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Method for preparing small-molecule imide modified carbon nano-tube

A molecular imide and carbon nanotube technology, applied in the field of materials, can solve problems such as difficult dispersion, hindering the excellent performance of carbon nanotubes, and poor heat resistance, and achieve easy control, improved mechanical properties and electrical properties, and preparation methods simple and easy effects

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

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Problems solved by technology

It has been reported that short-chain aliphatic amines grafted on carbon nanotubes were used as curing agents for epoxy resins [1] , although aliphatic ammonia-modified carbon nanotubes are widely used and ideally dispersed in solvents, the presence of aliphatic chains makes them poor in heat resistance, and it is difficult to be well-prepared in high-performance resins other than epoxy resins. Dispersion, which hinders the excellent performance of carbon nanotubes

Method used

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  • Method for preparing small-molecule imide modified carbon nano-tube
  • Method for preparing small-molecule imide modified carbon nano-tube

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: Preparation of carboxylated carbon nanotubes

[0021] First mix 500mg MWNT with 150ml H 2 SO 4 with HNO 3 mixed solution (98%H 2 SO 4 : 68% HNO 3 = 3:1) mixed, and reflux reaction for 4 hours at 35-40° C. and 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. Then the above acidified and washed product was placed 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.

Embodiment 2

[0022] Embodiment 2: the preparation of multi-walled carbon nanotube-g-ethylenediamine-g-nitrophenylmaleimide, its operational route is as follows:

[0023]

[0024] Step 1: Put 400 mg of acidified carbon nanotubes prepared in Example 1 into a reaction flask, add 8 g of condensing agent N,N-diisopropylcarbodiimide, and 20 ml of ethylenediamine, and mix evenly. Reflux in 50ml of N,N dimethylformamide in an oil bath at 120°C for 24h. After the reaction is complete, use absolute ethanol to ultrasonically wash away the excess amine, filter with a microporous membrane (0.45μm in diameter), and repeat the cleaning for several times. The carbon nanotubes were collected until the pH value of the filtrate was neutral, and dried in vacuum at 40° C. for 24 hours to obtain black aminated multi-walled carbon nanotubes.

[0025]Step 2: Take 100 mg of aminated carbon nanotubes obtained in step (1) and place them in a reaction flask, add 5 g of nitrogen-phenylmaleimide, add catalyst 5 ml o...

Embodiment 3

[0026] Example 3: Preparation of multi-walled carbon nanotube-g-ethylenediamine-g-maleimide.

[0027] Step 1: Take 200 mg of acidified carbon nanotubes prepared in Example 1 and place them in a reaction flask, add 6 g of 1-ethyl-3-dimethylaminopropyl carbodiimide, and add 20 ml of ethylenediamine, and mix evenly . Reflux in 100ml of N,N-dimethylacetamide at 150°C for 8h. After the reaction is complete, use absolute ethanol to ultrasonically wash away the excess amine, filter with a microporous membrane (0.45μm in diameter), and repeat the washing several times until The pH value of the filtrate was neutral, and the carbon nanotubes were collected and vacuum-dried at 40° C. for 24 hours to obtain black aminated multi-walled carbon nanotubes.

[0028] Step 2: Take 100 mg of aminated carbon nanotubes obtained in step (1) and place them in a reaction flask, add 13 g of maleimide, add 5 ml of glacial acetic acid as a catalyst, and use 50 ml of diethyl ether as a solvent, reflux at...

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Abstract

The invention relates to a preparation method for carbon nanotubes modified by micromolecule imide, and belongs to the material technical field. The method adopts the following specific steps: firstly, pure multi-wall carbon nanotubes are acidified in two steps to obtain carboxylated carbon nanotubes; the carboxylated carbon nanotubes further react with diamine to obtain aminated carbon nanotubes; then the aminated carbon nanotubes react with maleimide under the function of a catalyst to obtain multi-wall carbon nanotubes grafted and modified by the maleimide. The invention realizes covalent grafting of a maleimide group to the carbon nanotubes. The obtained product can be well dispersed in a resin matrix with high performance, thus various mechanical properties and mechanical properties of the resin matrix can be improved, the promotion and the updating of products such as bismaleimide, polyimide, cyanate, etc. can be realized, or new application fields can be developed.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of carbon nanotubes modified by small molecule imides. Background technique [0002] Carbon nanotubes (MWNTs) have excellent physical, chemical and mechanical properties, and they have great potential application value in many aspects. The preparation of carbon nanotube / polymer composite materials can improve the mechanical properties of polymers, prepare photoelectric functional materials, lubricating additives, etc. At present, polymer / carbon nanotube composites have become the main research and application direction of carbon nanotubes. However, carbon nanotubes with a micron-scale length are insoluble in water and organic solvents, and are usually mixed with a polymer solution to form a suspoemulsion state. In the final composite material, there is an undesirable aggregation state, and the intertwined carbon nanotube coils are not formed. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C3/08C09C1/44
Inventor 李文峰王翀刘琳
Owner TONGJI UNIV
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