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Preparation method for hydroxylapatite with controllable grain size

A technology of hydroxyapatite and particle size, which is applied in the direction of chemical instruments and methods, phosphorus compounds, nanotechnology for materials and surface science, etc., can solve the problems of large amount of templates used and increased cost of raw materials, and achieve The effect of using less

Active Publication Date: 2018-11-06
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the methods of using templates to synthesize hydroxyapatite, most templates are used in large amounts (An Yan, Yin Yating, Gu Xuemei, et al. Research on the influence of surfactants on the preparation of nano-hydroxyapatite[J]. Inorganic Salt Industry, 2012,44(5):19-21.), leading to an increase in the cost of raw materials and post-processing

Method used

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  • Preparation method for hydroxylapatite with controllable grain size
  • Preparation method for hydroxylapatite with controllable grain size
  • Preparation method for hydroxylapatite with controllable grain size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 9.54g of calcium nitrate tetrahydrate and 3.20g of diammonium hydrogen phosphate in 100ml of deionized water, respectively. Weigh 0g, 0.02g, 0.1g, 0.2g and 0.6g (the numbers of the obtained products correspond to S1, S2, S3, S4 and S5 respectively) and add the hydrolyzed keratin into the calcium nitrate tetrahydrate solution. Under the condition of heating in a water bath at 95°C, slowly add the diammonium hydrogen phosphate solution into the mixed solution of calcium nitrate tetrahydrate and hydrolyzed keratin, while stirring and adding ammonia water to adjust the pH to 8.5. After reacting for 4 hours, heating and stirring were stopped, and the reaction system was allowed to stand and age for 12 hours, the precipitate was washed with water three times, and freeze-dried to obtain hydroxyapatite.

[0029] Figure 1 to Figure 5 The transmission electron micrographs of hydroxyapatite synthesized when the hydrolyzed keratin content (mass / solution volume) are respe...

Embodiment 2

[0033] Dissolve 95.4g of calcium nitrate tetrahydrate and 32.0g of diammonium hydrogen phosphate in 1000ml of deionized water respectively. Weigh 0g, 0.2g, 1g, 2g and 6g (the numbers of the obtained products correspond to S1, S2, S3, S4 and S5 respectively) and add the hydrolyzed keratin into the calcium nitrate tetrahydrate solution. Under the condition of heating in a water bath at 85°C, slowly add the diammonium hydrogen phosphate solution into the mixed solution of calcium nitrate tetrahydrate and hydrolyzed keratin, while stirring and adding ammonia water to adjust the pH to 12.5. After reacting for 5 hours, the heating and stirring were stopped, and the reaction system was left to age for 24 hours, the precipitate was washed 5 times with water, and dried at 110° C. for 5 hours to obtain the product hydroxyapatite.

[0034] Figure 8 It is the Raman characterization diagram of the hydroxyapatite prepared in Example 2. 425 and 580cm -1 The characteristic peaks at can be...

Embodiment 3

[0036] Dissolve 185.37g of calcium chloride and 380.14g of trisodium phosphate dodecahydrate in 1000ml of deionized water, respectively. Weigh 0g, 0.2g, 1g, 2g and 6g (corresponding to S1, S2, S3, S4 and S5 respectively) of hydrolyzed keratin and add it into the calcium nitrate tetrahydrate solution. Under the condition of heating in a water bath at 80°C, slowly add the diammonium hydrogen phosphate solution into the mixed solution of calcium nitrate tetrahydrate and hydrolyzed keratin, while stirring and adding ammonia water to adjust the pH to 11. After reacting for 5 hours, the heating and stirring were stopped, and the reaction system was aged for 24 hours. The precipitate was washed 5 times with water, and dried at 110° C. for 5 hours to obtain the product hydroxyapatite.

[0037] Figure 9 The hydroxyapatite polycrystalline X-ray diffraction characterization spectrum prepared in Example 3 shows that almost all peaks in the figure conform to the standard HA (JCPDS No. 0...

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Abstract

The invention discloses a preparation method for hydroxylapatite with a controllable grain size. The method comprises the following steps of adding hydrolytic keratin into a calcium salt solution firstly, dropwise adding a phosphate solution slowly under a 70-100 DEG C water bath condition to obtain a mixed solution, then adjusting pH value to be 8.5-12.5, stirring to react for 4 h or more, standing and ageing after finishing reaction, washing, and drying to obtain nanoscale hydroxylapatite. The hydrolytic keratin is taken as a template agent, the grain size of synthesized hydroxylapatite is adjusted through adjusting the dosage of the hydrolytic keratin, and the template agent is non-toxic, less in dosage and easy to remove. The hydroxylapatite synthesized by the method is controllable ingrain size and good in biocompatibility and can meet different requirements.

Description

technical field [0001] The technical field of preparation of biomedical materials of the present invention relates to a preparation method of hydroxyapatite, in particular to a preparation method of hydroxyapatite with controllable particle size. Background technique [0002] Hydroxyapatite (hydroxyapatite, HA), the chemical formula is Ca 10 (PO 4 ) 6 (OH) 2 , belonging to the hexagonal crystal system, with a density of 3.14-3.16cm 2 , not only has good stability, bioactivity and biocompatibility, but also has good osteoconduction and the ability to induce bone formation, and is biodegradable. It is an excellent and nearly ideal bone repair and alternative material. Corresponding to the needs of different occasions, hydroxyapatite with different particle sizes and shapes is usually required. [0003] Existing methods for synthesizing hydroxyapatite mainly include precipitation method, hydrothermal method, sol-gel method, ultrasonic synthesis method, microemulsion metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32B82Y30/00
CPCB82Y30/00C01B25/32C01P2002/72C01P2002/01C01P2002/82C01P2004/64
Inventor 朱沛志赵科陈岗高春霞林理伟
Owner YANGZHOU UNIV
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