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A kind of modified graphene oxide, mgo-sio 2 Nano-hybrid materials and mgo-sio 2 Preparation method of modified phenolic resin hot melt adhesive film

A nano-hybrid material, phenolic resin technology, applied in chemical instruments and methods, film/sheet adhesives, adhesives, etc., can solve problems such as no reported properties of phenolic resin hot-melt adhesive films, and achieve good compatibility and interface properties, low cost, high hydrophilicity

Active Publication Date: 2019-07-23
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, introducing nano-silica into the matrix can improve wear resistance, increase material toughness, improve tensile strength and impact strength, and heat resistance. However, there is no report in the prior art to improve phenolic resin by modifying graphene. Technology of Hot Melt Adhesive Film Properties

Method used

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  • A kind of modified graphene oxide, mgo-sio  <sub>2</sub> Nano-hybrid materials and mgo-sio  <sub>2</sub> Preparation method of modified phenolic resin hot melt adhesive film
  • A kind of modified graphene oxide, mgo-sio  <sub>2</sub> Nano-hybrid materials and mgo-sio  <sub>2</sub> Preparation method of modified phenolic resin hot melt adhesive film
  • A kind of modified graphene oxide, mgo-sio  <sub>2</sub> Nano-hybrid materials and mgo-sio  <sub>2</sub> Preparation method of modified phenolic resin hot melt adhesive film

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Effect test

Embodiment 1

[0045] The method for preparing modified graphene oxide of the present invention includes the following steps:

[0046] 1a) Weigh graphite oxide, ethanol A, catalyst, silane coupling agent, and ethanol B, then add graphite oxide to ethanol A, stir for 1 hour and then ultrasonically disperse for 2 hours to obtain a graphene oxide dispersion;

[0047] 2a) Add the catalyst to the graphene oxide dispersion obtained in step 1a) to obtain a mixed solution A;

[0048] 3a) Mix the silane coupling agent with ethanol B and stir for 30 minutes to obtain mixed solution B, then add mixed solution B to mixed solution A, and stir and react at 75°C for 12 hours, and then perform suction filtration and drying to obtain Modified graphene oxide;

[0049] Among them, the ratio of graphite oxide, ethanol A, catalyst, silane coupling agent, and ethanol B is 0.1 g: 50 mL: 0.05 g: 1.6 g: 20 mL.

[0050] The catalyst is dicyclohexylcarbodiimide.

[0051] The silane coupling agent is γ-aminopropyltriethoxysilane...

Embodiment 2

[0067] The method for preparing modified graphene oxide of the present invention includes the following steps:

[0068] 1a) Weigh graphite oxide, ethanol A, catalyst, silane coupling agent and ethanol B, then add graphite oxide to ethanol A, stir for 1 hour and then ultrasonically disperse for 2 hours to obtain a graphene oxide dispersion;

[0069] 2a) Add the catalyst to the graphene oxide dispersion obtained in step 1a) to obtain a mixed solution A;

[0070] 3a) Mix the silane coupling agent with ethanol B and stir for 30 minutes to obtain mixed solution B, then add mixed solution B to mixed solution A, and stir and react at 75°C for 12 hours, and then perform suction filtration and drying to obtain Modified graphene oxide;

[0071] Among them, the ratio of graphite oxide, ethanol A, catalyst, silane coupling agent, and ethanol B is 0.1 g: 50 mL: 0.05 g: 1.6 g: 65 mL.

[0072] The catalyst is triphenylphosphine.

[0073] The silane coupling agent is γ-(2,3-glycidoxy)propyltrimethoxysi...

Embodiment 3

[0089] The method for preparing modified graphene oxide of the present invention includes the following steps:

[0090] 1a) Weigh graphite oxide, ethanol A, catalyst, silane coupling agent and ethanol B, then add graphite oxide to ethanol A, stir for 3 hours and then ultrasonically disperse for 3 hours to obtain a graphene oxide dispersion;

[0091] 2a) Add the catalyst to the graphene oxide dispersion obtained in step 1a) to obtain a mixed solution A;

[0092] 3a) Mix the silane coupling agent with ethanol B and stir for 30 minutes to obtain mixed solution B, then add mixed solution B to mixed solution A, and stir and react at 60°C for 12 hours, and then perform suction filtration and drying to obtain Modified graphene oxide;

[0093] Among them, the ratio of graphite oxide, ethanol A, catalyst, silane coupling agent, and ethanol B is 0.1 g: 50 mL: 0.05 g: 1.5 g: 10 mL.

[0094] The catalyst is a mixture of dicyclohexylcarbodiimide and triphenylphosphine in a mass ratio of 1:1.

[0095...

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Abstract

The invention discloses a preparation method for modified graphene oxide, an MGO-SiO2 nano-hybrid material and an MGO-SiO2 modified phenolic resin hot melting adhesive film. The preparation method includes the following steps that (1c), the MGO-SiO2 nano-hybrid material is added into a solvent, then ultrasonic dispersion is performed, and MGO-SiO2 dispersion liquid is obtained; (2c), a film forming agent is added into a thermosetting phenolic resin solution, stirring is performed, and a mixed solution D is obtained; (3c), the MGO-SiO2 dispersion liquid obtained in the step (1c) is added into the mixed solution D obtained in the step (2c), stirring is performed so that the MGO-SiO2 dispersion liquid can be evenly dispersed in the mixed solution D, and a mixed solution E is obtained; and (4c), the mixed solution E is subjected to a vacuum constant-temperature stirring reaction at the temperature of 25-80 DEG C, a redundant solvent in the solution E is removed, when viscosity of reaction products is larger than or equal to a preset value, the reaction products are poured out, and the MGO-SiO2 modified phenolic resin hot melting adhesive film is obtained. The phenolic resin hot melting adhesive film prepared through the preparation method has excellent heat resistance and film forming performance, is low in cost, and can be applicable to a dry method prepreg forming process.

Description

Technical field [0001] The invention belongs to the technical field of phenolic resin preparation suitable for hot-melt prepreg technology, and relates to a modified graphene oxide, MGO-SiO 2 Nano hybrid materials and MGO-SiO 2 Preparation method of modified phenolic resin hot melt adhesive film. Background technique [0002] In the structure of traditional phenolic resin cured products, there are easily oxidized groups (phenolic hydroxyl, methylene), which affects its heat resistance. In addition, the poor processing performance of phenolic resin greatly limits its development. In addition, in the dry prepreg molding process, the phenolic resin film has the shortcomings of high brittleness and poor fiber wettability. The wet prepreg molding process commonly used in the industry is difficult to accurately control the resin content, high cost, and environmental pollution. Such drawbacks have severely restricted the development of high-performance composite materials. In order to m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J161/14C09J175/06C09J175/08C09J175/04C09J175/14C09J11/04C09J7/10C09C1/44C09C3/08C09C3/12C01B32/198
CPCC08K2201/011C08L2201/08C08L2205/025C08L2205/035C09C1/44C09C3/006C09C3/08C09C3/12C09J7/00C09J11/04C09J161/14C09J2461/00C09J2475/00C08L75/06C08K9/06C08K3/36C08K3/04C08L75/08C08L75/04C08L75/14C08L61/14
Inventor 刘育红井新利吕游姜雪雷子萱
Owner XI AN JIAOTONG UNIV