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Two-step oil-solute hydroxyapatite nanorod preparing method

A hydroxyapatite, oil-soluble technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of nanocrystal crystallinity, morphology, size deficiency, material application cannot be realized, low solubility of sodium phosphate, etc. problems, to achieve the effects of good morphology controllability, low cost, and stable product quality

Active Publication Date: 2019-04-05
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 most methods of synthesizing oil-soluble hydroxyapatite are deficient in crystallinity, morphology, size, etc., which makes it impossible to realize the material application;
[0006] 2. The solubility of sodium phosphate is low, the dissolution is slow, and the alkalinity is too strong, resulting in a long time-consuming synthesis process and uniform product appearance;
[0007] 3. Most of them require hydrothermal treatment, but relative to the production rate, the hydrothermal efficiency is too low and the energy consumption is large

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

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

[0036] 2) Dissolve 0.032mol ethylenediamine in a mixture of 40g ethanol and 0.04mol 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) Dissolve 0.012mol of trisodium phosphate in 30g 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) Centrifuge or filter the suspension obtained in step 5) to obtain a precipitate, redisperse the precipitate in 100 g of deionized water, and adjust the pH...

Embodiment 2

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

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

[0049] 2) Dissolve 0.032mol ethylenediamine in a mixture of 40g ethanol and 0.02mol 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) Dissolve 0.012mol of trisodium phosphate in 30g of water to obtain solution D;

[0054]6) Centrifuge or filter the suspension obtained in step 5) to obtain a precipitate, redisperse the precipitate in 100 g of deionized water, and adjust the pH to 10.5 with 1 mol / L sodium hydroxide to obtain a reaction solution 1;

[0055] 7) The reaction solution 1 obtained in step 6) was placed in a high-temperatur...

Embodiment 3

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

[0057] 1) Dissolve 0.02mol calcium nitrate in 20g water to obtain solution A;

[0058] 2) Dissolve 0.032mol sodium hydroxide in a mixed solution of 40g ethanol and 0.04mol 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 molar ratio of oleic acid to ethylenediamine is 5:4.

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

[0063] 6) Centrifuge or filter the suspension obtained in step 5) to obtain a precipitate, redisperse the precipitate in 100 g of deionized water, adjust the pH to 7 with 1 mol / L sodium hydroxide, and obtain a reaction solution 1;

[0064] 7) The reaction solution 1 obtained in step 6) was placed in a h...

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Abstract

The invention relates to a two-step oil-solute hydroxyapatite nanorod preparing method. The method comprises dissolving a soluble calcium salt into water to obtain a solution A; dissolving a soluble alkali into an ethyl alcohol and oleic acid mixed solution to obtain a solution B; filling the solution B into a three-neck flask, then slowly dropwise stirring in the solution A to obtain a solution C; dissolving a soluble phosphate into water to obtain a solution D; dropwise stirring the solution D into the solution C to obtain a suspension; centrifuging or suction-filtering the suspension to obtain precipitates, dispersing the precipitates into deionized water to obtain a reaction liquid I; subjecting the reaction liquid I to reaction in a high-temperature reactor, and then cooling down to room temperature to obtain a reaction liquid II; performing centrifugal separation on the reaction liquid II to obtain precipitates, and alternately centrifugally washing the precipitates with absoluteethyl alcohol and cyclohexane to obtain oil-soluble hydroxyapatite nanorods. The two-step oil-solute hydroxyapatite nanorod preparing method is rich and simple in raw material acquisition, low in cost, simple in synthesizing process and good in process repeatability; the produced oil-solute hydroxyapatite nanorods are good in morphological controllability and dispersibility and can be widely applied to the fields such as biomedical materials and coating materials.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic nanometer materials, in particular to a method for preparing oil-soluble hydroxyapatite nanorods based on a two-step method. Background technique [0002] As an important part of mammalian bones and teeth, hydroxyapatite nanocrystals exhibit excellent mechanical properties to maintain their survival needs. In addition, hydroxyapatite also has important applications in bone replacement or repair, drug carrier, fluorescent labeling, etc. In order to give full play to the composition and biological characteristics of hydroxyapatite in biological applications, it is often required that the prepared hydroxyapatite nanorods have good crystallinity, suitable size, good stability and dispersibility. So people have been looking for different ways to prepare hydroxyapatite nanorods. [0003] At present, the method of synthesizing oil-soluble hydroxyapatite nanorods has been extensively studied. ...

Claims

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Application Information

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IPC IPC(8): C01B25/32B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B25/32C01P2004/04C01P2002/72C01P2004/64
Inventor 谭军军刘洋龚静张荣
Owner HUBEI UNIV OF TECH
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