Method for preparing oil-soluble hydroxyapatite nanometer particles based on nonaqueous system

A technology of hydroxyapatite and nanoparticles, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, and can solve the crystallinity, morphology, and uniformity of hydroxyapatite flake nanocrystals Nano size cannot achieve optimization, surface modifiers are difficult to biocompatibility, modifiers cannot be covalently bonded, etc., to achieve good shape controllability, good dispersion, and stable product quality

Active Publication Date: 2018-03-02
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The flaky hydroxyapatite 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
[0006] (2) 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 a large number of defects for subsequent material preparation and affects the quality of materials. performance improvement
[0007] (3) Generally, in order to obtain sufficient lipophilicity on the surface of particles, surface modifiers are often added, but the biocompatibility of surface modifiers is often difficult to meet subsequent applications, and the modifiers adsorbed on the surface of particles cannot interact with polymers. Molecules form a strong covalent bond, and the interface bond strength is not ideal
[0008] (4) The common water-alcohol mixed solvent synthesis system either requires high pressure and high temperature conditions, or requires a long synthesis time to complete the crystallization at a relatively low temperature (the time is calculated in days), which have caused great harm to its industrialization and commercialization. big obstacle

Method used

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  • Method for preparing oil-soluble hydroxyapatite nanometer particles based on nonaqueous system
  • Method for preparing oil-soluble hydroxyapatite nanometer particles based on nonaqueous system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0036] 2) Dissolve 0.005 mol of potassium hydroxide in 20 grams of ethylene glycol to obtain solution B;

[0037] 3) Add solution A obtained in step 1), 20 grams of propylene glycol, 0.01 mol oleic acid and solution B obtained in step 2) into a three-necked flask for mixing, and stir to obtain solution C;

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

[0039] The molar ratio of described oleic acid and potassium hydroxide is 2.

[0040] 4) Dissolve 0.012 mol of disodium hydrogen phosphate in 20 grams of ethylene glycol 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 10 minutes after the dropwise addition to obtain a mixed solution;

[0042] The mol ratio of described calcium nitrate and disodium hydrogen phosphate is 5:3;

...

Embodiment 2

[0045] Embodiment 2, with embodiment 1, difference is,

[0046] 1) Dissolve 0.02mol calcium nitrate in 20 grams of ethylene glycol to obtain solution A;

[0047] 2) Dissolve 0.01mol of sodium hydroxide in 20 grams of ethylene glycol to obtain solution B;

[0048] 3) Add solution A obtained in step 1), 30 grams of propylene glycol, 0.01 mol oleic acid and solution B obtained in step 2) into a three-necked flask for mixing, and stir to obtain solution C;

[0049] The mol ratio of described oleic acid and calcium nitrate is 1 / 2;

[0050] The molar ratio of described oleic acid and sodium hydroxide is 1.

[0051] 4) Dissolve 0.012 mol of dipotassium hydrogen phosphate in 20 grams of ethylene glycol to obtain solution D;

[0052] 6) The mixed solution obtained in step 5) was heated to 120° C. for 12 hours of reaction, and then naturally cooled to room temperature to obtain a reaction solution.

Embodiment 3

[0053] Embodiment 3, with embodiment 1, difference is,

[0054]1) Dissolve 0.02mol calcium nitrate in 20 grams of ethylene glycol to obtain solution A,

[0055] 2) 0.013mol ethylenediamine was dissolved in 20 grams of ethylene glycol to obtain solution B,

[0056] 3) Add solution A obtained in step 1), 40 grams of propylene glycol, 0.018mol oleic acid and solution B obtained in step 2) into a three-necked flask for mixing, and stir to obtain solution C;

[0057] The mol ratio of described oleic acid and calcium nitrate is 9 / 10;

[0058] The molar ratio of oleic acid and ethylenediamine is 18 / 13.

[0059] 4) Dissolve 0.012 mol of trisodium phosphate in 20 grams of ethylene glycol to obtain solution D;

[0060] 6) The mixed solution obtained in step 5) was heated to 150° C. for 3 hours to react, and then naturally cooled to room temperature to obtain a reaction solution.

[0061] The X-ray diffraction figure of the oil-soluble hydroxyapatite nanocrystal obtained in the above...

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Abstract

The invention relates to a method for preparing oil-soluble hydroxyapatite nanometer particles based on a nonaqueous system. Soluble calcium salts are dissolved into glycol to obtain a solution A; soluble alkali is dissolved into glycol to obtain a solution B; the solution A, propylene glycol or propanol, fatty acid and the solution B are added into a three-opening flask to be mixed and stirred; asolution C is obtained; soluble phosphate is dissolved into glycol to obtain a solution D; the solution D is dripped into the solution C; stirring is performed to obtain a mixed solution; the temperature of the mixed solution is raised to 80 to 160 DEG C; reaction is performed for 3 to 24 hours; cooling is performed to reach room temperature to obtain reaction liquid; the reaction liquid is subjected to centrifugal separation to obtain precipitates; absolute ethyl alcohol and cyclohexane are used for alternate centrifugal washing to obtain the oil-soluble hydroxyapatite nanometer particles. The method has the advantages that the raw materials are rich in resource and can be easily obtained; the cost is low; a synthesis process is simple; the process repeatability is high; the product quality is stable; the appearance controllability is good; the dispersivity is good; the method can be widely applied to the fields of biomedical materials, coating materials and the like.

Description

technical field [0001] The invention relates to a method for preparing nanomaterials, in particular to a method for preparing oil-soluble hydroxyapatite nanoparticles based on a non-aqueous system. 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. [0003] At present, the method of synthesizing oil-soluble hydroxyapatite nanoparticles has been extensively studied. CN106063947A discloses a preparation method of monodisperse selenium-doped nano-hydroxyapatite, the method is to add...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B25/325C01P2002/72C01P2004/03C01P2004/20
Inventor 谭军军刘洋龚静黄亿
Owner HUBEI UNIV OF TECH
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