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CN-121991466-A - Temperature-resistant corrosion-resistant solid epoxy resin composite material and preparation method thereof

CN121991466ACN 121991466 ACN121991466 ACN 121991466ACN-121991466-A

Abstract

The invention relates to the technical field of epoxy resin composite materials, in particular to a temperature-resistant and corrosion-resistant solid epoxy resin composite material and a preparation method thereof, wherein the solid epoxy resin composite material comprises, by weight, 30-70 parts of an epoxy resin matrix, 6-24 parts of an aromatic curing agent, 3-17 parts of an organosilicon modifier, 6-30 parts of fly ash, 4-10 parts of montmorillonite, 0.6-2.4 parts of a silane coupling agent, 0.3-1.2 parts of 2-ethyl-4-methylimidazole, 0.3-0.8 part of triphenylphosphine and 0.05-0.8 part of an antioxidant 1010, and the epoxy resin matrix is at least one of bisphenol A epoxy resin and bisphenol F epoxy resin. The temperature-resistant corrosion-resistant solid epoxy resin composite material and the preparation method thereof provided by the invention effectively solve the technical problems of insufficient temperature resistance, poor corrosion resistance, difficult compromise of comprehensive performance and the like of the traditional epoxy resin composite material, and have various excellent effects.

Inventors

  • Zhong Gaozhong
  • WU RUNHUI

Assignees

  • 铜陵圣创新材料有限公司

Dates

Publication Date
20260508
Application Date
20260305

Claims (9)

  1. 1. The heat-resistant corrosion-resistant solid epoxy resin composite material is characterized by comprising, by weight, 30-70 parts of an epoxy resin matrix, 6-24 parts of an aromatic curing agent, 3-17 parts of an organosilicon modifier, 6-30 parts of fly ash, 4-10 parts of montmorillonite, 0.6-2.4 parts of a silane coupling agent, 0.3-1.2 parts of 2-ethyl-4-methylimidazole, 0.3-0.8 part of triphenylphosphine and 0.05-0.8 part of an antioxidant 1010, wherein the epoxy resin matrix is at least one of bisphenol A epoxy resin and bisphenol F epoxy resin; the aromatic curing agent is at least one of 4,4 '-diamino diphenyl sulfone and 4,4' -diamino diphenyl ether, the organosilicon modifier is at least one of polydimethylsiloxane and hydroxyethoxy polysiloxane, and the silane coupling agent is at least one of KH-550 and KH-560.
  2. 2. The temperature-resistant corrosion-resistant solid epoxy resin composite material according to claim 1, further comprising at least one of 0-4 parts of graphene and 0-1.5 parts of carbon black in parts by weight.
  3. 3. The solid state epoxy resin composite of claim 1, wherein the epoxy resin matrix is a mixture of bisphenol a epoxy resin and bisphenol F epoxy resin, and the silane coupling agent is a mixture of KH-550 and KH-560.
  4. 4. The solid state epoxy resin composite material of claim 1 wherein the silicone modifier is polydimethylsiloxane when the aromatic curative is 4,4 '-diaminodiphenyl sulfone and hydroxyethoxy polysiloxane when the aromatic curative is 4,4' -diaminodiphenyl ether.
  5. 5. A method of preparing a temperature-resistant corrosion-resistant solid epoxy resin composite material according to any one of claims 1 to 4, comprising the steps of: Firstly, pretreating a filler, namely mixing fly ash, montmorillonite and optional graphene, adding a silane coupling agent, stirring for 25-55 minutes at 70-100 ℃, then placing the mixture at 100-130 ℃ for drying for 1.5-3.5 hours, cooling to room temperature, crushing, and sieving with a 90-130 mesh sieve to obtain a modified composite filler; Step two, resin modification, namely placing an epoxy resin matrix into a reaction kettle, heating to 70-100 ℃, stirring at a rotating speed of 180-270r/min, slowly adding an organosilicon modifier, and stirring at a constant temperature for 55-85 minutes to obtain modified epoxy resin; Step three, mixing and dispersing, namely adding modified composite filler and optional carbon black into modified epoxy resin, heating to 85-110 ℃, stirring for 40-75 minutes at a rotating speed of 280-400r/min, and then adding antioxidant 1010 to continuously stir for 12-22 minutes to obtain a mixed matrix; And fourthly, curing and forming, namely uniformly mixing an aromatic curing agent, 2-ethyl-4-methylimidazole and triphenylphosphine, adding the mixture into a mixed matrix, stirring for 20 minutes until the system is uniform, pouring the mixture into a mold, curing by adopting a gradient heating curing process, cooling to room temperature, and demolding to obtain the temperature-resistant and corrosion-resistant solid epoxy resin composite material, wherein the gradient heating curing process sequentially comprises pre-curing, medium curing and post curing, the pre-curing time is 2 hours, the medium curing time is 3 hours, and the post curing time is 2 hours.
  6. 6. The preparation method according to claim 5, wherein in the first step, when graphene is added, the stirring temperature is 85-100 ℃, the stirring time is 40-55 minutes, the drying temperature is 115-130 ℃, the drying time is 2.5-3.5 hours, and the sieving mesh number is 120-130 meshes.
  7. 7. The method according to claim 5, wherein in the second step, when the epoxy resin matrix is a mixture of bisphenol A epoxy resin and bisphenol F epoxy resin, the temperature is raised to 85 ℃, the stirring speed is 230r/min, and the constant temperature stirring time is 75 minutes.
  8. 8. The method according to claim 5, wherein in the third step, when adding carbon black, the temperature is raised to 100 to 110 ℃, the stirring speed is 350 to 400r/min, the stirring time after adding the modified composite filler is 60 to 75 minutes, and the stirring time after adding the antioxidant 1010 is 18 to 22 minutes.
  9. 9. The method according to claim 5, wherein in the fourth step, the pre-curing temperature is 70-100 ℃, the intermediate curing temperature is 115-140 ℃, the post-curing temperature is 145-170 ℃, and when the aromatic curing agent is 4,4' -diaminodiphenyl ether, the pre-curing temperature is 90-100 ℃, the intermediate curing temperature is 130-140 ℃, and the post-curing temperature is 160-170 ℃.

