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Method for preparing macromolecule modified carbon nano-tube and application thereof

A carbon nanotube and polymer technology, which is applied in the field of materials to achieve wide application prospects, improve compatibility and improve performance.

Inactive Publication Date: 2010-12-08
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polymer functionalized carbon nanotubes with maleic anhydride segments prepared by in situ polymerization of acid anhydride, carbon nanotubes and compounds with double bonds have not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 1: mix 500mg multi-walled carbon nanotubes with 150ml H 2 SO 4 with HNO 3 mixed solution (98%H 2 SO 4 : 68% HNO 3 = 3:1) mixed, and refluxed for 4 hours at 35-40° C. under the condition of ultrasonic vibration. Then filter with a metafluoride membrane with a pore size of 0.45 μm, and wash with water until the pH is neutral. The product was placed in a vacuum oven and dried under vacuum at 40°C for 24h. Place the above-mentioned one-step acidified and washed product in H 2 SO 4 with H 2 o 2 mixed solution (98%H 2 SO 4 : 30%H 2 o 2 =4:1) at 70°C for 2h. Then filter with a metafluoride membrane with a pore size of 0.45 μm, and wash with water until the pH is neutral. The product was placed in a vacuum oven and dried under vacuum at 40°C for 24h.

[0021] Step 2: Take 400 mg of carbon nanotubes that have been acidified in two steps and place them in a reaction flask, add 20 ml of SOCl 2 And 1ml of dimethylformamide, stirred and refluxed at 70°C for 24h...

Embodiment 2

[0025] The first step and the second step are the same as in Example 1. In the third step, 200 mg of hydroxy carbon nanotubes are added to the xylene solution containing 6 g of maleic anhydride, vigorously stirred, and 0.15 g of p-toluenesulfonic acid is added, at 120 React at ℃ for 24 hours, stop the reaction, filter with a vinylidene fluoride membrane with a pore size of 0.45 μm, wash with acetone, and filter with a nylon membrane with a pore size of 0.45 μm to obtain a black powder. Add 180 mg of this black powder and 5.07 g of maleic anhydride to a three-necked flask, then add 1 / 3 of the toluene solution of nitrostyrene and azobisisobutyronitrile, and control the temperature at reflux at 70°C for 2 hours; 80°C, 1h. Then drop the remaining 2 / 3 of the toluene solution of nitrostyrene and azobisisobutyronitrile through the separatory funnel, and the reaction was carried out for about 3 hours, and the reaction was stopped. Washing with acetone, until the filtrate is precipita...

Embodiment 3

[0027] The first step and the second step are the same as in Example 1. In the third step, 200 mg of hydroxycarbon nanotubes are added to a xylene solution containing 6 g of maleic anhydride, vigorously stirred, 0.15 g of benzenesulfonic acid is added, and the mixture is heated at 100° C. After reacting for 24 hours, stop the reaction, filter with a vinylidene fluoride membrane with a pore size of 0.45 μm, wash with acetone, and filter with a nylon membrane with a pore size of 0.45 μm to obtain a black powder. Add 180 mg of this black powder and 5.07 g of maleic anhydride to a three-necked flask, then add 1 / 3 of the toluene solution of styrene and azobisisobutyronitrile, and control the temperature of reflux at 70°C for 2h; 80°C for 1h. Then drop the remaining 2 / 3 of the toluene solution of styrene and azobisisobutyronitrile through the separatory funnel, and the reaction was carried out for about 3 hours, and the reaction was stopped. Washing with acetone, until the filtrate ...

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Abstract

The present invention provides a macromolecule modified carbon nano-tube made by in situ polymerization and the related preparation method. Concentrated sulfuric acid and concentrated nitric acid are used for the first-step acidification treatment of the carbon nano-tube; then concentrated sulfuric acid and hydrogen peroxide are used for the second-step acidification treatment; afterward, the acidified carbon nano-tube reacts with dichloride sulfoxide and the product will then react with diol to produce a modified carbon nano-tube with hydroxyl; finally, the carbon nano-tube containing polymerizable double bonds is obtained after the pre-reaction between hydroxy and maleic anhydride. The carbon nano-tube containing polymerizable double bonds and maleic anhydride have in situ polymerization reaction with substances containing double bonds and then are connected on the external surface of the carbon nano-tube so that the carbon nano-tube can be well dispersed into composite materials toimprove the compatibility between the carbon nano-tube and other materials in order to maximize the advantages of the carbon nano-tube and realize the functionalized design and application of the carbon nano-tube.

Description

technical field [0001] The invention belongs to the field of materials and relates to carbon nanotubes, in particular to a method for chemically modifying the surface of carbon nanotubes. Background technique [0002] Since Lijima discovered carbon nanotubes in 1991, carbon nanotubes have been a research hotspot in recent years because of their unique structure, good electrical properties and mechanical properties. Carbon nanotubes have nanoscale diameters and micron-scale lengths, and the aspect ratio can reach 100-1000. They are extremely strong and have ideal elastic modulus. They are an excellent fiber material, and their performance is better than any current fiber. Therefore, it can be used as a superfiber for the reinforcement of advanced composite materials; because carbon nanotubes combine the semi-metallic properties of graphite with the quantum laws of energy levels and electronic waves, and have nanoscale dimensions, making them in the field of electronics The a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02C08F292/00
Inventor 王国建屈泽华刘琳郭建龙李岩
Owner TONGJI UNIV
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