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Oil-soluble hydroxyapatite nano-sheet preparation method

A technology of hydroxyapatite and nanosheets, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., and can solve the problem that the crystallinity, shape, and uniformity of hydroxyapatite nanocrystals cannot be optimized. In order to achieve the effects of easy implementation, good shape controllability and good dispersibility, etc.

Inactive Publication Date: 2016-02-03
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The first major defect is that hydroxyapatite flake nanocrystals prepared by general synthesis methods cannot achieve optimal combination in terms of crystallinity, morphology, uniformity, and nanometer size, which is not conducive to giving full play to the advantages of this type of material
The second major defect is that the prepared flaky hydroxyapatite nanoparticles often exist in the oil phase or monomer solution in the form of large aggregates, rather than forming a complete dispersion state, which causes serious problems for subsequent material preparation. A large number of defects affect the improvement of material performance
The third major defect is that in order to obtain sufficient lipophilicity on the particle surface, surface modifiers are often added, but the biocompatibility of surface modifiers is often difficult to meet subsequent applications, and the modifiers adsorbed on the particle surface cannot Form a strong covalent bond with polymer molecules, and the interface bond strength is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Add 24 mL of 2.08 mol / L calcium nitrate aqueous solution and 48 mL of ethanol, 0.0125 mol oleic acid and 0.0125 mol ethylenediamine into a three-necked flask and mix, and stir to obtain a uniform solution; the molar ratio of soluble calcium salt and soluble phosphate is 5: 3. Under stirring conditions, slowly add 24 mL of triammonium phosphate aqueous solution into the above solution dropwise, and continue stirring for 10 minutes after the addition is completed;

[0036] 2) heating the mixed liquid obtained in step 1) to 80° C. for 6 hours, and then naturally cooling to room temperature to obtain a reaction liquid;

[0037] 3) Use a high-speed centrifuge to centrifuge the reaction solution obtained in step 2) to obtain a precipitate, and use absolute ethanol and cyclohexane to alternately centrifuge and wash 3 times to remove electrolytes and excess fatty acids in the system to obtain oil-soluble hydroxyapatite nanosheets .

[0038] The X-ray diffraction pattern of ...

Embodiment 2

[0040] 1) Add 24 mL of 2.08 mol / L calcium nitrate aqueous solution and 48 mL of ethanol, 0.025 mol of oleic acid and 0.025 mol of ethylenediamine into a three-necked flask and mix, and stir to obtain a uniform solution; the molar ratio of soluble calcium salt and soluble phosphate is 5: 3. Under stirring conditions, slowly add 24 mL of diammonium hydrogen phosphate aqueous solution to the above solution dropwise, and continue stirring for 10 minutes after the addition is completed;

[0041] 2) heating the mixed liquid obtained in step 1) to 80° C. for 3 hours and then cooling it to room temperature naturally to obtain a reaction liquid;

[0042] 3) Use a high-speed centrifuge to centrifuge the reaction solution obtained in step 2) to obtain a precipitate, and use absolute ethanol and cyclohexane to alternately centrifuge and wash 3 times to remove electrolytes and excess fatty acids in the system to obtain oil-soluble hydroxyapatite nanosheets .

[0043] The X-ray diffraction...

Embodiment 3

[0045] 1) Add 24 mL of 2.08 mol / L calcium chloride aqueous solution, 24 mL of propanol and 24 mL of ethanol, 0.0375 mol of oleic acid and 0.0375 mol of ethylenediamine into a three-necked flask and mix, and stir to obtain a uniform solution; soluble calcium salt and soluble phosphate The molar ratio is 5:3. Under stirring conditions, 24 mL of ammonium dihydrogen phosphate aqueous solution is slowly added dropwise to the above solution, and the stirring is continued for 10 minutes after the addition is completed;

[0046] 2) heating the mixed solution obtained in step 1) to 80° C. for 12 hours, and then naturally cooling to room temperature to obtain a reaction solution;

[0047] 3) Use a high-speed centrifuge to centrifuge the reaction solution obtained in step 2) to obtain a precipitate, and use absolute ethanol and cyclohexane to alternately centrifuge and wash 3 times to remove electrolytes and excess fatty acids in the system to obtain oil-soluble hydroxyapatite nanosheets ...

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Abstract

The invention relates to an oil-soluble hydroxyapatite nano-sheet preparation method, which comprises: adding 24 mL of a 2.08 mol / L soluble calcium salt aqueous solution, 48 mL of low-carbon alcohol, 0.0125-0.1 mol of fatty acid and 0.0125-0.2 mol of an organic amine to a three-necked flask, mixing, and stirring to obtain a uniform solution; under a stirring condition, slowly adding 24 mL of a soluble phosphate aqueous solution to the obtained solution in a dropwise manner, and continuously stirring for 10 min after completing the stirring; and heating to a temperature of 50-90 DEG C, carrying out a reaction for 3-24 h, naturally cooling to a room temperature, carrying out centrifugation separation by using a high-speed centrifuge to obtain a precipitate, carrying out alternating centrifugation washing three times with absolute alcohol and cyclohexane, and removing electrolytes and excess fatty acids from the system so as to obtain the oil-soluble hydroxyapatite nano-sheets. According to the present invention, the method has characteristics of rich and easily-available raw materials, low cost, simple synthesis process and easy performing, and the product has characteristics of stable quality, good process repeatability, good shape controllability, and good dispersion property.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic lyotropic liquid crystals, in particular to a preparation method of oil-soluble hydroxyapatite nanosheets. Background technique [0002] Hydroxyapatite is the main inorganic component of human bones and teeth. It has excellent biological activity and biocompatibility, and the crystal has strong ion substitution, so it has great potential in the fields of biological materials, environmental treatment and optical functional materials. Wide range of applications. Flake hydroxyapatite nanoparticles are the main form of hydroxyapatite in bone, and are also the most ideal basic unit for preparing bone repair and bone replacement polymer-based nanocomposites. Although the current method of synthesizing hydroxyapatite nanoparticles has been deeply researched and expanded, there are still three significant problems. [0003] The first major defect is that hydroxyapatite flake nanocrystals prepar...

Claims

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Application Information

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IPC IPC(8): C01B25/32B82Y30/00
Inventor 谭军军金小影胡兵
Owner HUBEI UNIV OF TECH
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