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Method for preparing graft polymer containing carbon nano-tube

A technology of grafted polymers and carbon nanotubes, which is applied in fiber modification, spinning, and plastic fields, can solve problems such as difficult bonding, large surface energy, and influence on uniform dispersion, so as to improve dissolution and dispersion performance and increase interface The effect of binding force and broad application prospects

Inactive Publication Date: 2008-07-09
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Carbon nanotubes have a high aspect ratio and large surface energy, which directly lead to the insolubility of carbon nanotubes, and are extremely prone to agglomeration, which affects their uniform dispersion in solutions or composite materials.
At the same time, its surface is complete and smooth, with very few dangling bonds, and it is difficult to bond with the matrix, so it cannot achieve ideal performance, which hinders the application of carbon nanotubes in composite materials.

Method used

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  • Method for preparing graft polymer containing carbon nano-tube

Examples

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Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Using multi-walled carbon nanotubes as starting materials, after acidification, acyl chloride and alcoholization, hydroxyl groups are introduced on the surface of carbon nanotubes, and then a redox initiation system is formed with cerium ions to initiate the polymerization of acrylonitrile to obtain carbon-containing Nanotube-grafted polymers.

[0033] Step 1: Add 3.0g of multi-walled carbon nanotubes (MWNTs), 40mL of nitric acid, and 120mL of sulfuric acid into a 1000mL flask with a condenser, which needs to be equipped with a strong stirring device; immerse the flask in an ultrasonic bath (59KHz) for 10min It is well dispersed; then, heating in an oil bath, reflux reaction for 110min, and at the same time, the heating temperature is gradually increased from 90°C to 120°C, and the thick brown gas generated during this period is collected by a plastic conduit through a condenser and treated with a sodium hydroxide solution; After the reaction is completed and...

Embodiment 2

[0038] Step 1: Add 3.0g of multi-walled carbon nanotubes (MWNTs), 60mL of hydrogen peroxide, and 120mL of sulfuric acid into a 1000mL flask with a condenser, which must be equipped with a strong stirring device; immerse the flask in an ultrasonic bath (40KHz) 48h to make it well dispersed; then, heat in an oil bath and reflux for 48h, while the heating temperature gradually rises from 90°C to 150°C. Treatment: After the reaction is completed, after cooling to room temperature, the reaction mixture is first diluted, separated by a centrifuge, and then vacuum filtered through a 0.22 μm polyvinylidene fluoride membrane, washed with deionized water several times until the pH value is close to 7; vacuum at 25°C Drying at lower temperature for 48h to obtain acidified carbon nanotubes;

[0039] Step 2: Add 0.28g of acidified MWNTs-COOH and 15mL of excess phosphorus trichloride to the ampoule with a stirring and condensing reflux device, and immerse the flask in an ultrasonic bath (40...

Embodiment 3

[0043] Step 1: Add 3.0g of multi-walled carbon nanotubes (MWNTs) and 180mL of concentrated nitric acid into a 1000mL flask with a condenser, which must be equipped with a strong stirring device; immerse the flask in an ultrasonic bath (100KHz) for 24 hours to make it well Disperse; then, heat in an oil bath and reflux for 24 hours, while the heating temperature gradually rises from 25°C to 100°C. During this period, the thick brown gas generated is collected by a plastic conduit through a condenser and treated with sodium hydroxide solution; the reaction is over , after cooling to room temperature, the reaction mixture was first diluted, separated with a centrifuge, then vacuum filtered through a 0.22 μm polyvinylidene fluoride membrane, washed with deionized water several times until the pH value was close to 7; dried in an oven at 100°C 0.5h, obtain acidified carbon nanotubes;

[0044] Step 2: Add 0.28g of acidified MWNTs-COOH and 15mL of excess phosphorus tribromide to the ...

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Abstract

The invention relates to a process for preparing graft polymers containing carbon nano-tubes. The process comprises oxygenizing carbon nano-tubes with strong acid, getting carboxylic group on the surface of the carbon nano-tubes after acidizing, further reacting with alcohols after reacting with acylating agent, getting carbon nano-tube whose surface is provided with hydroxyl group, and then, an oxidation-reduction initiation system is combined by ceric ion and the carbon nano-tube whose surface is provided with hydroxyl group under acidic condition, leading vinyl monomers to polymerize, realizing grafting polymer chains on the surface of the carbon nano-tube, and getting graft polymers which contain the carbon nano-tube. The structure of the carbon nano-tube is specifically changed after grafting, dissolution and dispersion properties of the carbon nano-tube are greatly improved, and the carbon nano-tube can be well dispersed into plastic and fiber, which can be used to prepare film material with high intensity, fiber with high performance and the like, and the carbon nano-tube itself can be dissolved in organic solvent to be electrically spun into silks. The invention can be applied in the field such as plastic, fiber modification, spinning and the like.

Description

Technical field: [0001] The invention relates to a preparation method for surface modification of carbon nanotubes, in particular to a preparation method for graft polymers containing carbon nanotubes, which can be applied to the fields of plastics, fiber modification and spinning. Background technique: [0002] Carbon nanotubes (CNTs) are seamless, hollow tubes rolled from graphite sheets formed by carbon atoms, and the tube wall is generally composed of carbon hexagons. In addition, there are some pentagonal carbon rings and heptagonal carbon rings that can close or bend the top of carbon nanotubes. According to the number of tube wall layers, carbon nanotubes can be divided into single-walled carbon nanotubes (SWNTs) and multi-walled carbon nanotubes (MWNTs). [0003] Carbon nanotubes have a high aspect ratio and large surface energy, which directly lead to the insolubility of carbon nanotubes, and are extremely prone to agglomeration, which affects their uniform dispers...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08K3/04
Inventor 隋坤艳杨春嘉孙宁纪全夏延致孔庆山
Owner QINGDAO UNIV
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