Hydroxyapatite crystal whisker with high length-diameter ratio and preparation method thereof

A technology of hydroxyapatite and high aspect ratio, which is applied in the field of chemical and biological materials, can solve the problems of impure crystal phase, small whisker aspect ratio, and target product variation, and achieve improved mechanical properties and good biological properties. The effect of activity and mild reaction conditions

Inactive Publication Date: 2008-03-26
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the research on the preparation of HA whiskers by the hydrothermal method has made great progress, it is not perfect, and there are still many problems to be further systematically studied, such as the concentration and phase of raw materials (nutrients), heating rate, and stirring conditions. , reaction temperature, pressure (filling degree), hydrothermal time, PH value and appropriate selection of additives and other physical and chemical conditions can affect the reaction results to varying degrees, and even cause a large change in the target product
In addition, due to the high pressure and airtight characteristics of the hydrothermal reaction system, timely observation and monitoring of phase composition and morphology changes are still difficult to accurately grasp and implement.
In short, the above methods all have defects such as small HA whisker aspect ratio, impure crystal phase and low product conversion rate, which need to be further improved and improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a. In a nitrogen protective atmosphere, dissolve analytically pure Ca(NO 3 ) 2 4H 2 O and (NH 4 ) 2 HPO 4 , respectively prepare 0.1mol·l -1 of aqueous solution.

[0025] b. In a reactor with a volume of 250ml and a reflux device, fill it with atmospheric nitrogen to form a protective atmosphere, and add 0.1mol·l -1 Ca(NO 3 ) 2Solution 92ml, then add 0.75g additives, stir magnetically to dissolve and mix evenly.

[0026] c. Set the concentration of 58ml to 0.1mol·l -1 of (NH 4 ) 2 HPO 4 The solution is added dropwise to the reaction solution obtained in the above step b, and the two solutions are fully mixed with continuous stirring.

[0027] d. Use 0.5mol·l -1 HNO 3 Adjust the pH of the reaction mixture in step c to 2.5.

[0028] e. Raise the temperature of the reaction mixture to 75° C., and reflux at this temperature for 3.5 hours.

[0029] This step contributes to the intermediate CaHPO 4 Conversion to HA, ie: Ca 2+ +HPO 4 2- →CaHPO 4 ; CaHPO ...

Embodiment 2

[0034] a. In a nitrogen protective atmosphere, dissolve analytically pure Ca(NO 3 ) 2 4H 2 O and (NH 4 ) 2 HPO 4 Prepare 0.5mol·l respectively -1 of aqueous solution.

[0035] b. In a reactor with a volume of 250ml and a reflux device, fill it with atmospheric nitrogen to form a protective atmosphere, and add 0.5mol l -1 Ca(NO 3 ) 2 Solution 126ml, then add 2.4g additives, stir magnetically to dissolve and mix evenly.

[0036] c. Set the concentration of 74ml to 0.5mol·l -1 of (NH 4 ) 2 HPO 4 The solution is added dropwise to the reaction solution obtained in the above step b, and the two solutions are fully mixed with continuous stirring.

[0037] d. Use 0.5mol·l -1 HNO 3 Adjust the pH of the reaction mixture in step c to 4.5.

[0038] e. Raise the temperature of the reaction mixture to 100° C., and reflux at this temperature for 4.5 hours. This step contributes to the intermediate CaHPO 4 Conversion to HA, ie: Ca 2+ +HPO 4 2- →CaHPO 4 ; CaHPO 4 +H 2 O...

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Abstract

The process of preparing hydroxyapatite crystal whisker in great length/diameter ratio includes mixing calcium source solution and phosphorus source solution in proper concentration under the protection of nitrogen while adding assistant for crystal to grow in certain direction, reflux reaction at proper acidity and temperature conditions for certain time, and transferring the reflux resultant to a pressure kettle for static hydrothermal growth to obtain hydroxyapatite crystal whisker in great length/diameter ratio and high purity. The process has the advantages of mild conditions, short preparation period, controllable length/diameter ratio and high product purity. In addition, the product has high bioactivity.

Description

technical field [0001] The invention relates to a hydroxyapatite whisker and a preparation technology thereof, belonging to the field of chemical and biological materials. Background technique [0002] Hydroxyapatite, chemical formula Ca 10 (PO 4 ) 6 (OH) 2 HA, referred to as HA, is the main inorganic component that constitutes the hard tissues (bones, teeth) of organisms. In bone tissue, HA exists in the form of needles and rod-shaped whiskers, and is skillfully combined with biological organic tissues such as collagen to form a HA / biopolymer composite material. Porous and interconnected HA microcrystals have different degrees of bioactivity, biocompatibility and biodegradability, have no toxic side effects and rejection, and can produce good osteoinductivity with organisms. Therefore, in recent years, HA It has rapidly developed into one of the widely used bone substitute materials, and has shown more and more broad application prospects in biotissue engineering scaff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/10C30B29/62C30B7/10
Inventor 张军宋邦才郭进武卢伟伟柴元武胡瑞华
Owner HENAN UNIV OF SCI & TECH
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