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Preparation of carbonate-containing hydroxylapatite powder

A carbonate hydroxyapatite and powder technology, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of short powder cycle, good crystal crystallinity, and many other metal elements, and achieve raw material Convenient and easy to purchase, increase the unit output, and the effect of high particle crystallinity

Inactive Publication Date: 2011-09-28
CHONGQING UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] It can be seen from the above-mentioned published patents that the sol-gel method is a common preparation method for carbonate-containing hydroxyapatite. This method has a long cycle and low output, which is not conducive to industrial production. The secondary crystallization process is likely to cause powder Pollution; the production cycle of the novel in-situ deposition method is too long, and the glass contains many other metal elements, so it is not easy to obtain hydroxyapatite powder doped with only carbonate groups; there have been many reports on the preparation of hydroxyapatite by hydrothermal method , which proves that the preparation of powder by hydrothermal method has short cycle time, good crystal crystallinity and less pollution, and is especially suitable for fields with high requirements on powder purity, such as the field of biological materials.
However, the technical scheme of preparing carbonate-containing hydroxyapatite powder by hydrothermal and carbon dioxide gas pressure has not been reported yet.

Method used

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  • Preparation of carbonate-containing hydroxylapatite powder
  • Preparation of carbonate-containing hydroxylapatite powder
  • Preparation of carbonate-containing hydroxylapatite powder

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh 4.3319g of calcium nitrate and 2.5182g of dipotassium hydrogen phosphate, and dissolve them in 187.3ml and 110.0ml of distilled water respectively to prepare a solution. Pour the dipotassium hydrogen phosphate solution into the calcium nitrate solution, and stir continuously with a glass rod to mix evenly. Then the solution was poured into the reaction kettle, and the lid of the kettle was closed. The carbon dioxide gas used is 99.5% pure. First pre-fill carbon dioxide gas into the kettle to discharge the air in the kettle, then fill in 0.1MPa carbon dioxide gas, and close the inlet valve. In the hydrothermal process, the heating rate is 1.4°C / min, the reaction temperature is 200°C, the holding time is 3 hours, the stirring speed is 110 rpm during the heating and holding period, and the stirring speed is 50 rpm during the cooling period, cooling with the kettle. After the reaction, the precipitate was filtered with a water circulating vacuum pump to obtain a fil...

Embodiment 2

[0037]Weigh 4.3404g of calcium nitrate and 2.5142g of dipotassium hydrogen phosphate, and dissolve them in 187.3ml and 110.0ml of distilled water respectively to prepare a solution. Pour the dipotassium hydrogen phosphate solution into the calcium nitrate solution, and use a glass rod to continuously stir and mix well. Then the solution was poured into the reaction kettle, and the lid of the kettle was closed. The carbon dioxide gas used is 99.5% pure. First pre-charge carbon dioxide gas into the kettle to discharge the air in the kettle, then fill in 0.21MPa carbon dioxide gas, and close the inlet valve. In the hydrothermal process, the heating rate is 1.32°C / min, the reaction temperature is 200°C, the holding time is 3 hours, the stirring speed is 108 rpm during the heating and holding period, and the stirring speed is 55 rpm during the cooling period, cooling with the kettle. After the reaction, the precipitate was filtered with a water circulation vacuum pump to obtain a...

Embodiment 3

[0039] Weigh 4.3361g of calcium nitrate and 2.5088g of dipotassium hydrogen phosphate, and dissolve them in 187.3ml and 110.0ml of distilled water respectively to prepare a solution. Pour the dipotassium hydrogen phosphate solution into the calcium nitrate solution, and stir continuously with a glass rod to mix evenly. Then the solution was poured into the reaction kettle, and the lid of the kettle was closed. The carbon dioxide gas used is 99.5% pure. First pre-charge carbon dioxide gas into the kettle to discharge the air in the kettle, then fill in 0.4MPa carbon dioxide gas, and close the inlet valve. In the hydrothermal process, the heating rate is 1.25°C / min, the reaction temperature is 200°C, the holding time is 3 hours, the stirring speed is 110 rpm during the heating and holding period, and the stirring speed is 45 rpm during the cooling period, cooling with the kettle. After the reaction, the precipitate was filtered with a water circulation vacuum pump to obtain a ...

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Abstract

The invention relates to a method for preparing hydroxyl apatite powder containing carbonate by introducing carbon dioxide gas for pressurization by adopting a hydrothermal method, which pertains to the field of inorganic non-metallic material. The production method is as follows: calcium nitrate and dipotassium hydrogen phosphate are taken as raw materials, the two dissolve in water in accordance with certain concentration respectively to form solutions which are mixed in accordance with certain Ca / P; and the mixture is put into a high-pressure reaction kettle. Before the reaction kettle is heated, carbon dioxide gas with certain pressure is led in. The hydrothermal reaction is realized by the setting of parameters such certain stirring speed, temperature rise speed, heating temperature and holding time and the like. After the reaction, the hydroxyl apatite powder containing carbonate is obtained by filtration, cleaning and drying. The method is simple and easy to be operated and theobtained power has high degree of crystallinity; the crystal grain takes the shape of rod with primary particle size length of about 500nm and length-diameter ratio of about 2; and carbonate belongs to type A and type B mixed substitution in hydroxyl apatite, and the hydroxyl apatite powder containing carbonate is suitable for industrial production in the biomaterial field.

Description

technical field [0001] The invention relates to a method for preparing carbonate-containing hydroxyapatite powder, specifically a method for preparing carbonate-containing hydroxyapatite powder by using hydrothermal and carbon dioxide gas pressurization, and belongs to the field of inorganic non-metallic materials. Background technique [0002] In physiological bone, a small amount of elements enter the hydroxyapatite lattice in the form of substitution, and the main substitute is carbonate, which accounts for about 5% to 8% in bone mineral mass. Studies have shown that consciously introducing some carbonate groups during the artificial synthesis of hydroxyapatite crystals can improve the bioactivity and osteoconductivity of the material. Carbonate-containing hydroxyapatite powder is currently widely used in hard tissue repair and replacement, and due to its excellent biocompatibility and chemical reactivity to different biological materials, it is also expected to become a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32
Inventor 高家诚张敏陈飞宏
Owner CHONGQING UNIV