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Technological process for preparing beta-tricalcium phosphate micro powder by sol-gel self-propagating combustion method

A tricalcium phosphate micropowder, self-propagating combustion technology, applied in the field of chemical and biological materials, can solve the problems of difficult to accurately control the material ratio, uneven particle size of β-TCP, easy mixing of impurity phases, etc., to achieve a single crystal phase, The effect of small average particle size and uniform distribution

Inactive Publication Date: 2011-07-06
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently reported methods involving the preparation of β-TCP mainly fall into two categories, namely, wet method and dry method, both of which have their own strengths, but also have shortcomings. The main disadvantages are: high reaction temperature, high temperature heat treatment is required; The particle size of the obtained β-TCP is uneven, the average particle size is large; the crystal phase is impure; the material ratio is not easy to control accurately, the reaction time is long, and the impurity phase is easy to mix in, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Accurately weigh 0.0926mol of Ca(NO 3 ) 2 4H 2 O, 0.0926mol of citric acid and 0.0617mol of (NH 4 )H 2 PO 4 , were dissolved in 200ml deionized water respectively to obtain respective transparent solutions; under stirring conditions, the above citric acid solution, (NH 4 )H 2 PO 4 The solution was slowly added dropwise to the Ca(NO 3 ) 2 in solution. During the reaction, slowly drop by drop 0.5mol l -1 Adjust the pH value of the reaction solution to 2 with dilute nitric acid, slowly heat and hydrolyze until the sol appears. Then, the temperature was raised to 80°C, stirred, and the water was slowly evaporated at a constant temperature, and the sol was transformed into a gel. Then raise the temperature to 95° C., continue to evaporate water, and make the gel completely form a xerogel. Collect the dry gel and move it into a constant temperature electric furnace at 250°C. In the furnace, the dry gel is spontaneously ignited, burns rapidly, expands in volume, an...

Embodiment 2

[0020] Accurately weigh 0.0926mol of Ca(NO 3 ) 2 4H 2 O, 0.0926mol of citric acid and 0.0597mol of (NH 4 )H 2 PO 4 , were dissolved in 200ml deionized water to obtain respective transparent solutions. Under stirring conditions, the above citric acid solution, (NH 4 )H 2 PO 4 The solution was slowly added dropwise to the Ca(NO 3 ) 2 in solution. During the reaction, slowly drop by drop 0.5mol l -1 Adjust the pH value of the solution to 4 with dilute nitric acid, and slowly heat and hydrolyze until the sol appears. Then, the temperature was raised to 90°C, stirred, and the water was slowly evaporated at a constant temperature, and the sol was transformed into a gel. Then raise the temperature to 100°C, continue to evaporate water, and make the gel completely form a xerogel. Collect the dry gel and move it into a constant temperature electric furnace at 350°C. In the furnace, the dry gel is spontaneously ignited, burns rapidly, expands in volume, and produces white p...

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Abstract

The present invention belongs to ceramic material and the preparation field thereof, and relates to a new method for preparing Beta-tricalcium phosphate micro-powders, which comprises the steps as follows: citric acid solution is dropwise added in a soluble calcium salt solution that is Ca (NO3)2, the quantity of the citric acid solution is equal to that of the Ca (NO3)2, and then (NH4)H2PO4 solution is added, so as to lead the mol ratio (nCa / nP) between calcium atoms and phosphorus atoms to be kept between 1.47 to 1.55 in the solution; diluted nitric acid is utilized to adjust until the pH value of the solution is 2 to 4, and the solution is hydrolyzed to form collosol through heating; the collosol is heated to vaporize the moisture contents until gelatin and xerogel are formed; the xerogel is moved to an electric furnace, the temperature of which is 250 to 350 DEG C, the xerogel is ignited spontaneously quickly in the electric furnace, the self-propagating combustion occurs rapidly, the volume expands, and white powders are generated. The white powders are calcined to obtain a shaggy coralloid fragile product which is mulled to obtain Beta-TCP micro-powders. The new method has the characteristics that in-situ oxidation, spontaneous combustion and the rapid synthesis of a product precursor can be implemented at lower temperature. The mixture ratio of reagents is precise, the mixing is even, the reaction velocity is high, the feed stock conversion is high, and the energy consumption is low; the product purity is high, the crystal phase is single, the average particle size is small, the distribution is even, and the hard agglomeration is less.

Description

technical field [0001] The invention belongs to the field of chemistry and biological materials, and relates to a process for preparing β-tricalcium phosphate micropowder by a sol-gel self-propagating combustion method. Background technique [0002] Calcium phosphate, mainly including hydroxyapatite, tricalcium phosphate, etc., is the main inorganic component of human hard tissues (bones, teeth). In recent years, due to the rapid development of bone tissue engineering technology and bionic technology, the research on calcium phosphate-based bioceramics has been continuously deepened. Calcium phosphate-based bioceramics has good biocompatibility, bioactivity and biodegradability, and is non-toxic, so it is considered to be the most promising modern bioceramic. and replacement, etc.) have very attractive prospects for clinical application. [0003] Compared with hydroxyapatite, the content of β-tricalcium phosphate in natural bone is lower, but the solubility of β-tricalcium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32
Inventor 张军宋邦才郭进武卢伟伟姚开胜时清亮李素芹
Owner HENAN UNIV OF SCI & TECH
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