Preparation method of pH-responsive graphene/polymer nanometer hybrid material

A nano-hybrid material, graphene technology, applied in the fields of nano-materials and biomedical engineering, can solve problems such as functional limitations, limited wide application, poor dispersion, etc., achieve good biocompatibility, wide range of raw material sources, good dispersive effect

Active Publication Date: 2014-02-26
南通茂林医用材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although graphene has outstanding properties, its poor dispersion and functional limitations limit its wide application.

Method used

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  • Preparation method of pH-responsive graphene/polymer nanometer hybrid material

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Embodiment 1

[0019] The following examples are to further illustrate the present invention, but not to limit the scope of the present invention.

[0020] Weigh 1 gram of graphene oxide in a reaction kettle, disperse it with 80 grams of N,N-dimethylformamide, add 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride 12 grams of salt. Dissolve 22 grams of 2-(dodecyltrithiocarbonate)-2-methylpropionic acid in N,N-dimethylformamide and drop it into the reaction kettle at 0°C for 20 minutes After dropping, react at 5°C for 72 hours. After centrifugation at 5000 rpm for 30 minutes and drying at 30°C for 48 hours, the graphene oxide RAFT macromolecular chain transfer agent was obtained. Weigh 0.1 g of RAFT macromolecular chain transfer agent and disperse it in 2 g of dioxane, add 2 g of N,N-diethylaminoethyl methacrylate, then add 0.002 g of initiator azobisisobutyronitrile, and Vacuumize and fill with nitrogen three times, and react in an oil bath at 20° C. for 24 hours under the protec...

Embodiment 2

[0023] Weigh 1 gram of graphene oxide in a reaction kettle, disperse it with 100 grams of N,N-dimethylformamide, and then add 10 grams of chlorosulfonic acid. Dissolve 24 grams of 2-(dodecyltrithiocarbonate)-2-methylpropionic acid in N,N-dimethylformamide and drop it into the reaction kettle at 5°C for 30 minutes After dropping, react at 10°C for 60 hours. After centrifugation at 6000 rpm for 20 minutes and drying at 40 oC for 30 hours, the graphene oxide RAFT macromolecular chain transfer agent was obtained. Weigh 0.1 g of RAFT macromolecular chain transfer agent and disperse it in 3 g of anisole, add 3 g of N,N-diethylaminoethyl methacrylate, then add 0.004 g of initiator azobisisobutyronitrile, and Vacuum-inflate with nitrogen three times, and react in an oil bath at 30° C. for 20 hours under the protection of nitrogen. After the product was centrifuged at 6000 rpm for 20 minutes and dried at 40°C for 30 hours, a pH-responsive graphene oxide / polymer nano-hybrid material w...

Embodiment 3

[0026] Weigh 1 gram of graphene oxide into a reaction kettle, disperse it with 120 grams of N,N-dimethylacetamide, and then add 16 grams of thionyl chloride. Dissolve 24 grams of 2-(dodecyltrithiocarbonate)-2-methylpropionic acid in N,N-dimethylacetamide and drop it into the reaction kettle at 20°C for 35 minutes After dropping, react at 20°C for 40 hours. After centrifugation at 7000 rpm for 15 minutes and drying at 40°C for 30 hours, the graphene oxide RAFT macromolecular chain transfer agent was obtained. Weigh 0.1 g of RAFT macromolecular chain transfer agent and disperse it in 4 g of N,N-diethylformamide, add 4 g of N,N-diethylaminoethyl methacrylate, and then add the initiator azobisisobutyl Nitrile 0.006 g, through the process of evacuating and filling with nitrogen three times, and reacted in an oil bath at 40° C. for 12 hours under the protection of nitrogen. After the product was centrifuged at 7000 rpm for 15 minutes and dried at 40°C for 30 hours, a pH-responsive...

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Abstract

The invention discloses a preparation method of a pH-responsive graphene /polymer nanometer hybrid material. The preparation method comprises the following steps: under the protection of inert gas of argon or nitrogen, carrying out an esterification reaction by using a reversible addition-breakage chain transfer polymerization chain transfer agent of hydroxyl and terminal carboxyl on the surface of graphene oxide to obtain a macromolecular chain transfer agent for reversible addition-breakage chain transfer polymerization; and then, carrying out reversible addition-breakage chain transfer polymerization under initiation of azodiisobutyronitrile to obtain the pH-responsive grapheme/polymethylacrylic acid-N,N-lignocaine ethyl ester nanometer hybrid material. The graphene oxide/polymer nanometer hybrid material not only ensures that the dispersibility of graphene in water is greatly improved but also has pH responsiveness, and can be widely applied to the fields of drug controlled release carriers, biosensors, intelligent nanometer materials and the like. The preparation method is simple and easy, and industrial production of materials can be realized, so that the method has good popularization and application values.

Description

technical field [0001] The invention relates to the fields of nanomaterials and biomedical engineering, in particular to a preparation method of a pH-responsive graphene / polymer nano-hybrid material. Background technique [0002] Graphene is a new type of two-dimensional nanomaterial with excellent physical and chemical properties and has application prospects in many fields. It is known as the thinnest material in the world. The 2010 Nobel Prize in Physics is awarded to scientists who have made outstanding contributions in the field of graphene. Although graphene has outstanding properties, its poor dispersion and functional limitations limit its wide application. Graphene oxide is an important component of graphene-like materials. The reactive groups on the surface of graphene oxide allow graphene oxide to be further modified and modified. Through special polymer surface grafting, graphene materials are expected to be further functionalized and intelligent. [0003] En...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/34C08F2/38
Inventor 何敏袁伟忠薛剑其他发明人请求不公开姓名
Owner 南通茂林医用材料有限公司
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