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Preparation method of nano hydroxyapatite grafted polyhydroxybutyrate-hydroxyvalerate (PHBV)

A technology of polyhydroxybutyrate copolyester and nano-hydroxyapatite, which can be used in prosthetics, tissue regeneration, medical science, etc., can solve problems such as easy reunion, achieve mild reaction conditions, simple methods, and promising application prospects broad effect

Active Publication Date: 2016-05-18
HENAN INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The modified nano-hydroxyapatite obtained by the preparation method improves the compatibility between nano-hydroxyapatite and polyhydroxybutyrate copolyester matrix, and solves the problem of nano-hydroxyapatite in polyhydroxybutyrate copolyester matrix. The problem of easy agglomeration in the acid copolyester matrix improves the mechanical properties of the PHBV / HA composite material; the present invention is basically carried out at room temperature, the reaction conditions are mild, the preparation process is simple, and the preparation efficiency is high. In addition, the material shows Good cell and tissue compatibility, especially suitable for tissue engineering applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation method of the nano-hydroxyapatite grafted polyhydroxybutyrate valeric acid copolyester of the present embodiment is as follows:

[0020] (1) The PHBV film is evacuated to 7Pa in the plasma processor, then ammonia gas is introduced to 40Pa, and treated at 60W for 120 seconds, and then the treated PHBV material is cleaned and dried to obtain aminated PHBV (PHBV- NH2);

[0021] (2) Prepare 100mL of 1% dilute glutaraldehyde solution, then add the PHBV-NH2 material to the glutaraldehyde aqueous solution at a molar ratio of 1:1, react for 6 hours under stirring conditions, centrifuge, wash and dry after the reaction is completed , that is, the PHBV (PHBV-CHO) with surface aldehydes was obtained;

[0022] (3) Add 1ml of 3-aminopropyl triethoxy silicon into the mixed solution of 100ml of ethanol water, fully hydrolyze, then add 4.29g of hydroxyapatite into the mixed solution, react for 6h, and then put the reacted The product is centrifuged, washed, and dried ...

Embodiment 2

[0025] The preparation method of the nano-hydroxyapatite grafted polyhydroxybutyrate valeric acid copolyester of the present embodiment is as follows:

[0026] (1) The PHBV film is evacuated to 7Pa in the plasma processor, then ammonia gas is introduced to 80Pa, and treated at 80W for 180 seconds, and then the treated PHBV material is cleaned and dried to obtain aminated PHBV (PHBV- NH2);

[0027] (2) Prepare 100mL of 1% dilute glutaraldehyde solution, then add the PHBV-NH2 material to the glutaraldehyde aqueous solution at a molar ratio of 1:1.5, react for 8 hours under stirring conditions, centrifuge, wash and dry after the reaction is completed , that is, the PHBV (PHBV-CHO) with surface aldehydes was obtained;

[0028] (3) Add 1ml of 3-aminopropyl triethoxy silicon into 200ml of ethanol water mixed solution, fully hydrolyze, then add 4.29g of hydroxyapatite into the mixed solution, react for 6h, and then put the reacted The product is centrifuged, washed, and dried to ob...

Embodiment 3

[0031] The preparation method of the nano-hydroxyapatite grafted polyhydroxybutyrate valeric acid copolyester of the present embodiment is as follows:

[0032] (1) The PHBV membrane is vacuumed to 7Pa in the plasma processor, then ammonia gas is introduced to 60Pa, and treated at 80W for 180 seconds, and then the treated PHBV material is cleaned and dried to obtain aminated PHBV (PHBV- NH2);

[0033] (2) Prepare 100mL of 1% dilute glutaraldehyde solution, then add the PHBV-NH2 material to the glutaraldehyde aqueous solution at a molar ratio of 1:1, react for 8 hours under stirring conditions, centrifuge, wash and dry after the reaction is completed , that is, the PHBV (PHBV-CHO) with surface aldehydes was obtained;

[0034] (3) Add 1ml of 3-aminopropyl triethoxy silicon into the mixed solution of 100ml of ethanol water, fully hydrolyze, then add 8.56g of hydroxyapatite into the mixed solution, react for 6h, and then put the reacted The product is centrifuged, washed, and dri...

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PUM

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Abstract

The invention discloses a preparation method of nano hydroxyapatite grafted polyhydroxybutyrate-hydroxyvalerate (PHBV), which mainly comprises the following steps: (1) introducing amino groups on PHBV molecules by utilizing an ammonia plasma processing method; (2) processing PHBV after amination by utilizing glutaraldehyde so as to carry out hydroformylation on PHBV; (3) processing nano hydroxyapatite by utilizing a silane coupling agent so as to carry out amination on nano hydroxyapatite; and (4) reacting PHBV after hydroformylation and nano hydroxyapatite after amination to obtain PHBV grafted nano hydroxyapatite. The method disclosed by the invention effectively solves the problem that nano hydroxyapatite is easy to agglomerate in a PHBV substrate; meanwhile, the method is basically carried out at normal temperature and is mild in reaction condition, simple in preparation process, relatively high in preparation efficiency and wide in application prospect; Nano hydroxyapatite grafted PHBV prepared by the method disclosed by the invention has potential application in tissue engineering and bone defect repair.

Description

technical field [0001] The invention relates to a preparation method and application of nano-hydroxyapatite-grafted polyhydroxybutyrate-valeric acid copolyester, and belongs to the technical field of biomedical polymer materials. Background technique [0002] Hydroxyapatite (HA), which has a composition and structure similar to human bone tissue and has good biocompatibility, is a recognized bone repair material, but it does not have biodegradability and toughness in vivo poor. Polyhydroxybutyrate copolyester (PHBV) is a good medical polymer material, which is biodegradable, non-antigenic, non-toxic, and non-carcinogenic, and has received extensive attention in recent years. In recent years, the PHBV / HA composite material prepared by mixing PHBV and HA has shown good mechanical properties and degradable properties. At the same time, the composite material also combines the toughness of PHBV and the strength of HA, and is suitable for tissue engineering bone defects. Repair...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L27/44A61L27/46A61L27/50C08G63/91C08J7/12
CPCA61L27/44A61L27/46A61L27/50A61L2430/02C08G63/912C08J7/12C08J2367/04C08L67/04
Inventor 于翔王延伟杨柳徐茜丁宁
Owner HENAN INST OF ENG
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