rises 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 3 hours, and the temperature is lowered to 800°C at a rate of 5°C / min. After ℃, the deionized water was stopped, and the desired BCP (1wt% β-TCP+99wt% HA) composite powder was obtained after natural cooling. The results of XRD and SEM analysis show that the grain size of the product is 2-15 μm, and the crystallinity is above 85%.

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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 dual-phase composite powder of hydroxyapatite and β-tricalcium phosphate synthesized by high-temperature solid-state reaction and a preparation method thereof. Background technique [0002] Bone grafting is the main method for treating bone defects. As the gold standard of bone transplantation, autologous bone transplantation has achieved good results in clinical practice, but its source is limited and there are surgical complications at the bone harvesting site. Allogeneic demineralized bone has limited sources and risks of immunogenicity, unstable osteoinductivity, long-term resorption, perioperative and subsequent infection. Hydroxyapatite (HA) has excellent biocompatibility, can conduct bone regeneration relatively quickly, and can directly bond with bone without passing through an intermediate medium. However, the crystallinity of HA ob...

Claims

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Application Information

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Patent Type & Authority Applications(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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