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Preparation method of hydroxyapatite nano grain

A technology of hydroxyapatite and nanocrystalline particles, which is applied in chemical instruments and methods, pharmaceutical formulations, phosphorus compounds, etc., can solve the problems that cannot meet the requirements of human tooth enamel tissue size and structure, small order range of materials, and limited size and structure. Gap and other issues

Inactive Publication Date: 2012-05-23
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this type of method, the range of order degree of the obtained material is small, and there is also a gap between the size structure of the material and the size structure of human tissue, which cannot meet the size and structure of human tooth enamel tissue.

Method used

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  • Preparation method of hydroxyapatite nano grain
  • Preparation method of hydroxyapatite nano grain
  • Preparation method of hydroxyapatite nano grain

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add calcium nitrate (0.3mol / L), calcium chloride (0.2mol / L), disodium hydrogen phosphate (0.3mol / L), collagen (20g / L), and a mixed solvent of ethanol and water ( 2:1), adding sodium hydroxide solution to adjust the pH to 11, and reacting at a constant temperature in a water bath, the reaction temperature is 60° C., and the reaction time is 5 hours.

[0028] (2) Take out the reacted mixed solution and transfer it to a sealed stainless steel reaction kettle lined with polytetrafluoroethylene to synthesize through hydrothermal reaction.

[0029] (3) The intermediate product was washed three times with water, filtered, and freeze-dried to obtain the final product.

[0030] The resulting product was characterized by XRD and SEM tests figure 1 and figure 2 .

[0031] figure 1 It is the XRD spectrum of the hydroxyapatite nanocrystals obtained in Example 1. It can be seen that it has a typical peak shape of hydroxyapatite, and is a hydroxyapatite nanocrystal; figure ...

Embodiment 2

[0033] (1) Calcium nitrate (1mol / L), dipotassium hydrogen phosphate (0.4mol / L), disodium hydrogen phosphate (0.2mol / L), gelatin (40g / L), add ethanol and water mixed solvent (1 : 2), adding sodium hydroxide solution to adjust the pH=11, and reacting at a constant temperature in a water bath, the reaction temperature is 40° C., and the reaction time is 3 hours.

[0034] (2) Take out the reacted mixed solution and transfer it to a sealed stainless steel reaction kettle lined with polytetrafluoroethylene to synthesize by hydrothermal reaction. The hydrothermal reaction temperature is 160° C., keep warm for 48 hours, and take out the intermediate product.

[0035] (3) The intermediate product was washed three times with water, filtered, and freeze-dried to obtain the final product.

[0036] After testing, the obtained product is hydroxyapatite nano crystal grains, which are in the bundle structure formed by rod-shaped nano crystals arranged in parallel, similar to the tooth prism str...

Embodiment 3

[0038] (1) Calcium nitrate (0.1mol / L), dipotassium hydrogen phosphate (0.04mol / L), disodium hydrogen phosphate (0.02mol / L), gelatin (5g / L), and a mixed solvent of ethanol and water ( 1:4), adding sodium hydroxide solution to adjust the pH=10, and reacting at a constant temperature in a water bath, the reaction temperature is 20° C., and the reaction time is 24 hours.

[0039] (2) Take out the reacted mixed solution and transfer it to a sealed stainless steel reactor lined with polytetrafluoroethylene inside to synthesize by hydrothermal reaction. The hydrothermal reaction temperature is 100° C., keep it warm for 100 hours, and take out the intermediate product.

[0040] (3) The intermediate product was washed three times with water, filtered, and freeze-dried to obtain the final product.

[0041] After testing, the obtained product is hydroxyapatite nano crystal grains, which are in the bundle structure formed by rod-shaped nano crystals arranged in parallel, similar to the to...

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Abstract

The invention relates to a preparation method capable of regulating and controlling uniform size and ordered arrangement of a hydroxyapatite nano grain, belonging to the field of biological materials. The preparation method comprises the steps of: adding a calcium source, a phosphorus source and a fat-free protein colloid into a mixed solvent of an organic solvent and water, regulating pH of a solution to be 10-14 by using a pH regulating agent, carrying out water bath constant-temperature reaction to obtain a mixes solution; and then transferring to a sealed stainless steel agitated reactor internally lined with polytetrafluoroethylene to obtain an intermediate product through a hydro-thermal reaction, and finally, washing with water, freezing and drying to obtain a final product. The method can be used for preparing a hydroxyapatite nano rod structure with the characteristics of uniform size and appearance and a certain parallel arrangement. The hydroxyapatite nano grain can be widely applied to biological materials such as a dental material, a bone substitution material, a biological agent and the like.

Description

technical field [0001] The invention belongs to the field of biological materials, and relates to a preparation method capable of regulating the uniform size and orderly arrangement of hydroxyapatite nanocrystal grains. Background technique [0002] Dental tissue is the hardest tissue in the human body. Tooth decay, trauma, disease, etc. will cause damage or damage to tooth tissue, and artificial dental materials are required for repair. Dental material is an important biological material, which plays an important role in clinical application. With the growth and aging of the population, the demand for human tooth replacement materials is increasing year by year. my country is a populous country, and the annual demand for dental materials is very large. [0003] Hydroxyapatite is an important dental biomaterial, which has good biocompatibility and bioactivity, as well as reliable mechanical properties, and widely exists in the structure of human bones and teeth. More tha...

Claims

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Application Information

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IPC IPC(8): C01B25/32A61L27/12A61L27/50A61K6/033A61K6/838
Inventor 张郡凌江东亮张景贤林庆玲黄政仁
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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