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Preparation method of flower-shaped hydroxyapatite whisker

A hydroxyapatite and whisker technology, which is applied in the field of preparation of flower-like hydroxyapatite whiskers, can solve the problem of optimal parameters of reaction system pressure, product crystallinity and shape uniformity without description of reactor filling degree Not high, no mention of calcium source and other issues, achieving the effect of strong repeatability, short preparation cycle and uniform shape

Active Publication Date: 2015-12-16
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

People such as Sun Kangning (Chinese patent, publication number CN102431986A) have invented a kind of preparation method of hydroxyapatite nanofiber, and this method is to utilize homogeneous precipitation method to produce HAp nanofiber, and its diameter is about 20 ～30 nm, the length is about 200 ～ 900nm, the aspect ratio is basically controllable, and there are no other impurity phases, but the whole process needs to add the template agent cetyltrimethylammonium bromide (CTAB), and the crystallinity and shape uniformity of the product are not high, which can be repeated Poor sex
The hydrothermal method is currently the most common and mature method for preparing hydroxyapatite whiskers. Zhang Jizhong (Chinese patent, publication number CN101297978A) invented a method for preparing hydroxyapatite nanorods. Under the oleic acid-ethanol-water phase transfer system, the prepared HAp powder has uniform size, controllable shape, and low production cost, but there are many kinds of drugs required, and the filling degree of the reaction kettle when hydrothermal is not described in the article and the optimal parameters of reaction system pressure
Zhang Meijuan (Chinese Patent, Publication No. CN101723341A) invented a method for preparing hydroxyapatite nanofibers or nanowires. The prepared hydroxyapatite nanowires have high purity, uniform particle size, and single appearance, but in the examples The introduction of calcium source is not mentioned, and the yield is not high

Method used

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  • Preparation method of flower-shaped hydroxyapatite whisker
  • Preparation method of flower-shaped hydroxyapatite whisker

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Step 1: Weigh 0.8g of light calcium carbonate with an electronic balance, measure 1.7ml of 85.0wt.% concentrated phosphoric acid with a pipette gun, and dilute to 10ml, so that the mass ratio of phosphoric acid to calcium carbonate is 3.2:1;

[0016] Step 2: Use ammonia water to adjust the pH value of the concentrated phosphoric acid diluted in step 1 to 9, place the light calcium carbonate in step 1 in the phosphoric acid solution that has adjusted the pH value, and place the phosphoric acid solution on a magnetic stirrer , stirred at room temperature for 15 minutes to obtain the precursor;

[0017] Step 3: Place the precursor obtained in Step 2 in a hydrothermal reaction kettle, and react at 180°C for 10 hours. After the hydrothermal reaction is completed, cool it down to room temperature naturally, take out the obtained product, and wash it with water three times, alcohol three times in sequence. Wash, centrifuge to remove reaction residues and impurities, and put th...

Embodiment 2

[0021] Step 1: Weigh 0.7g of light calcium carbonate with an electronic balance, measure 1.5ml of 85.0wt.% concentrated phosphoric acid with a pipette gun, and dilute to 10ml, so that the mass ratio of phosphoric acid to calcium carbonate is 3.2:1;

[0022] Step 2: Use ammonia water to adjust the pH value of the concentrated phosphoric acid diluted in step 1 to 7, place the light calcium carbonate in step 1 in the phosphoric acid solution that has adjusted the pH value, and place the phosphoric acid solution on a magnetic stirrer , stirred at room temperature for 20 minutes to obtain the precursor;

[0023] Step 3: Place the precursor obtained in Step 2 in a hydrothermal reaction kettle, and react at 160°C for 10 hours. After the hydrothermal reaction is completed, cool down to room temperature naturally, take out the obtained product, and wash with water three times, alcohol three times in sequence. Wash, centrifuge to remove reaction residues and impurities, and put the obta...

Embodiment 3

[0025] Step 1: Weigh 0.6g of light calcium carbonate with an electronic balance, measure 1.3ml of 85.0wt.% concentrated phosphoric acid with a pipette gun, and dilute to 10ml, so that the mass ratio of phosphoric acid to calcium carbonate is 3.2:1;

[0026] Step 2: Use ammonia water to adjust the pH value of the concentrated phosphoric acid diluted in step 1 to 8, place the light calcium carbonate in step 1 in the phosphoric acid solution that has adjusted the pH value, and place the phosphoric acid solution on a magnetic stirrer , stirred at room temperature for 10 minutes to obtain the precursor;

[0027] Step 3: Place the precursor obtained in Step 2 in a hydrothermal reaction kettle and react at 200°C for 10 hours. After the hydrothermal reaction is completed, cool it down to room temperature naturally, take out the obtained product, and perform three times of washing with water and three times of alcohol in sequence. Wash, centrifuge to remove reaction residues and impuri...

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Abstract

The invention provides a preparation method of flower-shaped hydroxyapatite whisker. Calcium carbonate and phosphoric acid are taken as raw materials, the mass ratio of phosphoric acid to calcium carbonate is controlled to be larger than 3:1, light calcium carbonate is put in a phosphoric acid solution with an adjusted pH (potential of hydrogen) value, the mixture is stirred, a precursor is obtained, put in a hydrothermal reaction kettle to have a hydrothermal reaction and cooled to the room temperature after the reaction, a product is taken out, sequentially washed with water for three times, washed with alcohol for three times and then subjected to centrifugal separation, reaction residues and impurities are removed, the obtained product is put in a constant-temperature drying box to be dried, and then the flower-shaped hydroxyapatite whisker can be obtained. The length-diameter ratio of the prepared flower-shaped hydroxyapatite whisker is controllable, the morphology is uniform, the fracture toughness is remarkably improved, and the flower-shaped hydroxyapatite whisker has the characteristics of low cost, high yield, simple process and high repeatable operability.

Description

technical field [0001] The invention relates to the technical field of preparation of bioceramic materials, in particular to a method for preparing flower-shaped hydroxyapatite whiskers. Background technique [0002] Hydroxyapatite (HAp) has excellent biocompatibility and bioactivity, and its osteoinductive activity is more prominent. As a special form of hydroxyapatite whiskers, it not only retains excellent biological properties, And it has higher tensile properties and lower dislocation density. As fibers grown in the form of single crystals, HAp whiskers are stronger and tougher than ordinary hydroxyapatite ceramics by about 3～8 It can be used as a reinforcement or filler for hard tissue repair ceramic materials. HAp whiskers absorb energy in bioceramics through deflection effect, bridging effect, pull-out effect and micro-crack effect, and eliminate the concentrated stress at the tip of the crack, which can greatly improve the toughness of the material. Based on its m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B29/62C30B29/14
Inventor 刘毅张彪张利锋郑鹏原晓艳郭守武
Owner SHAANXI UNIV OF SCI & TECH