Functionalized carbon nano-tube used as solidifying agent of epoxy resin and preparation method

A technology of epoxy resin curing and carbon nanotubes, applied in the direction of dyeing low-molecular organic compound treatment, fibrous fillers, etc., to achieve functional design and application, and improve the effect of the interface

Inactive Publication Date: 2009-01-14
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, functionalized carbon nanotubes prepared by reacting aromatic polybasic anhydride compounds with carbon nanotubes have not been reported yet.

Method used

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  • Functionalized carbon nano-tube used as solidifying agent of epoxy resin and preparation method
  • Functionalized carbon nano-tube used as solidifying agent of epoxy resin and preparation method
  • Functionalized carbon nano-tube used as solidifying agent of epoxy resin and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 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 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. Place the product after the above acidification and washing 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.

[0027] Step 2: Take 400 mg of the above-mentioned acidified carbon nanotubes and place them in a reaction flask, add 20 ml of SOCl 2 and 1ml of N,N-dimethylformamide (DMF), stirred and refluxed at 70°C for 24h. Filter and ...

Embodiment 2

[0031] According to the method described in Example 1, 400 mg of hydroxylated carbon nanotubes was dissolved in dimethyl sulfoxide, ultrasonically oscillated for 30 minutes, 5 g of benzophenone tetracarboxylic anhydride was added, and 1 g of catalyst 4,4-dithiol was added, stirred evenly, and heated at 90 ° C. Under nitrogen protection, magnetic stirring, condensing and reflux, and a reaction time of 48 hours, a carbon nanotube epoxy resin curing agent containing acid anhydride groups and carboxyl groups on the surface was prepared. The schematic diagram of the reaction route is as figure 2 shown.

Embodiment 3

[0033] Acyl chloride carbon nanotubes were prepared according to the method described in Example 1. Take 400mg of acid chloride and place it in a 50ml single-necked bottle, add 30ml of ethylenediamine and 5ml of 3,3-dichlorobenzidine hydrochloride (DCB), heat to 120°C, condense and reflux for 48h with magnetic stirring. Then filter with a vinylidene fluoride membrane with a pore size of 0.45 μm, rinse with anhydrous THF for 5 times, put the product in a vacuum oven, and dry it at 40° C. for 24 hours to obtain a product of surface aminated carbon nanotubes.

[0034] Dissolve 400 mg of aminated carbon nanotubes in dimethyl sulfoxide, oscillate ultrasonically for 30 minutes, add 4 g of mellitic acid trianhydride, add catalyst nickel dibutyldithiocarbamate 1 g, stir evenly, at 90 ° C, under nitrogen protection , magnetically stirred, condensed and refluxed, the reaction time was 48h, and a carbon nanotube epoxy resin curing agent containing acid anhydride groups and carboxyl group...

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Abstract

The invention relates to a functionalized carbon nanotube which can be used as epoxy resin curing agent and the preparation method, which belongs to the technical field of the nano-material. After a purified carbon nanotube is treated with strong oxidative acid, a carboxylated carbon nanotube is obtained; the carboxylated carbon nanotube is chlorided by thionyl chloride, and the obtained product is reacted with polyhydric alcohol or polybasic amine to obtain a modified carbon nanotube with hydroxyl or amidogen; then the hydroxyl is utilized to react with aromatic polybasic acid anhydride compound to obtain the functionalized carbon nanotube with anhydride group and carboxyl group, which can be further used as curing agent to ensure carbon nanotube well dispersed in epoxy resin, thus to improve the compatibility between the carbon nanotube and the epoxy resin, both the mechanical property and the thermal stability of the epoxy resin can be improved, thereby the advantage of the carbon nanotube can be exerted to the maximum, and the functional design and the application of the carbon nanotube can be achieved.

Description

technical field [0001] The invention relates to a surface-modified carbon nanotube, in particular to a method for preparing a functionalized carbon nanotube which can be used as an epoxy resin curing agent. Background technique [0002] Epoxy resin is a thermosetting oligomer with poor properties. In addition to being used as a stabilizer for polyvinyl chloride, it has no direct use value. But when it reacts with the curing agent to form a three-dimensional cross-linked network structure, it presents a series of excellent properties. Therefore, the chemical reaction between curing agent and epoxy resin is the basis and core of epoxy resin application. The behavior of the epoxy resin during the curing process and the performance of the cured product depend to a large extent on the performance of the curing agent and the interaction and reasonable coordination between her and the resin, which in turn depends on the molecular structure of the curing agent. Therefore, studyin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/44C09C3/08C08K3/04C08L63/00
Inventor 王国建王瑶黄思浙商伟辉
Owner TONGJI UNIV
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