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Preparation method of modified nano-hydroxyapatite/polyethylene glycol compound hydrogel

A nano-hydroxyapatite and composite hydrogel technology, applied in the field of biological materials, can solve problems such as poor dispersibility, achieve the effects of improving compatibility, mild reaction conditions, and solving easy agglomeration

Inactive Publication Date: 2017-03-15
HENAN INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of poor dispersion of nHA in PEG matrix, the present invention provides a preparation method of modified nano-hydroxyapatite / polyethylene glycol composite hydrogel, in which PEG molecules are grafted on the surface of nHA, and then Thermosensitive PEG hydrogels were prepared by compounding modified nHA with PEG

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The method for preparing the modified nano-hydroxyapatite / polyethylene glycol composite hydrogel of this embodiment includes the following steps:

[0020] (1) Add 1mL of 3-aminopropyltriethoxysilane (0.004mol) (Shanghai Jingchun Reagent Co., Ltd.) coupling agent to 100mL of ethanol and water mixed solution for 0.5h at room temperature, and then 2.1g (0.004mol) hydroxyapatite (Shanghai Jingchun Reagent Co., Ltd.) was added to the mixed solution and stirred for 8h at room temperature (rotating speed 800rpm), then the reacted product was centrifuged and dried, and the dried product was used Wash with ethanol and dry in vacuum to obtain hydroxyapatite with amino groups on the surface. The silane coupling agent is grafted to the surface of nano-hydroxyapatite to aminate the surface (HA-NH2);

[0021] (2) Dissolve 1g (0.016mol) of dried (water content 30ppm) polyethylene glycol (PEG-COOH) with terminal carboxyl groups (PEG-COOH) (Suzhou Angu Nanotechnology Co., Ltd.) in 100mL of d...

Embodiment 2

[0024] The method for preparing the modified nano-hydroxyapatite / polyethylene glycol composite hydrogel of this embodiment includes the following steps:

[0025] (1) The silane coupling agent is grafted onto the surface of nano-hydroxyapatite to aminate the surface to obtain nano-hydroxyapatite (HA-NH2) modified with amino groups;

[0026] (2) Dissolve 1g (0.016mol) of dried (water content 30ppm) polyethylene glycol (PEG-COOH) containing terminal carboxyl groups in 100mL of dichloromethane, and then add 10.44g (0.064mol) N to the solution ,N'-carbonyldiimidazole, activate the carboxyl group for 2h (activation temperature 4℃, stirring speed 300rpm) to obtain the PEG-COOH solution after activation of the carboxyl group, and then add 4.01g (0.008mol) HA- to the PEG-COOH solution NH2, stirred and reacted at room temperature for 12h, after the reaction, the product was centrifuged, washed, and dried to obtain PEG-modified nano-hydroxyapatite (HA-PEG);

[0027] (3) Dissolve 10g 8-arm end ...

Embodiment 3

[0029] The method for preparing the modified nano-hydroxyapatite / polyethylene glycol composite hydrogel of this embodiment includes the following steps:

[0030] (1) Graft the silane coupling agent onto the surface of nano-hydroxyapatite to aminate the surface to obtain nano-hydroxyapatite (HA-NH2) modified with amino groups;

[0031] (2) Dissolve 1g (0.016mol) of dried polyethylene glycol (PEG-COOH) containing terminal carboxyl groups (PEG-COOH) in 100mL of dichloromethane after drying (30ppm water content), and then add 7.83g (0.048mol) N to the solution ,N'-carbonyldiimidazole, activate the carboxyl group for 1h (activation temperature 4℃, stirring speed 300rpm) to obtain the PEG-COOH solution after activation of the carboxyl group, and then add 2.67g (0.0053mol) HA- to the PEG-COOH solution NH2, stirred and reacted at room temperature for 12h, after the reaction, the product was centrifuged, washed, and dried to obtain PEG-modified nano-hydroxyapatite (HA-PEG);

[0032] (3) Diss...

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PUM

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Abstract

The invention discloses a preparation method of modified nano-hydroxyapatite / polyethylene glycol compound hydrogel. The preparation method mainly comprises the following steps: (1) grafting a silane coupling agent to the surface of nano-hydroxyapatite, so as to generate surface amination (HA-NH2); (2) grafting polyethylene glycol containing terminal carboxyl groups to the surface of HA-NH2, so as to obtain PEG modified HA; and (3) mixing the modified HA with a multi-arm amine terminated PEG solution, regulating the temperature to 37 DEG C and hatching for a certain period of time by taking genipin as a cross-linking agent, so as to obtain the modified nano-hydroxyapatite / polyethylene glycol compound hydrogel. By virtue of the preparation method, the problem that PEG hydrogel is relatively poor in mechanical strength, and HA easily aggregates are effectively solved; and meanwhile, all reactions are carried out at the normal temperature, so that reaction conditions are mild, the preparation process is simple, and the application prospect is relatively wide.

Description

Technical field [0001] The invention belongs to the field of biomaterials and wound repair, and specifically relates to a method for preparing modified nano-hydroxyapatite / polyethylene glycol composite hydrogel. Background technique [0002] Hydrogel is a three-dimensional polymer network structure formed by cross-linking hydrophilic molecules through physical or chemical methods. It has swelling, biocompatibility and biodegradability. It is an elastomer between solid and liquid. It is precisely because the hydrogel has a three-dimensional network structure and the water content is about 70-90%, which is similar to the water content of articular cartilage (the water content is 70-80%), and the hydrogel is an elastic body similar to the cartilage structure. It has low solid content and fewer degradation products, which can greatly reduce the immune response of degradation products to the human body. In addition, the hydrogel has stable chemical properties and good moldability, so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/075C08L71/02C08K9/04C08K9/06C08K3/32C08K5/101
CPCC08J3/075C08J2371/02C08K3/32C08K5/101C08K9/06C08K9/08C08K2003/325C08K2201/011C08L71/02
Inventor 王延伟于翔杨柳徐茜张浩
Owner HENAN INST OF ENG