Method for preparing oil-soluble hydroxyapatite nanorod through one-step method

A hydroxyapatite, oil-soluble technology, applied in the field of one-step preparation of oil-soluble hydroxyapatite nanorods, can solve the problem of nanocrystal crystallinity, shape, size deficiency, material application can not be fully realized, oil phase dispersion effect Unsatisfactory and other problems, to achieve the effect of good shape controllability, good dispersion and stable product quality

Inactive Publication Date: 2019-03-22
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The nanocrystals obtained by the method of synthesizing oil-soluble hydroxyapatite are deficient in crystallinity, morphology, size, etc., which makes it impossible to fully realize its application in materials;
[0006] 2. The solubility of sodium phosphate is low, the dissolution is slow, and the strong alkalinity leads to a long synthesis process, and the product has a uniform appearance;
[0007] 3. Most of the synthesis methods have unsatisfactory dispersion effects in the oil phase

Method used

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  • Method for preparing oil-soluble hydroxyapatite nanorod through one-step method
  • Method for preparing oil-soluble hydroxyapatite nanorod through one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Dissolve 0.02mol calcium nitrate in 20 grams of water to obtain solution A;

[0036] 2) Dissolve 0.032 mol of ethylenediamine in a mixture of 40 g of ethanol and 0.04 mol of oleic acid to obtain solution B;

[0037] 3) Add solution B obtained in step 2) into a three-necked flask, then slowly drop solution A obtained in step 1) into solution B, and stir for 10 minutes to obtain solution C;

[0038] The mol ratio of described oleic acid and calcium is 2:1;

[0039] The molar ratio of oleic acid to ethylenediamine is 5:4.

[0040] 4) 0.012mol trisodium phosphate was dissolved in 30 grams of water to obtain solution D;

[0041] 5) Under stirring conditions, slowly drop the solution D obtained in step 4) into the solution C obtained in step 3), and continue stirring for 20 minutes after the dropwise addition to obtain a suspension;

[0042] 6) slowly drop 0.012mol sodium hydroxide solution into the suspension, and stir for 10 minutes to obtain a mixed solution;

[004...

Embodiment 2

[0047] Embodiment 2, with embodiment 1, difference is,

[0048] 1) Dissolve 0.02mol calcium nitrate in 20 grams of water to obtain solution A;

[0049] 2) Dissolve 0.016 mol of ethylenediamine in a mixture of 40 g of ethanol and 0.02 mol of oleic acid to obtain solution B;

[0050] 3) Add solution B obtained in step 2) into a three-necked flask, then slowly drop solution A obtained in step 1) into solution B, and stir for 10 minutes to obtain solution C;

[0051] The mol ratio of described oleic acid and calcium is 1:1;

[0052] The molar ratio of oleic acid to ethylenediamine is 5:4.

[0053] 4) 0.012mol trisodium phosphate was dissolved in 30 grams of water to obtain solution D;

[0054]6) slowly drop 0.008mol sodium hydroxide solution into the suspension obtained in step 5), and stir for 10 minutes to obtain a mixed solution;

[0055] 7) Put the mixed solution obtained in step 6) in a high-temperature and high-pressure reactor, heat it with water at 180° C. for 3 hours,...

Embodiment 3

[0056] Embodiment 3, with embodiment 1, difference is,

[0057] 1) Dissolve 0.02mol calcium chloride in 20 grams of water to obtain solution A;

[0058] 2) Dissolve 0.016mol of sodium hydroxide in a mixed solution of 40 grams of ethanol and 0.02mol of oleic acid to obtain solution B;

[0059] 3) Add solution B obtained in step 2) into a three-necked flask, then slowly drop solution A obtained in step 1) into solution B, and stir for 10 minutes to obtain solution C;

[0060] The mol ratio of described oleic acid and calcium is 1:1;

[0061] The mol ratio of described oleic acid and sodium hydroxide is 5:4.

[0062] 4) Dissolve 0.012mol sodium dihydrogen phosphate in 30 grams of water to obtain solution D;

[0063] 6) slowly drop 0.008mol potassium hydroxide solution into the suspension obtained in step 5), and stir for 10 minutes to obtain a mixed solution;

[0064] 7) Put the mixed solution obtained in step 6) in a high-temperature and high-pressure reactor, heat it under ...

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Abstract

The invention relates to a method for preparing an oil-soluble hydroxyapatite nanorod through one-step method. The preparation method comprises the following steps: dissolving soluble calcium salt inthe water to obtain a solution A; dissolving soluble alkali in the mixed solution of ethanol and oleic acid to obtain a solution B; dropwise adding the solution B in a three-necked flask, and slowly dropwise adding the solution A under a stirring condition to obtain a solution C; dissolving the soluble phosphate in water to obtain a solution D, dropwise adding the solution D in the solution C, andstirring to obtain suspension liquid; dropwise adding the soluble alkali in the suspension liquid to obtain the mixed solution; reacting the mixed solution in a high-temperature and high-pressure reaction still at 80-180 DEG C, and cooling to room temperature to obtain a reaction solution; and centrifugally separating the reaction solution to obtain precipitate, and alternatively and centrifugally washing with absolute ethyl alcohol and cyclohexane to obtain oil-soluble hydroxyapatite nanorod. The raw material resource is rich and easy to obtain, the cost is low, the synthesis process is simple, and the process repeatability is high; the product is stable in quality and high in morphology controllability, and high in dispersion; and the method can be extensively used for the biomedical materials and the coating material and like fields.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic nanomaterials, in particular to a method for preparing oil-soluble hydroxyapatite nanorods in one step Background technique [0002] Hydroxyapatite, referred to as HA, the chemical formula is Ca 10 (PO 4 ) 6 (OH) 2 , its nanocrystals are hexagonal, and its structure is a hexagonal column. Hydroxyapatite has a similar chemical composition to natural bone, has excellent biological properties, and the crystal has strong ion substitution, so it is widely used in bone replacement or repair, drug carrier, fluorescent labeling, etc. The preparation of hydroxyapatite with good crystallinity, high aspect ratio, good dispersion and stability has always been the goal pursued by people. [0003] At present, the method of synthesizing oil-soluble hydroxyapatite nanorods has been extensively studied. CN106835847A discloses a preparation method of biocompatible carbon nanotube / hydroxyapatite compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32B82Y40/00
CPCB82Y40/00C01B25/325C01P2002/72C01P2004/04C01P2004/16
Inventor 谭军军刘洋龚静张荣
Owner HUBEI UNIV OF TECH
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