Synthesis method of dimer acid glycidyl ester
The technology of a glycidyl ester and a synthesis method is applied in the synthesis field of glycidyl dimer acid, can solve the problems to be further improved and the like, and achieves the effects of stable product index, high epoxy value and low hydrolysis chlorine
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Embodiment 1
[0019] Add 178g of dimer acid, 569g of epichlorohydrin and 2.5g of NaOH into a 1L reaction flask, stir, raise the temperature to 90°C, and maintain the reaction temperature at 90°C for 2h to obtain an intermediate with a chlorohydrin ester structure, and continue to add 2.67g of benzyltrimethylammonium chloride, then raise the vacuum of the system to 140torr, control the temperature at 65°C, and add 53.36g of 50% NaOH solution dropwise at a constant speed within 3 hours. After the dropwise addition, continue at this temperature The reaction was stirred for 1 hour. After the reaction was completed, break the vacuum, add 200g of 80°C deionized water, stir for 5 minutes and let stand, separate liquid to remove salt, remove excess unreacted epichlorohydrin, and filter to obtain 202g of dimer acid glycidyl ester. Epoxy equivalent 412g / eq, hydrolyzed chlorine 3850ppm.
Embodiment 2
[0021] Add 178g of dimer acid, 569g of epichlorohydrin and 5g of NaOH into a 1L reaction flask, stir, raise the temperature to 85°C, and maintain the reaction temperature at 85°C for 4h to obtain an intermediate with a chlorohydrin ester structure, and continue to add 5.34g to the system Benzyltriethylammonium chloride, then raise the vacuum degree of the system to 140torr, control the temperature at 65°C, add 49.48g of 50% NaOH solution dropwise at a constant speed within 2 hours, and continue to stir the reaction at this temperature after the dropwise addition is completed 1 hour. After the reaction, break the vacuum, add 200g of 80°C deionized water, stir for 5 minutes and let it stand, then separate the liquid to remove the salt and excess unreacted epichlorohydrin, and filter to obtain 196g of dimer acid glycidyl ester. Epoxy equivalent 425g / eq, hydrolyzed chlorine 4542ppm.
Embodiment 3
[0023] Add 178g of dimer acid, 569g of epichlorohydrin and 5g of KOH into a 1L reaction bottle, stir, raise the temperature to 90°C, and maintain the reaction temperature at 90°C for 2h to obtain an intermediate with a chlorohydrin ester structure, and continue to add 2.67g to the system Tetramethylammonium bromide, then raise the vacuum degree of the system to 130torr, control the temperature at 60°C, add 48.13g of 50% NaOH solution dropwise at a constant speed within 2 hours, after the dropwise addition, continue to stir and react at this temperature for 1 hour . After the reaction is complete, break the vacuum, add 200g of 80°C deionized water, stir for 5 minutes and let stand, separate liquid to remove salt, remove excess unreacted epichlorohydrin, and filter to obtain 198g of dimer acid glycidyl ester. The epoxy equivalent is 436g / eq, and the hydrolyzed chlorine is 5210ppm.
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Abstract
Description
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