A kind of epoxy curing agent and its preparation method, epoxy resin composition and its preparation method and application
An epoxy curing agent and epoxy resin technology, applied in the direction of epoxy resin coatings, coatings, etc., can solve problems such as difficult to control, low solid content, easy blackening and mildew, etc., to meet the requirements of fast surface drying and amine odor Lightweight, fast dry time effect
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Embodiment 1
[0105] (1) Preparation of epoxy curing agent
[0106] 1) Under nitrogen protection, react piperazine and acrylonitrile in methanol at a molar ratio of 1:1 at 60°C for 5 hours to obtain reaction intermediate I;
[0107] 2) In the high-pressure reaction kettle, first replace the air in the kettle with nitrogen for 3 times, and then use hydrogen for 3 times to replace the nitrogen in the kettle; then pressurize the hydrogen to 5MPa, heat up to 100°C, and add the prepared Reaction intermediate I, react until the pressure drops to 1MPa and complete the hydrogenation reaction to obtain reaction intermediate II;
[0108] 3) The prepared reaction intermediate II is subjected to rotary steaming to remove methanol, the condition of rotary steaming is that the temperature is 70°C, and the vacuum pressure is 20KPa; atmospheric distillation removes piperazine, and the condition of atmospheric distillation is a rectifying column The temperature is controlled at 150°C; finally, the target p...
Embodiment 2
[0116] (1) Preparation of epoxy curing agent
[0117] 1) Under nitrogen protection, react piperazine and acrylonitrile in methanol at a molar ratio of 1:1.1 at 50°C for 6 hours to obtain reaction intermediate I;
[0118] 2) In the high-pressure reaction kettle, first use nitrogen to blow 3 times to replace the air in the kettle, then use hydrogen to blow 3 times to replace the nitrogen in the kettle; then pressurize the hydrogen to 5MPa, raise the temperature to 110°C, and add Reaction intermediate I, react until the pressure drops to 1MPa and complete the hydrogenation reaction to obtain reaction intermediate II;
[0119] 3) The prepared reaction intermediate II is subjected to rotary steaming to remove methanol, the condition of rotary steaming is that the temperature is 80°C, and the vacuum pressure is 25KPa; atmospheric distillation removes piperazine, and the condition of atmospheric distillation is rectification column The temperature is controlled at 160°C; finally, th...
Embodiment 3
[0127] (1) Preparation of epoxy curing agent
[0128] 1) Under nitrogen protection, react piperazine and acrylonitrile in methanol at a molar ratio of 1:1 at 55°C for 5 hours to obtain reaction intermediate I;
[0129] 2) In the high-pressure reaction kettle, first use nitrogen to blow the air in the replacement kettle for 3 times, and then use hydrogen to blow the nitrogen in the replacement kettle for 3 times; Reaction intermediate I, react until the pressure drops to 1MPa and complete the hydrogenation reaction to obtain reaction intermediate II;
[0130] 3) The prepared reaction intermediate II is subjected to rotary steaming to remove methanol, the condition of rotary steaming is that the temperature is 60°C, and the vacuum pressure is 20KPa; atmospheric distillation removes piperazine, and the condition of atmospheric distillation is a rectifying column The temperature is controlled at 150°C; finally, the target product aminopropylpiperazine is obtained after vacuum dis...
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Abstract
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