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Alpha-hemihydrate gypsum/ hydroxyapatite composite microsphere and preparation method thereof

A technology of hydroxyapatite and composite microspheres, which is applied in the fields of pharmaceutical formulation, medical science, tissue regeneration, etc., and can solve the problems of slow degradation, unfavorable bone tissue repair and replacement, unfavorable industrial production, etc.

Active Publication Date: 2018-09-14
HUBEI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, one of the main disadvantages of hydroxyapatite is that the degradation rate in the body is slow, the absorption effect is poor, and the implantation in the body affects the growth of new bone.
[0005] The degradation rate of α-hemihydrate gypsum is too fast, while the degradation rate of hydroxyapatite is slow. If these two substances are used directly, they are not conducive to the repair and replacement of bone tissue.
In order to prepare composite materials with excellent biological properties, a Chinese invention patent (patent number: ZL200710063903.4) discloses a new type of bone graft material, which is composed of α-hemihydrate gypsum and β-tricalcium phosphate in a certain proportion; Chinese invention The patent (application number 201110416270.7) discloses a hydroxyapatite-coated α-hemihydrate composite particle with a core-shell structure, which has certain application prospects in bone repair; the Chinese invention patent (application number 201010185090.8) discloses A composite bone repair material formed by blending α-hemihydrate gypsum and hydroxyapatite. It is worth pointing out that in this patent, α-hemihydrate gypsum and hydroxyapatite are simply mixed. The comprehensive performance of the repair material not effectively regulated
In addition, the preparation conditions of this patent are high temperature and high energy consumption, which is not conducive to industrial production

Method used

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  • Alpha-hemihydrate gypsum/ hydroxyapatite composite microsphere and preparation method thereof
  • Alpha-hemihydrate gypsum/ hydroxyapatite composite microsphere and preparation method thereof
  • Alpha-hemihydrate gypsum/ hydroxyapatite composite microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation:

[0029] Add 500ml distilled water, 8g hyperbranched polyethyleneimine, 50g CaCl 2 and 300g of dihydrate gypsum, stirred thoroughly, adjusted the pH value to 5.0 with dilute hydrochloric acid with a mass concentration of 25% to obtain a suspension, heated the suspension to 95°C, and reacted at a constant temperature for 3.5h. Under stirring, add 35g disodium hydrogen phosphate (Na 2 HPO 4 12H 2 (0), and slowly add dropwise a concentration of 1mol / L sodium hydroxide solution until the pH value reaches 10. Continue to react at a constant temperature of 85°C for 10 hours. After the reaction, the product after the reaction is suction-filtered, the solid is washed twice with absolute ethanol, and dried in a drying oven at a constant temperature of 50°C for 3 hours to obtain α-hemihydrate gypsum / hydroxyapatite Stone composite microspheres.

[0030] Sample Characterization:

[0031] Such as figure 1 As shown, the average particle size of the α-hemihydrate g...

Embodiment 2

[0032] Preparation:

[0033] Add 500ml distilled water, 7g hyperbranched polyethyleneimine, 80g CaCl 2 and 300g of dihydrate gypsum, stir well, adjust the pH value to 5.5 with dilute sulfuric acid to obtain a suspension, heat the suspension to 95°C, and react at constant temperature for 3.5h. Under stirring, add 60g disodium hydrogen phosphate (Na 2 HPO 4 12H 2(0), and slowly add dropwise a concentration of 1mol / L sodium hydroxide solution until the pH value reaches 10. Continue to react at a constant temperature of 85°C for 10 hours. After the reaction, the product after the reaction is suction-filtered, the solid is washed twice with absolute ethanol, and dried in a drying oven at a constant temperature of 50°C for 3 hours to obtain α-hemihydrate gypsum / hydroxyapatite Stone composite microspheres.

[0034] Sample Characterization:

[0035] The average particle size of the composite microspheres prepared in Example 2 is about 180 μm. Microspheres are hollow structures ...

Embodiment 3

[0037] Preparation:

[0038] Add 500ml distilled water, 10g hyperbranched polyethyleneimine, 100g CaCl 2 and 320g of dihydrate gypsum, stir well, adjust the pH value to 6.0 with dilute sulfuric acid to obtain a suspension, heat the suspension to 95°C, and react at a constant temperature for 4.0h. Under stirring, add 100g disodium hydrogen phosphate (Na 2 HPO 4 12H 2 (0), and slowly add dropwise a concentration of 1mol / L sodium hydroxide solution until the pH value reaches 10. Continue to react at a constant temperature of 80°C for 12 hours. After the reaction, filter the reacted product with suction, wash the solid twice with absolute ethanol, and dry it in a drying oven at a constant temperature of 60°C for 2 hours to obtain α-hemihydrate gypsum / hydroxyapatite Stone composite microspheres.

[0039] Sample Characterization:

[0040] The average particle size of the composite microspheres prepared in Example 3 is about 200 μm. Microspheres are hollow structures formed by...

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Abstract

The invention provides an alpha-hemihydrate gypsum / hydroxyapatite composite microsphere and preparation method thereof. The preparation method includes the steps of: (1) adding distilled water, hyperbranched polyethyleneimine, calcium salt and dihydrate gypsum to a reaction vessel to be fully stirred and adjusting pH value to be 4.5-6.5 to obtain suspension; (2) heating the suspension to 90-97 DEG C and conducting reaction for 3-5 hours, adding disodium hydrogen phosphate , adjusting the pH value to be 10 and performing reaction for 8-15 hours at the constant temperature of 80-85 DEG C and obtaining composite microsphere slurry; (3) carrying out suction filtration of the composite microsphere slurry, washing solids 2 to 3 times with absolute ethanol and drying to obtain the alpha-hemihydrate gypsum / hydroxyapatite composite microsphere. The preparation method of the alpha-hemihydrate gypsum / hydroxyapatite composite microsphere has the advantages of being capable of preparing the composite microsphere with large specific surface area and a stable structure through simple procedures, and regulating the degradation properties of composite microsphere materials according to different content of hydroxyapatite in the microsphere.

Description

technical field [0001] The invention belongs to the field of preparation of biomedical materials, and in particular relates to an α-hemihydrate gypsum / hydroxyapatite composite microsphere and a preparation method thereof. technical background [0002] Today, there are more and more cases of bone defects caused by trauma, infection or other bone diseases, and the number of autogenous and heterogeneous bodies is far from meeting the clinical needs of bone transplantation. The need is growing. In order to meet different application requirements, researchers have prepared alternative materials in various forms. Among these materials, microsphere materials have attracted more and more attention because of their good fluidity and injection properties, high strength, and not easy to agglomerate. [0003] α-hemihydrate gypsum is a widely recognized bone defect filling and repairing material, which has good biocompatibility and osteoconductivity. However, α-hemihydrate gypsum degr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L27/12A61L27/02A61L27/50A61L27/58
CPCA61L27/025A61L27/12A61L27/50A61L27/58A61L2400/06A61L2430/02
Inventor 冯驸胡颖胡卫兵胡盛余爱农陈栋栋薛凡凡
Owner HUBEI UNIV FOR NATITIES