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Preparation method of high temperature resistant single-component solventless epoxy adhesive

An epoxy adhesive, one-component technology, applied in the direction of adhesive types, epoxy resin adhesives, adhesives, etc., can solve the problems of inability to meet high temperature conditions, endanger human health, low bonding strength, etc., and achieve cost-effective Low, easy to operate, excellent bonding performance

Inactive Publication Date: 2012-12-12
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are also some problems in the epoxy resin adhesive system: (1) solvent type: the volatilization of the solvent pollutes the environment and endangers human health; (2) solvent-free type: high viscosity, poor manufacturability, and partial bonding strength Low; low heat resistance, can not meet the application under high temperature conditions

Method used

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  • Preparation method of high temperature resistant single-component solventless epoxy adhesive
  • Preparation method of high temperature resistant single-component solventless epoxy adhesive
  • Preparation method of high temperature resistant single-component solventless epoxy adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 36.6 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BAHPFP), 414.4 grams (0.8 moles) of 2,2-bis[4-(4-aminophenoxy Base) phenyl] hexafluoropropane (BAPOPFP) and 3045 milliliters of N-methyl-2-pyrrolidone solvent are added in the reaction kettle, stirred at room temperature, after completely dissolving, add 310.0 grams (1.0 mole) 3,3 ', 4, 4'-tetracarboxylic acid diphenyl ether dianhydride (ODPA) powder, after stirring at room temperature to dissolve completely, continue to react for 4 hours, add 6090 milliliters of toluene entrainer and 0.05 mole of 4-methylbenzenesulfonic acid catalyst, heat up, After 6 hours of reflux and water separation reaction in the temperature range of 120°C to 150°C, the reaction solution was concentrated, cooled to room temperature, and the reaction solution was slowly added to a high-speed (5000r / min-10000r / min ) in the crushing kettle under stirring state, separate out solid powder, filter, wash 2-3 times with deioniz...

Embodiment 2

[0049] Add 100.0 grams of ES216 epoxy resin, 8.0 grams of white thermoplastic polyimide HPI-1 powder, and 0.1 grams of 2-ethyl-4-methylimidazole into the reaction bottle, and heat up to a temperature of 100°C-120°C The reaction was carried out for 1-2 hours to obtain a viscous imine toughened modified epoxy resin system. Add 80.0 grams of 3,4-epoxycyclohexanecarboxylic acid-3',4'-epoxycyclohexane methyl ester reactive diluent, 10.0 grams of Dicyandiamide latent curing agent, stir evenly to obtain high temperature resistant one-component solvent-free epoxy adhesive.

[0050] Take an appropriate amount of the adhesive obtained above, and evenly spread it on a standard steel test piece. Cool to room temperature.

[0051] The adhesive system has good viscosity controllability, can be adjusted in a wide range, has good manufacturability, and has excellent bonding performance to metal substrates (such as steel, etc.). The specific test results are as follows:

[0052] Steel-steel...

Embodiment 3

[0055] 25.8 grams (0.1 moles) of 2,2-bis(3-amino-4-hydroxyphenyl)propane (BAHPP), 123.0 grams (0.3 moles) of 2,2-bis[4-(4-aminophenoxy) Phenyl] propane (BAPOPP) and 2728 milliliters of N, N-dimethylacetamide solvent are added in the reaction kettle, stirred at room temperature, after completely dissolving, add 124.0 grams (0.4 mol) 3,3',4,4'- Tetracarboxylic diphenyl ether dianhydride (ODPA) powder, after stirring and dissolving completely at room temperature, continue to react for 2 hours, add 275 milliliters of xylene entrainer and 0.08 mole of 4-methylbenzenesulfonic acid catalyst, heat up, at 120 After reflux and water separation reaction in the temperature range of ℃~150℃ for 12 hours, concentrate the reaction solution, cool to room temperature, slowly add the reaction solution to a high-speed (5000r / min-10000r / min) stirring solution containing 2728 ml of ethanol precipitant In the crushing still under state, separate out solid powder, filter, wash 2-3 times with deionize...

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Abstract

The invention relates to a preparation method of high temperature resistant single-component solventless epoxy adhesive. The method comprises the following steps: adding aromatic binary primary amine and strongly polar non-proton organic solvent in a reaction tank, stirring at room temperature to dissolve, adding aromatic binary acid anhydride to perform refluxing and water-segregating reaction at 120-150 DEG C for 6-12h, cooling, adding the reaction solution in a stamp tank with precipitant to precipitate solid powder, namely white thermoplastic polyimide powder, adding white thermoplastic polyimide powder and tertiary amine compound or imidazole compound in epoxy resin to react for 1-2h, adding active diluent and latent curing agent to stir evenly and obtaining the product. The production process is easy and the cost is low so as to realize industrialized production; the tensile shear intensions of the epoxy adhesive at room temperature and 120 DEG C are respectively up to 28Mpa and26Mpa and the epoxy adhesive has broad application prospect in fields such as electronics and microelectronics, electrical motors, aviation and aerospace and the like.

Description

technical field [0001] The invention belongs to the field of preparation of epoxy adhesives, in particular to a preparation method of high-temperature-resistant single-component solvent-free epoxy adhesives. Background technique [0002] As we all know, epoxy resin has many excellent properties: (1) Good bonding performance: high bonding strength, wide bonding surface, it is compatible with many metals (such as iron, steel, copper, aluminum, metal alloys, etc.) The bonding strength of metal materials (such as glass, ceramics, wood, plastics, etc.) is very high, and some even exceed the strength of the bonded material itself, so it can be used in many stressed structural parts and is the main component of structural adhesives One; (2) good processing performance: the flexibility of epoxy resin formula, the diversity of processing technology and product performance are the most prominent among polymer materials; (3) good stability performance: the curing of epoxy resin is main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J163/00C09J179/08C08G73/10
Inventor 虞鑫海
Owner DONGHUA UNIV
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