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High performance epoxy resins composite material and preparation thereof

A technology of epoxy resin and composite materials, which is applied in chemical instruments and methods, fibrous fillers, inorganic pigment treatment, etc., can solve the problems of uneven dispersion of carbon nanotubes, weak interface between carbon nanotubes and matrix materials, etc. Achieve the effects of reduced volume resistivity, convenient preparation, and simple process

Inactive Publication Date: 2009-04-15
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, there are problems that carbon nanotubes are not uniformly dispersed in the matrix material, and the interfacial interaction between the modified carbon nanotubes and the matrix material is not strong.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1: Mix 500 mg of multi-walled carbon nanotubes with an average diameter of 8 to 15 nm and a length of 50 μm with 150 ml of 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-mentioned one-step 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.

[0032] 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...

Embodiment 2

[0036] The first and second steps are to prepare acyl chloride carbon nanotubes according to the method described in Example 1.

[0037] Step 3: Mix 0.2 g of carbonyl chloride carbon nanotubes and 30 g of ethylene glycol evenly, and heat and reflux in an oil bath at 96° C. for 36 hours. After the reaction is completed, filter with a microporous membrane (0.45 μm in diameter) and dry in vacuum to obtain carbon nanotubes with hydroxyl groups on the surface. Dissolve 400 mg of hydroxyl carbon nanotubes in dimethyl sulfoxide, oscillate ultrasonically for 30 minutes, add 4 g of benzophenone tetraacid dianhydride, add 1 ml of concentrated sulfuric acid as a catalyst, and stir well. Under nitrogen protection at 90 ° C, magnetic stirring, the reaction time is 48 Hours, carbon nanotubes with acid anhydride groups on the surface were obtained.

[0038] Step 4: Take 30g E-51 epoxy resin and preheat it at 60°C. According to 1 wt% of the total amount, 0.3 g of carbon nanotubes modified w...

Embodiment 3

[0040] In the first to third steps, the carbon nanotubes modified with pyromellitic dianhydride were prepared according to the method described in Example 1.

[0041] Step 4: Take 30g E-51 epoxy resin and preheat it at 60°C. According to 1% of the total amount, 0.3 g of carbon nanotubes modified with pyromellitic dianhydride was taken, added to the preheated epoxy resin, vigorously stirred for 8 hours, ultrasonically dispersed for 4 hours, and mixed uniformly. Add 16g of curing agent diphenyl ether tetra-acid dianhydride, mechanically stir evenly; place in a vacuum oven to remove air bubbles, pour, cure at 200°C for 1 hour, and demould to obtain an epoxy resin composite material.

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PUM

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Abstract

The invention belongs to the technical field of nano materials, and particularly relates to a high-performance epoxide resin composite material and a preparation method. Carboxylic acid, chloroformylation, amination or hydroxylation are carried out to the carbon nano tube; and the carbon nano tube is modified by small molecular aromatic polyanhydride compound so as to prepare the carbon nano tube which carries acid anhydride group. The carbon nano tube is dispersed in epoxide resin substrate by ultrasonic oscillation and high-speed stirring, is cured by adopting organic acid anhydride curing agent so as to obtain the carbon nano tube / epoxide resin composite material. The invention leads the preparation of the carbon nano tube / epoxide resin composite material to be more convenient, the activity of taking part in reaction of the carbon nano tube is endowed, and acid anhydride group of the carbon nano tube and the epoxide resin group of the epoxide resin generate chemical cross linking, thus improving the dispersion of the carbon nano tube in the epoxide resin and obtaining high-performance epoxide resin composite material. Compared with the control sample, all the mechanical performance indexes of the cured composite material are improved by 5 percent to 300 percent and the volume resistivity is reduced by 3 to 9 order of magnitude.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, specifically relates to the preparation technology of carbon nanotube composite materials, and refers to a preparation method of carbon nanotube / epoxy resin composite materials used as surface structure materials, coatings or adhesives. Background technique [0002] Since Iijima discovered carbon nanotubes in 1991, carbon nanotubes have been a research hotspot in recent years because of their unique structure, good electrical 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 quant...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08K9/04C09C3/00C09C1/44
Inventor 王国建王瑶刘琳许乾慰
Owner TONGJI UNIV
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