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Preparation method of hydroxyapatite microsphere

A technology of hydroxyapatite and microspheres, which is applied in the field of preparation of hydroxyapatite microspheres, can solve the problems of high cost, complicated production process, unfavorableness and the like, achieves large specific surface and pores, good application prospects, easy to obtain Effect

Inactive Publication Date: 2009-01-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

QianjunHe et al. (Materials Letters 61 (2007) 141-143; Journal of Crystal Growth 300 (2007) 460-466) use diammonium hydrogen phosphate, calcium nitrate, urea as raw materials, Na 2 EDTA was used as a template, and a flower-shaped hydroxyapatite microsphere with perfect shape was prepared under the hydrothermal condition of 0.12MPa. Unfavorable in industrial production; Nishioka Hidehiko, Japan, etc. (CN1190282A) prepared a petal-shaped porous hydroxyapatite microsphere by reacting calcium carbonate and phosphoric acid or calcium phosphate salt, and the specific surface area can be 100-200m 2 / g adjustment, but this method requires the preparation of nano-scale calcium carbonate with satisfactory morphology, the production process is complicated and the cost is high

Method used

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  • Preparation method of hydroxyapatite microsphere
  • Preparation method of hydroxyapatite microsphere
  • Preparation method of hydroxyapatite microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0023] In the first step, at 0.6 mol / L Ca(OH) 2 Add 100ml of the suspension into a three-necked flask placed on an electric heating mantle, and add 10ml of 0.3 mol / liter EDTA ammonium salt under stirring;

[0024] In the second step, 20ml of 0.36 mol / L (NH 4 ) 2 HPO 4 and 80ml of 0.6 mol / l NH 4 HCO 3 After the solution is mixed evenly, it is gradually added dropwise into the three-necked flask, the dropwise addition time is 120min, and the stirring speed is 800r / min;

[0025] In the third step, the three-necked flask was heated to 50°C, and 80ml of 0.36 mol / L H 3 PO 4 solution, the dropping time is 150min, and after the dropping is completed, the reaction is continued for 300min to obtain hydroxyapatite slurry;

[0026] In the fourth step, the slurry is naturally cooled overnight, filtered, washed twice with deionized water, and then dried in a vacuum oven at 50°C for 24 hours, and ground after cooling to obtain hydroxyapatite microspheres .

[0027] The XRD figure an...

Embodiment 2

[0029] In the first step, at 0.4 mol / L Ca(OH) 2 Add 100ml of the suspension into a three-neck flask placed on an electric heating mantle, and add 5ml of 0.3 mol / liter EDTA ammonium salt under stirring;

[0030] In the second step, 50ml of 0.24 mol / L (NH 4 ) 2 HPO 4 and 50ml of 0.4 mol / l NH 4 HCO 3 After the solution is mixed evenly, it is gradually added dropwise into the three-necked flask, the dropping time is 120min, and the stirring speed is 500r / min;

[0031] In the third step, the three-neck flask was heated to 80°C, and 50ml of 0.24 mol / L H 3 PO 4 solution, the dropping time is 100min, and after the dropping is completed, the reaction is continued for 200min to obtain hydroxyapatite slurry;

[0032] In the fourth step, the slurry is naturally cooled overnight, filtered, washed twice with deionized water, and then dried in a vacuum oven at 50°C for 24 hours, and ground after cooling to obtain hydroxyapatite microspheres .

[0033]After testing: the phase of the ...

Embodiment 3

[0035] In the first step, at 0.6 mol / L Ca(OH) 2 Add 100ml of the suspension into a three-necked flask placed on an electric heating mantle, and add 10ml of 0.3 mol / liter EDTA ammonium salt under stirring;

[0036] In the second step, 70ml of 0.36 mol / liter (NH 4 ) 2 HPO 4 and 30ml of 0.6 mol / l NH 4 HCO 3 After the solution is mixed evenly, it is gradually added dropwise into the three-necked flask, the dropping time is 120min, and the stirring speed is 900r / min;

[0037] In the third step, the three-necked flask was heated to 80°C, and 30ml of 0.36 mol / L H 3 PO 4 solution, the dropping time is 60min, and after the dropping is completed, the reaction is continued for 300min to obtain hydroxyapatite slurry;

[0038] In the fourth step, the slurry was naturally cooled overnight, washed twice with deionized water, then dried in a vacuum oven at 50° C. for 24 hours, and ground after cooling to obtain hydroxyapatite microspheres.

[0039] The SEM image of the obtained hydrox...

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Abstract

The invention provides a preparation method of a hydroxyapatite micro-sphere, comprising: firstly, adding a soluble EDTA salt solution of 0.1 to 3M to a Ca(OH)2 suspension of 0.2 to 1.5M; secondly, further adding a mixture of (NH4)2HPO4 solution of 0 to 1.3M and NH4HCO3 solution of 0.2 to 1.5M to obtain a slurry; and the mole number of HCO3<-> in the mixture plus the mole number of 5 / 3HPO4<2-> is equal to the mole number of Ca<2+> in the suspension; thirdly, adding an H3PO4 or (NH4)2HPO4 solution of 0.1 to 1.0M in drops to the slurry with a temperature between 40 and 90DEG C to make the calcium-phosphorus molar ratio in the slurry be 1.66 to 1.7:1, and obtaining a hydroxyapatite slurry after the reaction for 1 to 12hr; and fourthly, obtaining the hydroxyapatite micro-sphere by cooling, filtering, washing and drying the hydroxyapatite slurry. The method is simple and convenient, and is high in specific surface area of products.

Description

technical field [0001] The invention relates to a preparation method of hydroxyapatite microspheres. Background technique [0002] High specific surface hydroxyapatite microspheres have broad application prospects in many fields such as artificial bone preparation, drug sustained release, chemical engineering, materials and environmental protection. At present, the methods for preparing hydroxyapatite microspheres with high specific surface area can be roughly divided into mechanical methods, combustion methods, hard template methods, and soft template methods. For example, the Chinese patent (patent No. 200610069677.6) first utilizes the chemical precipitation method to prepare hydroxyapatite slurry, and then adds ammonium bicarbonate to spray to obtain a hollow hydroxyapatite microsphere; the patent (WO2005 / 102405A1) discloses a A method for preparing porous material by adding flammable components into precursor slurry, drying and calcining. S. Madhavi et al. (Journal of...

Claims

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Application Information

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IPC IPC(8): C01B25/32
Inventor 王迎军喻新平魏坤陈晓峰
Owner SOUTH CHINA UNIV OF TECH
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