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Method for preparing hydroxylapatite ultrafine powder

A technology of hydroxyapatite and ultrafine powder, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problem of large particle size distribution range of products, uniform microscopic mixing of reaction materials, and large differences in reaction environments To achieve the effect of shortening the molecular diffusion distance, reducing the characteristic diffusion time, and realizing energy consumption

Inactive Publication Date: 2010-01-13
BEIJING UNIV OF CHEM TECH
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  • Abstract
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Problems solved by technology

[0005] Traditional typical forced mixing devices such as stirring tanks are mostly intermittently operated, with low production efficiency and high energy consumption. Moreover, the violent agitation of the stirring paddle often cannot achieve uniform microscopic mixing of the reaction materials before the chemical precipitation reaction occurs, making the mixing The reaction environment in different areas of the device is quite different, resulting in a large particle size distribution range of the product particles, which reduces the product quality

Method used

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  • Method for preparing hydroxylapatite ultrafine powder
  • Method for preparing hydroxylapatite ultrafine powder
  • Method for preparing hydroxylapatite ultrafine powder

Examples

Experimental program
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Effect test

Embodiment 1

[0034] see figure 1 . At room temperature, put 10 L of diammonium hydrogen phosphate solution with a concentration of 0.2 mol / L into the storage tank 1, put 16.7 L of calcium nitrate solution with a concentration of 0.2 mol / L into the storage tank 8, and add the two solutions respectively An appropriate amount of ammonia water with a mass concentration of 25% is used to adjust the pH value to 9-12. The two solutions are injected into the casing type annular microchannel reactor 4 through the centrifugal pumps 2 and 7 respectively, and the feed flow rates of the two solutions can be adjusted according to the display values ​​of the rotameters 3 and 6 respectively by adjusting Rotating speed is controlled, wherein the feeding flow of diammonium hydrogen phosphate solution is 30L / hr, and the feeding flow of calcium nitrate solution is 50L / hr. After the reaction was completed, the obtained precursor was put into a hydrothermal kettle for hydrothermal treatment at 220°C for 4 hou...

Embodiment 2

[0037] see figure 1 . At room temperature, put 10 L of diammonium hydrogen phosphate solution with a concentration of 0.2 mol / L into the storage tank 1, put 33.3 L of calcium nitrate solution with a concentration of 0.1 mol / L into the storage tank 8, and add the two solutions respectively An appropriate amount of ammonia water with a mass concentration of 25% is used to adjust the pH value to 9-12. The two solutions are injected into the casing type annular microchannel reactor 4 through the centrifugal pumps 2 and 7 respectively, and the feed flow rates of the two solutions can be adjusted according to the display values ​​of the rotameters 3 and 6 respectively by adjusting Rotating speed is controlled, wherein the feeding flow of diammonium hydrogen phosphate solution is 30L / hr, and the feeding flow of calcium nitrate solution is 100L / hr. After the reaction is complete, put the obtained precursor into a hydrothermal kettle for hydrothermal treatment at 220°C for 4 hours, t...

Embodiment 3

[0039] see figure 1 . At room temperature, put 5 L of diammonium hydrogen phosphate solution with a concentration of 0.4 mol / L into the storage tank 1, put 50 L of calcium nitrate solution with a concentration of 0.0667 mol / L into the storage tank 8, and add an appropriate amount of the two solutions respectively The mass concentration is 25% ammonia water to adjust the pH value to 9-12. The two solutions are injected into the casing type annular microchannel reactor 4 through the centrifugal pumps 2 and 7 respectively, and the feed flow rates of the two solutions can be adjusted according to the display values ​​of the rotameters 3 and 6 respectively by adjusting Rotating speed is controlled, wherein the feeding flow of diammonium hydrogen phosphate solution is 15L / hr, and the feeding flow of calcium nitrate solution is 150L / hr. After the reaction is complete, put the obtained precursor into a hydrothermal kettle for hydrothermal treatment at 220°C for 4 hours, then rinse t...

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Abstract

The invention relates to a method for preparing hydroxylapatite ultrafine powder. The method comprises the following steps that: soluble calcium salt and soluble phosphate aqueous solution react in a sleeve-type annular microchannel reactor at normal temperature to prepare hydroxylapatite precursor; and the precursor is prepared into the hydroxylapatite ultrafine powder through hydro-thermal treatment, washing, drying and other simple subsequent processes. The method has simple equipment and low cost, and can realize continuous operation, thereby greatly shortening the preparation period, and improving the production efficiency; and the hydroxylapatite ultrafine powder product prepared by the method has excellent quality, stable performance and even grain diameter, and has grains which have short-clubbed appearances mainly and diameters of between 40 and 100nm generally.

Description

Technical field: [0001] The invention relates to a preparation method of hydroxyapatite ultrafine powder. Background technique: [0002] At present, the methods for preparing hydroxyapatite powder mainly include solid-state reaction method, sol-gel method, chemical precipitation method, hydrothermal synthesis method and so on. [0003] The process flow of the solid phase reaction method is simple and the production capacity is high, but the disadvantages of this method are that the reaction temperature is high, the mixing of raw materials is not easy, the degree of reaction completion is difficult to control, impurities are easily generated and difficult to eliminate, and the product particles are seriously agglomerated (Zhao Zhongwei et al., Functional Materials , 2007, 38(3): 499~501; Liao Qilong et al., Journal of Sichuan University (Engineering Science Edition), 2003, 35(5): 107~110). Although the sol-gel method has a simple synthesis process and low cost, there are two...

Claims

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Application Information

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IPC IPC(8): C01B25/32
Inventor 陈建峰杨庆邵磊王洁欣郭奋
Owner BEIJING UNIV OF CHEM TECH
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