Graphene modified epoxy resin material and preparation method thereof
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A technology of graphene modification and epoxy resin, which is applied in the field of epoxy resin materials, can solve the problems of high brittleness and easy cracks, reduce shrinkage, improve structural stability, improve bonding strength and heat resistance stability sexual effect
Pending Publication Date: 2021-01-29
YANGZHOU POLYTECHNIC INST
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However, the volume of general oligomer resins will shrink more or less during the curing process, and the volume shrinkage of some widely used epoxy resins even reaches more than 5% when curing, and stress concentration is formed inside the product. prone to cracks
At the same time, this type of resin material is brittle, and its impact resistance and thermal conductivity still need to be improved.
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[0023] The invention provides a kind of preparation method of graphene modified epoxy resin material, comprises the following steps:
[0024] S1: Add graphene into nitric acid / sulfuric acid solution with a volume ratio of 1:3, ultrasonically disperse it evenly, and then reflux at 70-80°C for 2 hours to obtain carboxylated graphene;
[0025] S2: Adjust the silane coupling agent to acidity, then add it to absolute ethanol, add the carboxylated graphene for ultrasonic dispersion, react at 55-60°C for 6 hours, wash with acetone, filter, and dry to obtain graphene-grafted silane coupling agent;
[0026] S3: Add the carboxylated graphene, sodium dodecylbenzenesulfonate and ethanol in the container, ultrasonically disperse for 30 minutes, then add epoxy resin and mix evenly, continue ultrasonicating for 30 minutes, stir at 70-80°C to make the ethanol completely Volatilize to obtain graphene-doped epoxy resin;
[0027] S4: Transfer the graphene-doped epoxy resin to a stirred tank, a...
Embodiment 1
[0033] Embodiment 1: according to the above steps, the parts by weight of each component are 10 parts of graphene doped epoxy resin, 30 parts of inorganic nano fillers, 3 parts of curing agent and 1 part of modified silane coupling agent; wherein graphene doped The mass fraction of carboxylated graphene in the preparation of epoxy resin is 1% of epoxy resin, and the mass fraction of carboxylated graphene in the preparation of graphene-grafted silane coupling agent is 0.05% of silane coupling agent.
Embodiment 2
[0034] Embodiment 2: according to the above steps, the parts by weight of each component are 12 parts of graphene doped epoxy resin, 33 parts of inorganic nano fillers, 3 parts of curing agent and 1 part of modified silane coupling agent; wherein graphene doped The mass fraction of carboxylated graphene in the preparation of epoxy resin is 2% of epoxy resin, and the mass fraction of carboxylated graphene in the preparation of graphene-grafted silane coupling agent is 0.07% of silane coupling agent.
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Abstract
The invention relates to a graphene modified epoxy resin material and a preparation method thereof.The preparation method comprises the steps that firstly, carboxylated graphene is obtained after graphene is acidized, a graphene grafted silane coupling agent and graphene doped epoxy resin are prepared from the carboxylated graphene, and the graphene doped epoxy resin and an inorganic nano filler are heated and mixed; and the graphene grafted silane coupling agent and a curing agent are added, uniformly stirred, and vacuum degassing treatment is carried out to finally obtain the modified epoxyresin material. The shrinkage rate of the epoxy resin in the curing process is effectively reduced by utilizing the large specific surface area of the graphene and the nano-size effect of the nano inorganic filler, and the graphene of the layered structure is doped in the epoxy resin, so that the resin and the filler are mixed more sufficiently; in the curing process, the silane coupling agent grafted and modified by graphene participates in epoxy resin copolymerization, so that the structural stability of the resin material is improved, peeling or cracking caused by resin expansion at high temperature is avoided, and the bonding strength and the heat-resistant stability of the resin material are effectively improved.
Description
technical field [0001] The invention belongs to the field of epoxy resin materials, in particular to a preparation method of graphene-modified epoxy resin materials. Background technique [0002] Epoxy resin has the advantages of good adhesion, corrosion resistance, and low cost, and is currently one of the most widely used thermosetting resins. However, the volume of general oligomer resins will shrink more or less during the curing process, and the volume shrinkage of some widely used epoxy resins even reaches more than 5% when curing, and stress concentration is formed inside the product. Prone to cracks. At the same time, this type of resin material is highly brittle, and performances such as impact resistance and thermal conductivity still need to be improved. Contents of the invention [0003] Aiming at the deficiencies in the prior art, the present invention aims to combine graphene to reduce the shrinkage rate of epoxy resin material and improve the mechanical pr...
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