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Nano hydroxyapatite hybrid material and preparation method thereof

A technology of nano-hydroxyapatite and hybrid materials, which is applied in medical formulas, medical preparations of non-active ingredients, medical science, etc., to achieve the effect of mild conditions, good application prospects, and good biological activity

Inactive Publication Date: 2011-06-08
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no temperature-sensitive nano-hydroxyapatite hybrid material prepared by grafting cross-linked poly(N-isopropylacrylamide) on the surface of nano-hydroxyapatite by atom transfer radical polymerization. to report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) First, dissolve 2.21g APS in 100mL ethanol / water mixed solvent with a volume ratio of 90:10 and stir for 30 minutes, then add 6.63g HA, react for 3 hours, adjust the pH value of the reaction system to 9-10 with ammonia water, continue Stir for 3 hours. Centrifuge to collect the solid matter, and dry it in an oven at 130°C for 2 hours, then wash it with ethanol three times, and dry it to obtain hydroxyapatite (HA-APS) with amino groups on the surface. The thermal weight loss in the range of 200~800℃ is 2.5%.

[0017] 2) Add 1 g of HA-APS into the dry reactor under the protection of argon, then add 30 mL of anhydrous DMF into the reaction flask, add 0.6 mL of triethylamine and stir for 20 minutes, and then sonicate for 30 minutes HA-APS is fully dispersed. Take 1g of bromoisobutyryl bromide and dissolve it in 20mL of anhydrous DMF. Then the DMF solution of bromoisobutyryl bromide was added dropwise to the HA-APS turbid solution. After reacting at room temperature f...

Embodiment 2

[0020] 1) Same as operation 1) in Example 1.

[0021] 2) Same as operation 2) in Example 1.

[0022] 3) Take 200mg of HA-Br prepared in operation 2) into the reactor, then add 20mL of deionized water, then add 480mg of NIPAM, 12.3mg of bpy, 5.8mg of BIS, stir for 10 minutes, and then ultrasonically disperse. Feed N into the reactor 2 , bubbling for 30 minutes to fully eliminate the oxygen in the reaction system, and then, in N 2 Under protection, 5.4 mg of CuBr was added, stirred, and reacted at room temperature for 2 hours. Centrifuge, wash the solid product several times with deionized water, and dry to obtain a nano-hydroxyapatite hybrid material grafted with poly(N-isopropylacrylamide) on the surface. As determined by a thermogravimetric analyzer, the resulting hybrid material has a thermal weight loss of 26.87% in the range of 200 to 800°C. It is determined by theoretical analysis that the mass of poly(N-isopropylacrylamide) grafted on the surface of hydroxyapatite per...

Embodiment 3

[0024] 1) Same as operation 1) in Example 1.

[0025] 2) Same as operation 2) in Example 1.

[0026] 3) Take 100mg of HA-Br prepared in operation 2) into the reactor, then add 20mL deionized water, then add 480mg NIPAM, 12.3mg bpy, 5.8mg BIS, stir for 10 minutes, and then ultrasonically disperse. Feed N into the reactor 2 , bubbling for 30 minutes to fully eliminate the oxygen in the reaction system, and then, in N 2Under protection, 5.4 mg of CuBr was added, stirred, and reacted at room temperature for 5 hours. Centrifuge, wash the solid product several times with deionized water, and dry to obtain a nano-hydroxyapatite hybrid material grafted with poly(N-isopropylacrylamide) on the surface. Using a thermogravimetric analyzer, the resulting hybrid material has a thermal weight loss of 52.37% in the range of 200 to 800°C. It is determined by theoretical analysis that the mass of poly(N-isopropylacrylamide) grafted on the surface of hydroxyapatite per gram It is 1.22g.

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Abstract

The invention provides a nano hydroxyapatite hybrid material which is characterized in that poly(N-isopropylacrylamide) with temperature sensitivity is grafted on the surface of nano hydroxyapatite. A preparation method of the hybrid material is as follows: (1) dissolving a silane coupling agent gama-aminopropyltriethoxysilane in ethanol and water, adding the nano hydroxyapatite the weight of which is 0.5-3 times as heavy as that of the silane coupling agent into the solution, reacting for 3-5 hours, regulating the pH value to 9-10, reacting for 3 hours again, carrying out vacuum filtering, washing with ethanol, and drying; (2) under the protection of nitrogen or argon, reacting the product with bromoisobutyryl bromide for 2-5 hours in anhydrous dimethylformamide in the presence of triethylamine; and (3) reacting for 0.5-24 hours by taking the products as initiators, using cuprous bromide / 2-2' bipyridine as a catalyst and using N,N-methylenebisacrylamide as a cross-linking agent under an oxygen-free condition in water from room temperature to 70 DEG C. In the invention, the reaction condition is mild, the product has the advantages of good bioactivity, good biocompatibility and good temperature sensitivity, and hydrophobic-hydrophilic reverse transformation happens at the temperature of about 32 DEG C.

Description

technical field [0001] The invention relates to a nano-hydroxyapatite hybrid material grafted with temperature-sensitive poly(N-isopropylacrylamide) on the surface and a preparation method thereof. technical background [0002] The research on organic / inorganic hybrid materials has received extensive attention both in theory and in application. By grafting polymers and organic molecules on the surface of inorganic nanoparticles, the main properties such as hydrophilicity, adhesion and surface activity of the surface of inorganic nanoparticles can be effectively regulated (Biomaterials 2007, 28, 550; J. Mater.Chem.2007, 17, 174; Chem.Mater.2006, 18, 5864.), especially constructing a stimuli-responsive interface on the surface of nanoparticles to obtain a temperature-sensitive hybrid material, because of its application in artificial organs, drug controlled release, regeneration Medicine, microfluidic technology, biological separation and other fields have important applicati...

Claims

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Application Information

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IPC IPC(8): C08F292/00A61L27/16A61L27/12A61K47/32A61K47/02
Inventor 魏俊超戴延凤陈义旺陈玉凤
Owner NANCHANG UNIV
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