Method for preparing beta-tricalcium phosphate crystal material under low temperature condition

A technology for phase tricalcium phosphate and crystal materials, which is applied in the field of preparation of β-phase tricalcium phosphate crystal materials under low temperature conditions, can solve the problems of difficulty in synthesizing small-scale granular materials and high energy consumption, and achieve low reaction temperature and low energy consumption. The effect of less and low production cost

Active Publication Date: 2016-09-21
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] β-TCP crystal materials are generally prepared by high-temperature calcination or high-temperature solid-state reaction [Document 5: Oliveira, A., et al., A Comparative Study between β-TCP Prepared by Solid State Reaction and by AqueousSolution Precipitation: Application in Cements. Vol.361-363.2007.355-358. Document 6: Gibson, I., et al., Characterization of the transformation from calcium-deficient apatite tobeta-tricalcium phosphate. Journal of Materials Science: Materials in Medicine, 2000.11(12): p.799.], high energy consumption, difficult to synthesize smaller granular materials (such as nanoparticles)

Method used

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  • Method for preparing beta-tricalcium phosphate crystal material under low temperature condition
  • Method for preparing beta-tricalcium phosphate crystal material under low temperature condition
  • Method for preparing beta-tricalcium phosphate crystal material under low temperature condition

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Experimental program
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Effect test

Embodiment 1

[0033] Solution preparation: weigh 4.44 grams of anhydrous CaCl 2 Dissolve in 400 ml of deionized water, stir well to obtain CaCl with a concentration of 0.1 mol / L 2 Solution, mix 4.06 grams of MgCl in the ratio of 1:2 according to the molar ratio of magnesium to calcium 2 ·6H 2 O powder, stir well to make MgCl 2 Completely dissolved to give CaCl 2 and MgCl 2 mixture. Weigh 4.24 g of anhydrous Na 2 CO 3 Dissolve in 400ml deionized water to prepare Na with a concentration of 0.1mol / L 2 CO 3 solution.

[0034] Rapid precipitation reaction: the prepared 400 ml CaCl 2 and MgCl 2 Mix the solution with 400 mL of Na 2 CO 3 The solutions were mixed, magnetically stirred (700rpm), and immediately poured into a Buchner funnel for suction filtration under reduced pressure, followed by washing with deionized water for 3 times and absolute ethanol for 1 time. Obtain Mg-containing amorphous calcium carbonate ( figure 1 (A)).

[0035] Crystallization of amorphous calcium carb...

Embodiment 2

[0039] Solution preparation: weigh 4.44 grams of anhydrous CaCl 2 Dissolve in 400 ml of deionized water, stir well to obtain CaCl with a concentration of 0.1 mol / L 2 solution, and then mixed with 8.12 grams of MgCl according to the ratio of magnesium to calcium molar ratio of 1:1 2 ·6H 2 O powder, stir well to make MgCl 2 Completely dissolved to give CaCl 2 and MgCl 2 mixture. And weigh 4.24 grams of anhydrous Na 2 CO 3 Dissolve in 400ml deionized water to prepare Na with a concentration of 0.1mol / L 2 CO 3 solution.

[0040] Rapid precipitation reaction: the prepared 400 ml CaCl 2 and MgCl 2 Mix the solution with 400 mL of Na 2 CO 3 The solutions were mixed, stirred evenly by magnetic force (700rpm), immediately poured into a Buchner funnel for vacuum filtration, and then washed with deionized water for 3 times and absolute ethanol for 1 time. Obtain Mg-containing amorphous calcium carbonate ( figure 2 (A); Figure 5 (A, B)).

[0041] Amorphous calcium carbon...

Embodiment 3

[0046] Solution preparation: Weigh 4.11 grams of Ca(NO 3 ) 2 4H 2 O was dissolved in 20 ml of deionized water, and the Ca(NO 3 ) 2 solution, then according to the ratio of calcium to magnesium molar ratio of 9:1 mixed with 0.49g gram of Mg (NO 3 ) 2 ·6H 2 O powder, stir well to make Mg(NO 3 ) 2 Completely dissolved, Ca(NO 3 ) 2 and Mg(NO 3 ) 2 The solution was mixed and its pH was adjusted to 10 with 25 wt.% ammonia solution. and weighed 1.54 g (NH 4 ) 2 HPO 4 Dissolve in 20 ml of deionized water to prepare a concentration of 0.64mol / L (NH 4 ) 2 HPO 4 Solution, its pH value was adjusted to 10 with 25wt.% ammonia solution. 20 ml of the prepared Ca(NO 3 ) 2 and Mg(NO 3 ) 2 Mix the solution with 20 ml (NH 4 ) 2 HPO 4 Solution mixing, magnetic stirring (300rpm) is even, obtains the amorphous apatite ( image 3 (A)) Emulsion.

[0047] Hydrothermal synthesis reaction: place the amorphous apatite emulsion containing 10% Mg in a hydrothermal reaction kettle,...

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Abstract

The invention discloses a method for preparing a beta-tricalcium phosphate crystal material under a low temperature condition, and belongs to the technical field of biomaterials. The method comprises the following steps: preparing amorphous calcium carbonate doped with different contents of Mg and amorphous apatite doped with different contents of Mg and Sr through a rapid precipitation technology, and converting the Mg-containing calcite and the amorphous apatite containing Mg and Sr into Mg-doped or Mg and Sr codoped beta-TCP crystal material through using a hydrothermal synthesis technology. Compared with present high temperature calcining or solid phase reaction methods for preparing the beta-TCP crystal material, the method disclosed in the invention has the advantages of low reaction temperature, production cost reduction, and solving of the problem of preparation of beta-TCP crystal nanomaterial through a high temperature reaction. Mg and Sr element doping also can improve the bioactivity of the beta-TCP material, is in favor of promoting bone restoration, and has great values in the fields of bone restoration and bone transplantation.

Description

technical field [0001] The invention relates to the technical field of biological materials, in particular to a method for preparing a β-phase tricalcium phosphate (β-TCP) crystal material under low temperature conditions. Background technique [0002] β-phase tricalcium phosphate (β-TCP) has a similar composition to the inorganic salt of human bone. β-TCP bioceramics, as one of the commonly used bone defect repair materials in clinical practice, has the following advantages: good biocompatibility and osteoconduction [Document 1: Rezwan, K., et al., Biodegradable and bioactive porous polymer / inorganic composite scaffolds for bone tissue engineering. Biomaterials, 2006.27(18): p.3413-3431. Document 2: Vecchio, K.S., et al. ,Conversion of sea urchin spines toMg-substituted tricalcium phosphate for bone implants.Acta Biomaterialia,2007.3(5):p.785-793.Document 3:Gao,Z.,et al.,Vitalization of tubular coral scaffolds with cell sheets for regeneration of long bones: a preliminary ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32C01B25/34A61L27/12A61L27/04
CPCA61L27/047A61L27/12A61L2430/02C01B25/32C01B25/34C01P2002/72C01P2004/04C01P2004/64
Inventor 张兴崔嵬曹磊杨锐
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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