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Prepn process of nanometer calcium phosphat particle

A nanoparticle and calcium phosphate technology, applied in nanostructure manufacturing, nanotechnology, nanotechnology and other directions, can solve the problems of high cost, serious agglomeration, neglect, etc., and achieve cheap and easy-to-obtain raw materials, simple preparation process, and increased stability. Effect

Inactive Publication Date: 2007-03-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods used to prepare nano-calcium phosphate mainly include sol-gel method, solid-phase reaction method, hydrothermal method, etc. The calcium phosphate prepared by these methods is usually in the shape of flakes, needles, rods or irregular particles, and the size is uniform. Greater than 100 nanometers, and the agglomeration phenomenon is serious, and monodispersion cannot be achieved
The microemulsion method and normal phase micelle method proposed subsequently can artificially control the shape and size of the synthesized particles to a certain extent, and the dispersibility of the prepared powder is better. For example: Bose and Saha: Susmita Bose ; SusantaKumar Saha Chem.Mater.2003,15,4464-4469, take NP-5 and NP-12NP-5 as (poly(oxyethylene)5nonylphenol ether; NP-12 is poly(oxyethylene)12 nonylphenol ether) as surfactant , with cyclohexane as the oil phase, Ca(NO 3 ) 2 and H 3 PO 4 As a reactant, the microemulsion method is used to synthesize HAP with a particle size between 30nm and 50nm, needle-like, sheet-like and spherical shapes. However, this type of preparation method has high cost and low yield, and how to introduce a large amount of The complete removal of organic matter has become a new problem in the material preparation process; while Yao Jia et al., Masafumi Uota; Hiroshi Arakawa; Nana Kitamura; Takumi Yoshimura; Junzo Tanaka; Alkyltrimethylammonium bromide (CTAB) is a cationic surfactant, and short rod HAP particles with a thickness of 50-100nm and a length of 500-1000nm were synthesized by the normal phase micellar method
Their work showed that using CTAB as a surfactant can effectively control the morphology of the prepared calcium phosphate particles, but they did not systematically explore the mechanism of CTAB’s morphology control during the synthesis process, thus ignoring the According to the critical micelle concentration (CMC) theory, the important content of the size and morphology of calcium phosphate particles can be better regulated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A calcium phosphate nanoparticle, the preparation process of which is as follows:

[0015] 1. Keep the reaction temperature at 25°C, add 1.11ml of CTAB solution with a concentration of 0.09M to 79ml of deionized water, and stir at a speed of 200 rpm;

[0016] 2. After stirring the solution in the first step above for 30 minutes, add 0.167ml of disodium hydrogen phosphate solution with a concentration of 0.3M dropwise at a rate of 1 drop / second, and stir while adding;

[0017] 3. After stirring the solution in the second step above for 30 minutes, add ammonia water with a concentration of 1M to it, adjust the pH of the solution to 10, and stir while adding;

[0018] 4. After stirring the solution in the third step above for 30 minutes, slowly add 20ml of calcium nitrate solution with a concentration of 0.0025M to it at a rate of 1 drop / second. During the process of adding calcium chloride solution, use a concentration of 1M The ammoniacal liquor adjusts solution in the ...

Embodiment 2

[0021] A calcium phosphate nanoparticle, the preparation process of which is as follows:

[0022] 1. Keep the reaction temperature at 30°C, add 2ml of CTAB solution with a concentration of 0.09M to 230ml of deionized water, and stir at a speed of 300 rpm;

[0023] 2. After the above-mentioned first step solution was stirred for 60 minutes, 6ml of disodium hydrogen phosphate solution with a concentration of 0.3M was added dropwise to it at a rate of 2 drops / second, and the dropwise addition was accompanied by stirring;

[0024] 3. After stirring the solution in the second step above for 30 minutes, add sodium hydroxide with a concentration of 1M to it, adjust the pH of the solution to 9, and stir while adding;

[0025] 4. After stirring the solution in the third step above for 30 minutes, slowly add 60 ml of calcium chloride solution with a concentration of 0.05M to it, and the rate of addition is 1 drop / second. In the process of adding calcium chloride solution, use a concentr...

Embodiment 3

[0028] A calcium phosphate nanoparticle, the preparation process of which is as follows:

[0029] 1. Keep the reaction temperature at 20°C, add 1ml of CTAB solution with a concentration of 0.09M to 230ml of deionized water, add dropwise while stirring, and the stirring speed is 400 rpm;

[0030] 2. After the above-mentioned first step solution was stirred for 60 minutes, 6ml of disodium hydrogen phosphate solution with a concentration of 0.3M was added dropwise to it at a rate of 3 drops / second, and the dropwise addition was accompanied by stirring;

[0031] 3. After the above-mentioned second step solution was stirred for 30 minutes, potassium hydroxide with a concentration of 1M was added dropwise to it to adjust the pH of the solution to 11, and the dropwise addition was accompanied by stirring;

[0032] 4. After stirring the solution in the third step above for 30 minutes, slowly add 60ml of calcium acetate solution with a concentration of 0.05M to it at a rate of 2 drops / ...

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PUM

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Abstract

The preparation process of nanometer calcium phosphate particle includes the following steps: dropping solution containing calcium ion slowly into mixed solution containing phosphate radical ion and cetyl trimethyl ammonium bromide (CTAB), dropping alkali solution to regulate pH value of the solution to obtain calcium phosphate sol, filtering after reaction to obtain precipitate, washing the precipitate for several times, and vacuum drying to obtain nanometer calcium phosphate particle of average size smaller than 100 nm. Altering the amount of added CTAB during reaction can change the diameter of the prepared nanometer calcium phosphate particle in 20-80 nm effectively.

Description

Technical field: [0001] The invention discloses a preparation method for preparing size-controllable calcium phosphate nanoparticles, which belongs to the technical field of new materials. Background technique: [0002] Calcium phosphate is basically the same as the inorganic components of human hard tissues, and its biocompatibility and interface bioactivity are superior to all kinds of medical titanium, silicone rubber and carbon materials for bone grafting. It also has excellent osteoconductivity and bone The ability to combine, plus no toxic side effects, no carcinogenic effect, so it is widely used as hard tissue repair materials and bone filling materials. With the development of detection technology and nanoscience, it has recently been found that human hard tissue is composed of many calcium phosphate particles with a size smaller than 50 nanometers uniformly dispersed in organic components. In addition, new uses of nano-calcium phosphate have also been continuously...

Claims

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Application Information

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IPC IPC(8): C01B25/34B82B3/00
Inventor 唐睿康蔡玉荣陶锦晖胡晴红
Owner ZHEJIANG UNIV
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