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Preparation method of expanded graphite flake/thermosetting resin composite material

A resin composite material and expanded graphite technology, applied in the field of resin matrix composite material preparation, can solve the problems of complex process, long cycle, release a large amount of toxic gas, etc., and achieve the effect of reducing the possibility of agglomeration and speeding up the curing speed.

Inactive Publication Date: 2012-07-18
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] As far as the chemical method is concerned, the main method at present is the graphite oxide reduction method. Although this method can obtain very thin expanded graphite flakes, the process of this method is complicated, the cycle is long, and a large amount of toxic gas will be released during the preparation process, which limits range of application

Method used

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  • Preparation method of expanded graphite flake/thermosetting resin composite material
  • Preparation method of expanded graphite flake/thermosetting resin composite material
  • Preparation method of expanded graphite flake/thermosetting resin composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Put 1g of expandable graphite into a 50 mL porcelain crucible, put it in a muffle furnace at 900°C, stay for 30s, and take it out to obtain expanded graphite.

[0032] See attached figure 1 , It is the infrared spectrum of the expanded graphite provided in this example. As you can see, 1098cm -1 And 1395cm -1 There are the stretching vibration peak of C–O and the bending vibration peak of –OH, indicating the existence of hydroxyl active functional groups on the surface of expanded graphite.

[0033] 2) 10g bisphenol A epoxy resin (brand E51, epoxy value 0.51 mol / 100g, viscosity at 70°C is about 0.4Pa.s) mixed with 0.17g expanded graphite, and stirred with ultrasonic vibration at 70°C Uniform and obtain a mixed solution.

[0034] 3) Put the mixed solution in a vacuum oven at 70°C and apply a vacuum (vacuum degree of 6 Pa) for 30 minutes to obtain dispersion A.

[0035] 4) At 70°C, the dispersion A was stirred with ultrasonic vibration for 5 hours to obtain a dispersion B of ...

Embodiment 2

[0049] 1) Put 1g of expandable graphite into a 50 mL porcelain crucible, put it in a microwave oven, irradiate it with a microwave with a power of 700W and a frequency of 2.45G Hz for 10 seconds, and take it out to obtain expanded graphite.

[0050] 2) 10g of bisphenol A epoxy resin (brand E51) is mixed with 0.17g of expanded graphite, and stirred evenly with the aid of ultrasonic oscillation at 70°C to obtain a mixed solution.

[0051] 3) Put the mixed solution in a vacuum oven at 70°C and vacuum (vacuum 10 Pa) for 30 minutes to obtain dispersion A;

[0052] 4) At 70°C, the dispersion A was stirred with ultrasonic oscillation for 5 hours to obtain a dispersion B of expanded graphite flakes and epoxy resin;

[0053] 5) Add 0.5 g of curing agent (2-ethyl-4-methylimidazole) to dispersion B at 70°C, and stir the mixture with ultrasonic vibration for 5 minutes to obtain dispersion C;

[0054] 6) Pour dispersion C into the mold, and then put it in a microwave oven, use 700W power, 2.45G Hz m...

Embodiment 3

[0056] 1) Put 1g of expandable graphite into a 50 mL porcelain crucible, put it in a muffle furnace at 900°C, stay for 30 seconds, and take it out to obtain expanded graphite.

[0057] 2) At room temperature, at a molar ratio of 1:1.4, pour γ-glycidoxypropyltrimethoxysilane (brand KH-560) and deionized water into a three-necked flask and mix; gradually add an appropriate amount of hydrochloric acid, while Stir constantly to pre-hydrolyze at room temperature for about 15 minutes; condense and reflux at 55°C for 7 hours to obtain a colorless transparent liquid; put the liquid in a vacuum drying oven at 60°C and vacuum dry for 7 hours to obtain a colorless (light yellow) transparent Viscous liquid, which is hyperbranched polysiloxane (denoted as HBPSi).

[0058] 3) Add N,N'-4,4'diphenylmethane bismaleimide (BDM) and diallyl bisphenol A (DBA) to the beaker at a mass ratio of 1:0.86. Under stirring conditions, the temperature was raised to 135°C, and the reaction was stopped after 40 m...

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Abstract

The invention discloses a preparation method of an expanded graphite flake / thermosetting resin composite material, which comprises the following steps: allowing the internal void of expanded graphite to generate negative pressure in conditions that the degree of vacuum is lower than or equal to 10Pa, the temperature is the one keeping thermosetting resin to be in a liquid state, and the viscosityis lower than or equal to 1.5Pa.s, wherein the negative pressure is favorable for the resin to enter the lamellar structure of expanded graphite and sufficiently impregnate the lamellar structure of graphite; and stripping the lamella of expanded graphite through ultrasonic agitation to obtain expanded graphite flakes, at the same time, forming a physical or chemical bond action between the thermosetting resin and the surface groups of the expanded graphite flakes, and curing under a microwave condition to obtain uniformly dispersed expanded graphite flake / thermosetting resin composite material. The preparation method disclosed by the invention overcomes the defects in preparing the expanded graphite composite materials using a solvent method, including that the expanded graphite flakes are likely to agglomerate and the solvent pollutes the environment, and has the characteristics of simpleness, rapidness, environmental friendliness, and energy conservation.

Description

Technical field [0001] The invention relates to a method for preparing a resin-based composite material, in particular to a method for preparing an expanded graphite flake / thermosetting resin composite material. Background technique [0002] With the rapid development of information, electronics and power industries, expanded graphite flakes / polymer composites are used as functional materials due to their large diameter-to-thickness ratio, high electrical conductivity, simple preparation process and low price ( Such as conductive materials, electromagnetic shielding materials, antistatic materials, high-capacity batteries, etc.) have shown broad application prospects in many fields. [0003] Although most expanded graphite flakes / polymer composites use thermoplastic polymers as the matrix resin, thermosetting resins show obvious advantages in the preparation of nanocomposites due to their excellent molding process and reactivity. The research of polymer composite materials has att...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/28C08J3/24C08J3/02C08L63/00C08L79/08C08L79/04C08K3/04
Inventor 顾嫒娟常健飞梁国正袁莉
Owner SUZHOU UNIV
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