Description

Temperature-resistant corrosion-resistant solid epoxy resin composite material and preparation method thereof Technical Field The invention relates to the technical field of epoxy resin composite materials, in particular to a temperature-resistant and corrosion-resistant solid epoxy resin composite material and a preparation method thereof. Background The epoxy resin composite material is widely applied to a plurality of industrial fields such as chemical industry, machinery, electronics and the like by virtue of good mechanical property, molding processability and adhesion property with a base material, and becomes an important structural and functional material. However, the existing epoxy resin composite material still has a plurality of technical defects in practical application, and is difficult to meet the requirements of complex working conditions of high temperature and strong corrosion. The conventional epoxy resin composite material has insufficient temperature resistance, is easy to generate relaxation of a crosslinked network in a high-temperature environment, and has the advantages of rapid decay of mechanical property and structural stability, and limited long-term use temperature. Meanwhile, the existing material has poor corrosion resistance, and corrosion factors easily permeate into the material in salt mist, acid and alkaline corrosion mediums, so that matrix degradation and interfacial peeling are caused, and further material performance failure is caused. In addition, the existing modification means mostly adopt single organic silicon modification or filler modification, the modification effect is limited, the cooperative promotion of temperature resistance, corrosion resistance and mechanical properties is difficult to realize, and the mechanical properties of the material are reduced after the temperature resistance and corrosion resistance are improved by a partial modification scheme. The problem of dispersibility of the filler in the resin matrix is not solved effectively, and the filler which is not subjected to surface treatment is easy to agglomerate, so that the material performance is unevenly distributed. Meanwhile, the traditional curing process mostly adopts constant temperature curing, so that the material is easy to generate internal stress, the compactness of a crosslinked network is insufficient, and the comprehensive performance of the material is further influenced, so that the research and development of the solid epoxy resin composite material with excellent temperature resistance and corrosion resistance and good comprehensive mechanical property becomes an urgent requirement for industry development. Disclosure of Invention The invention aims at providing a temperature-resistant corrosion-resistant solid epoxy resin composite material and a preparation method thereof. The invention further aims to provide a temperature-resistant and corrosion-resistant solid epoxy resin composite material which comprises, by weight, 30-70 parts of an epoxy resin matrix, 6-24 parts of an aromatic curing agent, 3-17 parts of an organosilicon modifier, 6-30 parts of fly ash, 4-10 parts of montmorillonite, 0.6-2.4 parts of a silane coupling agent, 0.3-1.2 parts of 2-ethyl-4-methylimidazole, 0.3-0.8 part of triphenylphosphine and 0.05-0.8 part of an antioxidant 1010, wherein the epoxy resin matrix is at least one of bisphenol A epoxy resin and bisphenol F epoxy resin; the aromatic curing agent is at least one of 4,4 '-diamino diphenyl sulfone and 4,4' -diamino diphenyl ether, the organosilicon modifier is at least one of polydimethylsiloxane and hydroxyethoxy polysiloxane, and the silane coupling agent is at least one of KH-550 and KH-560. Preferably, the method further comprises at least one of 0-4 parts of graphene and 0-1.5 parts of carbon black by weight. Preferably, the epoxy resin matrix is a mixture of bisphenol A epoxy resin and bisphenol F epoxy resin, and the silane coupling agent is a mixture of KH-550 and KH-560. Preferably, when the aromatic curing agent is 4,4 '-diaminodiphenyl sulfone, the organosilicon modifier is polydimethylsiloxane, and when the aromatic curing agent is 4,4' -diaminodiphenyl ether, the organosilicon modifier is hydroxyethoxy polysiloxane. The preparation method of the temperature-resistant corrosion-resistant solid epoxy resin composite material comprises the following steps: Firstly, pretreating a filler, namely mixing fly ash, montmorillonite and optional graphene, adding a silane coupling agent, stirring for 25-55 minutes at 70-100 ℃, then placing the mixture at 100-130 ℃ for drying for 1.5-3.5 hours, cooling to room temperature, crushing, and sieving with a 90-130 mesh sieve to obtain a modified composite filler; Step two, resin modification, namely placing an epoxy resin matrix into a reaction kettle, heating to 70-100 ℃, stirring at a rotating speed of 180-270r/min, slowly adding an organosilicon modifier, and stirring at a constant temperature