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Preparation method of hydroxy phosephorite hollow microball

A technology of hydroxyapatite and hollow microspheres, which is applied in the field of preparation of hydroxyapatite microspheres, can solve the problems of difficult large-scale adjustment, high crystallinity of microspheres, complicated process, etc., and achieve simple and easy process operation , large specific surface area and simple preparation process

Inactive Publication Date: 2008-07-02
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After reacting at a certain temperature for a period of time, the glass microspheres are eroded, and finally the Ca-P-OH deposits can be converted into hydroxyapatite after heat treatment at 600°C for 4 hours, and hydroxyapatite microspheres with a hollow structure are prepared. [Huang Wenxuan, Wang Qing, Wang Deping, Preparation technology of hollow hydroxyapatite microspheres, Journal of Tongji University (Natural Science Edition), 2005, 33(1): 88-92], however, the process of this method is relatively complicated, and Requires glass microspheres as a precursor
In addition, the Chinese invention patent (publication number is CN1597610A, publication date is 2005.03.23) "Hydroxyapatite hollow microspheres and its preparation method" reports that the plasma spraying method is used to prepare hydroxyapatite hollow microspheres, but The crystallinity of the obtained microspheres is high and difficult to adjust in a wide range, thus limiting its application in some specific fields

Method used

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  • Preparation method of hydroxy phosephorite hollow microball
  • Preparation method of hydroxy phosephorite hollow microball
  • Preparation method of hydroxy phosephorite hollow microball

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Calcium nitrate tetrahydrate (Ca(NO 3 ) 2 4H 2 O) and diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) as raw material, according to the ratio of calcium to phosphorus molar ratio of 1.67, the hydroxyapatite slurry is prepared by the chemical precipitation method in the wet method, wherein Ca(NO 3 ) 2 4H 2 O and (NH 4 ) 2 HPO 4 The ratio of the mass (g) to the volume (ml) of the final obtained slurry is: 2.98: 1: 17, and the specific chemical reaction formula is:

[0034] 10Ca(NO 3 ) 2 +6(NH4 ) 2 HPO 4 +8NH 4 OH→Ca 10 (PO 4 ) 6 (OH) 2 +20NH 4 NO 3 +6H 2 o

[0035] (2) Dilute the hydroxyapatite slurry with distilled water at a ratio of 5:1 by volume ratio, and add ammonium bicarbonate at a concentration of 0.03 g / ml based on the volume of the diluted hydroxyapatite slurry , mix and stir evenly;

[0036] (3) Under the magnetic stirring speed of 400 rev / min, the above mixed solution is sprayed under the condition that the nozzle diameter is 1mm,...

Embodiment 2

[0042] (1) Calcium nitrate tetrahydrate (Ca(NO 3 ) 2 4H 2 O) and diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) as raw material, according to the ratio of calcium to phosphorus molar ratio of 1.67, the hydroxyapatite slurry is prepared by the chemical precipitation method in the wet method, wherein Ca(NO 3 ) 2 4H 2 O and (NH 4 ) 2 HPO 4 The ratio of the mass (g) to the volume (ml) of the final obtained slurry is: 2.98: 1: 17, and the specific chemical reaction formula is:

[0043] 10Ca(NO 3 ) 2 +6(NH 4 ) 2 HPO 4 +8NH 4 OH→Ca 10 (PO 4 ) 6 (OH) 2 +20NH 4 NO 3 +6H 2 o

[0044] (2) Dilute the hydroxyapatite slurry with distilled water at a ratio of 5:1 by volume ratio, and add ammonium bicarbonate at a concentration of 0.01 g / ml based on the volume of the diluted hydroxyapatite slurry , mix and stir evenly;

[0045] (3) At a magnetic stirring speed of 350 rev / min, spray the above-mentioned mixed solution with a nozzle diameter of 1 mm, an inlet air tempe...

Embodiment 3

[0049] (1) Calcium nitrate tetrahydrate (Ca(NO 3 ) 2 4H 2 O) and diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) as raw material, according to the ratio of calcium to phosphorus molar ratio of 1.67, the hydroxyapatite slurry is prepared by the chemical precipitation method in the wet method, wherein Ca(NO 3 ) 2 4H 2 O and (NH 4 ) 2 HPO 4 The ratio of the mass (g) to the volume (ml) of the final obtained slurry is: 2.98: 1: 17, and the specific chemical reaction formula is:

[0050] 10Ca(NO 3 ) 2 +6(NH 4 ) 2 HPO 4 +8NH 4 OH→Ca 10 (PO 4 ) 6 (OH) 2 +20NH 4 NO 3 +6H 2 o

[0051] (2) Dilute the above-mentioned hydroxyapatite slurry with distilled water at a ratio of 5:1 by volume ratio, and add ammonium bicarbonate at a concentration of 0.05 g / ml based on the volume of the diluted hydroxyapatite slurry , mix and stir evenly;

[0052] (3) At a magnetic stirring speed of 500 rev / min, the above-mentioned mixed solution is sprayed with a nozzle diameter of 1mm...

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Abstract

The present invention discloses a method for preparing hydroxyapatite hollow microsphere. Said method includes the following steps: using tetrahydrate calcium nitrate and ammonium hydrogen phosphate as raw material, adopting chemical precipitation method to prepare hydroxyapatite slurry, then diluting said hydroxyapatite slurry by using distilled water, adding ammonium hydrogen carbonate as additive, uniformly stirring them, spray drying, making following heat treatment so as to obtain the hydroxyapatite hollow microsphere formed from nano grains.

Description

technical field [0001] The invention relates to a preparation method of hydroxyapatite microspheres, in particular to a preparation method of hydroxyapatite hollow microspheres composed of nano crystal grains. Background technique [0002] The structure and composition of hydroxyapatite are similar to the main inorganic parts in human and animal bones and teeth, and it has excellent bioactivity and biocompatibility; currently, it has been used as a bioactive coating for implants and bone defect filling materials. It is widely used in clinical operations such as dentistry, orthopedics, and plastic surgery. [0003] The forms of hydroxyapatite used in clinical and experimental research mainly include dense blocks, porous blocks, solid particles, and porous and hollow particles. However, studies in recent years have shown that the use of irregularly shaped hydroxyapatite materials can easily cause tissue infection and affect the speed of new bone formation. Therefore, hydroxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32A61L27/12
Inventor 吕宇鹏孙瑞雪李木森
Owner SHANDONG UNIV
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