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Preparing method for oil-based hydroxyapatite colloidal crystals

An oil-based hydroxyapatite and colloidal technology, which is applied in the direction of liquid crystal materials, chemical instruments and methods, phosphorus compounds, etc., to achieve the effects of easy-to-obtain, low-cost, and easy-to-implement

Inactive Publication Date: 2016-03-23
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the research on hydroxyapatite petroleum-based colloidal liquid crystals. It is assumed that unsaturated fatty acids can be used to successfully prepare anisotropic hydroxyapatite nanoparticle liquid crystal (closest to bone microstructure) dispersion system and successfully apply it to nano Among composite materials, it is bound to be able to realize the structural bionics of artificial bone in the true sense, comprehensively improve the mechanical properties of bone repair substitute materials, and benefit patients with bone defects

Method used

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  • Preparing method for oil-based hydroxyapatite colloidal crystals
  • Preparing method for oil-based hydroxyapatite colloidal crystals
  • Preparing method for oil-based hydroxyapatite colloidal crystals

Examples

Experimental program
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Effect test

Embodiment 1

[0031] 1) Add 24 mL of 0.83 mol / L calcium nitrate aqueous solution and 48 mL of ethanol, 0.038 mol of oleic acid and 0.025 mol of ethylenediamine into a three-necked flask and mix, and stir to obtain a uniform solution; under stirring conditions, add 0.5 mol / L trisodium phosphate Add 24mL of aqueous solution to the above solution slowly dropwise, and continue to stir for 10min after the addition is complete;

[0032] 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;

[0033] 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 nanoparticles ;

[0034] The X-ray diffraction pattern of oil-soluble hydroxyapatite nanoparticles is shown in figure 1...

Embodiment 2

[0038] 1) Add 24 mL of 0.83 mol / L calcium chloride aqueous solution and 48 mL of ethanol, 0.038 mol of oleic acid and 0.025 mol of ethylenediamine into a three-necked flask and mix, and stir to obtain a uniform solution; Slowly add 24mL potassium aqueous solution to the above solution dropwise, and continue stirring for 10 minutes after the addition is complete;

[0039] 2) heating the mixed liquid obtained in step 1) to 80° C. for 3 hours, and then naturally cooling to room temperature to obtain a reaction liquid;

[0040] 3) Using a high-speed centrifuge to centrifuge the reaction solution obtained in step 2) to obtain a precipitate, and use absolute ethanol and toluene to alternately centrifuge and wash 3 times to remove electrolytes and excess fatty acids in the system to obtain oil-soluble hydroxyapatite nanoparticles;

[0041] Figure 5 It is the macrophotograph of the dispersion liquid of prepared oil-soluble hydroxyapatite nanoparticles, the particle mass concentratio...

Embodiment 3

[0045] 1) Add 24 mL of 0.83 mol / L calcium acetate aqueous solution and 48 mL of ethanol, 0.038 mol of oleic acid and 0.025 mol of ethylenediamine into a three-necked flask and mix, and stir to obtain a uniform solution; under stirring conditions, add 0.5 mol / L triammonium phosphate Add 24mL of aqueous solution to the above solution slowly dropwise, and continue to stir for 10min after the addition is complete;

[0046] 2) heating the mixed solution obtained in step 1) to 50° C. for 12 hours, and then naturally cooling to room temperature to obtain a reaction solution;

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

[0048] Figure 7 It is the macrophotograph of the dispersion liquid of prepared oil-soluble hydrox...

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Abstract

A preparing method for oil-based hydroxyapatite colloidal crystals comprises the steps that a soluble calcium saline solution is mixed with low alcohol, fatty acid and organic amine, and a uniform solution is obtained after stirring; under the stirring condition, soluble phosphoric acid saline is slowly dripped, the temperature is increased to 50-90 DEG C for a reaction for 3-24 h, the mixture is naturally cooled to the room temperature and centrifuged through a high-speed centrifugal machine, precipitate is obtained and subjected to centrifugal washed with absolute ethyl alcohol and a non-polar solvent alternately three times, electrolyte and redundant fatty acid in the system are removed, and oil-soluble hydroxyapatite nano-particles are obtained; the oil-soluble hydroxyapatite nano-particles are dispersed into the non-polar solvent with the particle concentration reaching 10-65% which exceeds the critical phase conversion concentration, and the oil-based hydroxyapatite colloidal crystals with intense birefringence are prepared. According to the preparing method, raw materials are rich in source and easy to obtain, cost is low, the synthesizing process is simple and easy to implement, and products are stable in quality and good in process repeatability and have good application prospects in biomedical composites and coating materials.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic lyotropic liquid crystals, in particular to a preparation method of oil-based hydroxyapatite colloidal liquid crystals. Background technique [0002] The hard tissues of many organisms in nature are not only light but also have excellent mechanical properties, such as shells, animal bones and teeth. Studies have shown that these excellent properties originate from the highly ordered distribution of anisotropic inorganic nanoparticles in the polymer matrix in hard tissues. The bones and teeth of mammals in nature are the result of highly ordered composites of rod-shaped hydroxyapatite nanoparticles and collagen. Originating from the biomimicry of natural hard tissue and meeting the society's increasingly urgent demand for replacement materials for human hard tissue, people have conducted in-depth research on hydroxyapatite / polymer nanocomposites. For most artificially synthesized nanocom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32C09K19/40
CPCC01B25/325C01P2002/72C01P2004/04C09K19/0216C09K19/404
Inventor 谭军军金小影胡兵
Owner HUBEI UNIV OF TECH
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