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Large-size hydroxyapatite porous microsphere material and preparation method thereof

A hydroxyapatite, porous microsphere technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problem that the three strong peaks of HA microspheres are not clearly separated, the crystallinity of the product needs to be improved, and the reaction period is long, etc. To avoid the use of organic solvents and large equipment, improve sphericity and size uniformity, and achieve low production costs

Active Publication Date: 2016-11-16
SHANDONG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0007] Patent CN201510333810.3 discloses the preparation method of HA microspheres. Amino acid is used as regulator, volatile ammonia water is used as pH regulator, and hydrothermal treatment at 180°C is preferred for 10 hours. The prepared HA microspheres are only 6.5 μm, and freeze-drying is required in the later stage. 24-48h, the reaction cycle is longer and the three strong peaks of the prepared HA microspheres are not clearly separated, and the crystallinity of the product needs to be improved

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  • Large-size hydroxyapatite porous microsphere material and preparation method thereof
  • Large-size hydroxyapatite porous microsphere material and preparation method thereof
  • Large-size hydroxyapatite porous microsphere material and preparation method thereof

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Embodiment 1

[0047] A method for preparing large-size HA porous microsphere material, the precursor solution is composed of the following components: n (calcium nitrate tetrahydrate): n (diammonium hydrogen phosphate): n (glutamic acid) = 11:6:15 , The concentrations of calcium nitrate tetrahydrate, diammonium hydrogen phosphate and glutamic acid are 0.108, 0.06 and 0.15 mol / L respectively, urea is 0.8-1.2 mol / L, dilute nitric acid / dilute hydrochloric acid is 0.03-0.08 mol / L, the solvent is Ionized water.

[0048] The preparation method of the above-mentioned precursor solution is as follows: first mix calcium nitrate tetrahydrate, diammonium hydrogen phosphate and urea in a beaker, magnetically stir and add dilute nitric acid / dilute hydrochloric acid until completely dissolved; then add glutamic acid to the solution, After stirring for 0.5h, put it into a hydrothermal kettle to set the reaction temperature to 180°C and the reaction time to be 10h; finally, the white precipitate obtained is c...

Embodiment 2

[0051] A preparation of a large-size HA porous microsphere material, the composition includes the following components by weight: n (calcium chloride): n (dipotassium hydrogen phosphate): n (glutamic acid) = 10.5:5.8:14.5, urea 0.8-1.2mol / L, dilute nitric acid / dilute hydrochloric acid 0.03-0.08mol / L, the solvent is deionized water.

[0052] The preparation method of the above precursor solution is as follows: firstly mix calcium chloride, dipotassium hydrogen phosphate, and urea in a beaker, magnetically stir and add dilute nitric acid or dilute hydrochloric acid until the precipitate is completely dissolved; then add glutamic acid to the solution, After stirring for 0.5h, put it into a hydrothermal kettle to set the reaction temperature to 180°C and the reaction time to be 15h; finally, the white precipitate obtained is centrifuged, washed and dried, and then heat treated for 1h, and the heat treatment temperature is 1000°C.

Embodiment 3

[0054] The preparation of a large-size HA porous microsphere material, the composition includes the following components by weight: n (calcium nitrate): n (disodium hydrogen phosphate): n (glutamic acid) = 10.5:6.2:15.3, urea 0.8 -1.2mol / L, dilute nitric acid / dilute hydrochloric acid 0.03-0.08mol / L, the solvent is deionized water.

[0055] The preparation method of the above precursor solution is as follows: firstly mix calcium nitrate tetrahydrate, diammonium hydrogen phosphate, and urea in a beaker, magnetically stir and add dilute nitric acid / dilute hydrochloric acid until the precipitate is completely dissolved; then add glutamic acid to the solution After stirring for 0.5h, put it into a hydrothermal kettle to set the reaction temperature to 180℃ and the reaction time to 0.5h; finally, the white precipitate obtained is centrifuged, washed and dried, and then heat treated for 1h. The heat treatment temperature is 1000℃.

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Abstract

The invention discloses a large-size hydroxyapatite porous microsphere material and a preparation method thereof. According to the present invention, the method is a hydrothermal homogeneous precipitation method, wherein the necessary amino acid glutamic acid is added into the reactant so as to be adopted as a microsphere growth regulator, and the growth of HA is effectively regulated through the adsorption and chelating effect of the glutamic acid so as to achieve the microsphere shape; and the reaction liquid is adjusted into the acid state, the principle that urea can be slowly decomposed to release OH at a temperature of more than 80 DEG C so as to adjust the pH value of the solution is used to gradually increase the pH value of the solution, such that the microspheres can gradually grow, and the size becomes large.

Description

Technical field [0001] The invention belongs to the field of inorganic biomedical materials, and relates to a large-size porous hydroxyapatite microsphere material and a preparation method thereof. Background technique [0002] Population health is the basic guarantee for the sustainable development of a people-oriented society. Biomedical materials are a new type of high-tech materials used to diagnose, treat, repair or replace human tissues, organs or enhance their functions. Their healthy and rapid development plays an important role in improving people’s quality of life and safeguarding human health. It has gradually become a rapidly developing emerging industry. With the rapid development and mutual penetration of many disciplines such as materials science, medicine, biology, chemistry, physics and modern high technology, biomedical materials, as a new interdisciplinary subject, have gradually become a major hot spot in modern research. At the same time, the development an...

Claims

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Application Information

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IPC IPC(8): C01B25/32
CPCC01B25/32C01P2002/72C01P2004/03C01P2004/32C01P2004/61
Inventor 吕宇鹏齐美丽肖桂勇
Owner SHANDONG UNIV
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