Porous hydroxyapatite flower-like microspheres and preparation method thereof

A hydroxyapatite and flower-like technology, applied in the field of porous hydroxyapatite flower-like microspheres and its preparation, to achieve the effects of shortened reaction time, strong diffraction peaks, and low cost

Inactive Publication Date: 2013-05-08
NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The rapid prototyping technology of 3D design is still in the development stage, and it will take a long time before it can be really applied to tissue engineering.

Method used

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  • Porous hydroxyapatite flower-like microspheres and preparation method thereof
  • Porous hydroxyapatite flower-like microspheres and preparation method thereof
  • Porous hydroxyapatite flower-like microspheres and preparation method thereof

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preparation example Construction

[0025] A kind of preparation method of porous hydroxyapatite flower-like microsphere of the present invention, comprises the following steps:

[0026] First, add CaO to 80°C distilled water to digest it into Ca(OH) with a concentration of 1% to 10%. 2 For slurry, the digestion time is more than 10h to ensure that the CaO is completely digested; at room temperature, the Ca(OH) 2 Slurry into CO 2 / N 2 Mixed gas, CO 2 and N 2 The molar ratio is 0.1-0.5, the speed is 1L / min, and the reaction stops when the pH value of the reaction system reaches 7.

[0027] Then add Al(OH) 3 The molar ratio of calcium to aluminum is 5:1~50:1; phosphate solution is added under heating (usually 60°C) and stirring, and NaOH solution is added during the reaction to keep the pH of the reaction system at 10.0. After 2~4 hours of reaction, the The white precipitate is separated from the mother liquor, and the precipitate is centrifuged and washed with distilled water until the pH value of the solut...

Embodiment 1

[0032] Add 0.56g CaO to 80°C distilled water to digest it into Ca(OH) with a mass concentration of 1%. 2 For slurry, the digestion time is 11 hours to ensure complete digestion of CaO. At room temperature, and with mechanical stirring, the slurry was bubbled with CO 2 / N 2 Mixed gas (CO 2 and N2 The molar ratio is 0.2), the speed is 1L / min, and the pH value of the reaction system reaches 7 to stop the reaction. Then add Al(OH) 3 , the molar ratio of calcium to aluminum is 20:1. Under electric stirring at 60°C in a water bath, 20ml of the prepared 0.3mol / L sodium phosphate solution was added dropwise. During the reaction, NaOH solution was added to keep the pH of the reaction system at 10.0, and the reaction was carried out for 2h. Centrifuge, wash the precipitate until the pH value of the solution reaches 7, centrifuge, and dry at 80°C for 24h to obtain a powder product. The stirring condition in this embodiment is 200 rpm.

[0033] Field emission scanning electron micr...

Embodiment 2

[0035] Add 0.56g CaO to 80°C distilled water to digest it into Ca(OH) with a mass concentration of 3%. 2 For slurry, the digestion time is more than 12 hours to ensure complete digestion of CaO. At room temperature, and with mechanical stirring, the slurry was bubbled with CO 2 / N 2 Mixed gas (CO 2 and N 2 The molar ratio is 0.3), the speed is 1L / min, and the pH value of the reaction system reaches 7 to stop the reaction. Then add Al(OH) 3 , the molar ratio of calcium to aluminum is 10:1. Electric stirring under 60 ° C water bath, the prepared 0.3mol / L Na 2 HPO 4 Add 20ml of the solution dropwise, add NaOH solution during the reaction to keep the pH of the reaction system at 10.0, and react for 3h. Centrifuge, wash the precipitate until the pH value of the solution reaches 7, centrifuge, and dry at 80°C for 24h to obtain a powder product. The stirring condition in this embodiment is 300 rpm.

[0036] Figure 4 It is a scanning electron micrograph of the porous hydro...

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Abstract

The invention discloses porous hydroxyapatite flower-like microspheres and a preparation method thereof. The preparation method comprises the following steps: adding 80 DEG C distilled water into CaO to slake the CaO into 1-10 wt% Ca(OH)2 slurry, introducing a CO2/N2 gas mixture into the slurry at room temperature while mechanically stirring, and stopping the reaction when the pH value of the reaction system reaches 7; under the conditions of heating and stirring, adding Al(OH)3 and a phosphate solution, wherein an NaOH solution is added in the reaction process to keep the pH value of the reaction system at 10.0; after some time, centrifuging, and washing the precipitate until the pH value of the solution is approximate to a neutral state; and centrifuging, and drying to obtain the porous hydroxyapatite flower-like microsphere powder product. The invention does not need to add any complex organic substance, polymer or the like, and also does not need to add any operation step for removing the template after the reaction; meanwhile, no impurity appears in the product, and thus, the method is simple to operate and low in cost, thereby laying foundation for industrial production; and the prepared porous hydroxyapatite flower-like microspheres have huge application prospects in the fields of tissue engineering, drug delivery and the like.

Description

technical field [0001] The invention relates to a porous hydroxyapatite flower-shaped microsphere and a preparation method thereof, belonging to the field of preparation of inorganic materials. Background technique [0002] According to the pore-forming (or pore-forming) principle, porous hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 , HAP) can be divided into bionic method (Dominic Walsh, Chem Mater, 1996,8,1994-2001; Mao Chuanbin, Chemical Progress, 1998,9,246-254), sintering method (H, US Patent, 1987-06-17 ), pore forming agent method, foaming agent method, template method (Hing K A, J Mater Sci: Mater in Medicine, 1999,10,135-145), three-dimensional design rapid prototyping technology and other seven categories. At present, most research institutions are committed to mixing HAP powder with a pore-forming agent, burning or decomposing the pore-forming agent after calcination, and finally making porous HAP. Ryshkewitch et al. (Arita I H, Biomaterials, 1995, 16, 403-408; E, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/32
Inventor 刘莹唐玉霞卢光明滕兆刚朱飞鹏杨楠楠
Owner NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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