Preparation method of nano hydroxyapatite

A technology of nano-hydroxyapatite and nano-spheres, applied in the field of nano-materials, can solve the problems of expensive raw materials, poor dispersion, and unsuitability for large-scale production, and achieve the effect of simple preparation method, mild and controllable conditions

Active Publication Date: 2012-06-13
SUZHOU UNIV
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Problems solved by technology

[0005] The prior art discloses a variety of reports on the preparation of hydroxyapatite nanoparticles using biomimetic technology, such as Thachepan S and other researchers published in the "NANOSCALE" document "Mesoscale crystallization of calcium phosphate nanostructures in protein (casein) micelles" in 2010 pointed out that the use of protein micelles as templates can regulate the nanostructure and morphology of hydroxyapatite; Rivera-Munoz, EM and other researchers published the document "Growth of Hydroxyapatite Nanoparticles on Silica Gels" in "JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY" in 2011 " pointed out that using silica gel as a template can control the morphology of hydroxyapatite, but the raw materials required by the above method are expensive and not suitable for large-scale production
[0006] The Chinese patent document with the application number CN201010618923.5 discloses a hydroxyapatite / silk fibroin composite material. First, calcium nitrate solution and sodium silicate solution are mixed and reacted, and the reactants are calcined to obtain wollastonite; Silk fibroin dissolves in molten calcium nitrate to form SF-Ca(NO 3 ) 2 solution; the wollastonite powder was dissolved in water to form a suspension, and then SF-Ca(NO 3 ) 2 Solution, obtain hydroxyapatite / silk fibroin composite material, but, the composite material dispersibility that this method obtains is poor; Lin Niu et al published the literature " A Novel Nanocomposite Particle of Hydroxyapatite and Silk in Journal of Nanomaterials in 2010 Fibroin: Biomimetic Synthesis and Its Biocompatibility", Chunquan Fan et al. published in "J Mater Sci" in 2010 in the literature "Facile fabrication of nano-hydroxyapatite / silk fibroin composite via a simplified coprecipitation route" all disclose the preparation of silk fibroin as a template The method of hydroxyapatite, but the structure and morphology of the obtained hydroxyapatite are uncontrollable, and the dispersion is poor, easy to agglomerate, and cannot be uniformly dispersed in aqueous solution, which seriously hinders the further application of hydroxyapatite

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[0030] The invention provides a method for preparing nano-hydroxyapatite, comprising the following steps:

[0031] After the silk fibroin aqueous solution is sealed and cultivated, the silk fibroin nanosphere aqueous solution is obtained;

[0032] The silk fibroin nanosphere aqueous solution is mixed with a phosphate source and a calcium source, and the nano-hydroxyapatite is obtained after reaction.

[0033] In the present invention, the silk fibroin aqueous solution is first sealed and cultivated to obtain the silk fibroin nanosphere aqueous solution; then, the silk fibroin nanosphere aqueous solution is used as a template to synthesize nano-hydroxyapatite on the surface of the silk fibroin nanosphere, and the silk fibroin and hydroxyl The apatite interaction can not only inhibit the agglomeration of hydroxyapatite, but also obtain nano-hydroxyapatite with controllable size and shape by controlling the concentration of silk fibroin aqueous solution.

[0034] In the inventio...

Embodiment 1

[0068] The silk in the mass concentration of 0.5% Na 2 CO 3 Boil in the solution for 60 minutes at 100°C to remove sericin on the outside of the silk; wash the obtained product with deionized water, repeat 3 times, and dry at 60°C to obtain silk fibroin;

[0069] Dissolve 27 grams of silk fibroin in 100 mL of lithium bromide solution, put the obtained silk fibroin solution in a dialysis bag and immerse it in deionized water for dialysis for 3 days, during which the water is changed every two hours to obtain a pure silk fibroin solution. The mass concentration is 5.9%; the silk fibroin solution is sealed and incubated at 60° C. for 12 hours to obtain a silk fibroin nanosphere solution, and the diameter of the silk fibroin nanosphere is 30 to 50 nanometers;

[0070] The silk fibroin nanosphere solution is subjected to atomic force microscope analysis and infrared spectrum analysis, the results can be found in figure 1 with figure 2 , figure 1 The atomic force microscope ana...

Embodiment 2

[0075] The silk in the mass concentration of 0.5% Na 2 CO 3 Boil in the solution for 60 minutes at 100°C to remove sericin on the outside of the silk; wash the obtained product with deionized water, repeat 3 times, and dry at 60°C to obtain silk fibroin;

[0076] Dissolve 27 grams of silk fibroin in 100 mL of lithium bromide solution, put the obtained silk fibroin solution in a dialysis bag and immerse it in deionized water for dialysis for 3 days, during which the water is changed every two hours to obtain a pure silk fibroin solution. The mass concentration is 5.9%;

[0077] The silk fibroin solution was sealed and incubated at 90° C. for 4 hours to obtain a silk fibroin nanosphere solution, and the diameter of the silk fibroin nanosphere was 20 to 40 nanometers;

[0078] The atomic force microscope analysis and infrared spectrum analysis were carried out on the silk fibroin nanosphere solution, and the results showed that the silk fibroin nanosphere was obtained in the pr...

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Abstract

The invention provides a preparation method of nano hydroxyapatite. The method comprises the steps that after silk fibroin water solution is conducted to sealing incubation, silk fibroin nanosphere water solution is obtained; and the silk fibroin nanosphere water solution is mixed with a phosphate group source and a calcium source, and then nano hydroxyapatite is obtained after reaction. The invention provides another preparation method of nano hydroxyapatite. The method comprises the steps that firstly, silk fibroin water solution is treated under electrostatic field, and silk fibroin nanosphere is obtained; secondly, the silk fibroin nanosphere obtained in the first step is mixed with a phosphate group source and a calcium source, and then nano hydroxyapatite is obtained after reaction. The preparation method has the advantages that noxious solvent is not required to be used, the preparation method is simple, the condition is mild and controllable, the secondary structure of silk fibroin can not be destroyed, and silk fibroin nanosphere with controllable size and appearance can be obtained, so that nano hydroxyapatite with controllable size and appearance can be obtained.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a preparation method of nanometer hydroxyapatite. Background technique [0002] Silk fibroin is a structural protein that exists widely in nature. It can be extracted from silk fiber of silkworm. It not only has sufficient sources and simple extraction methods, but also has good biocompatibility, biodegradability, good mechanical properties and good The adhesion, expansion and differentiation of cells is a kind of organic matrix material with good development prospects. Silk fibroin can be prepared into various forms such as solutions, films, porous scaffolds, gels, etc., and has good application prospects in the field of biomedicine. [0003] Hydroxyapatite (Hydroxyapatite, HA, Ca 10 (PO 4 ) 6 (OH) 2 ) is a weakly alkaline calcium phosphate salt slightly soluble in water, belonging to the hexagonal crystal system, and is a class of inorganic materials with good ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32B82Y40/00
Inventor 黄晓卫吕强张岑岑林莎莎赵荟菁
Owner SUZHOU UNIV
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