Method for preparing fluoroethylene carbonate
A technology of fluoroethylene carbonate and chloroethylene carbonate, applied in the field of preparation of fluoroethylene carbonate, can solve problems such as poor selectivity, low conversion rate, difficult control, etc., achieve mild reaction conditions, improve reaction Yield, effect of reducing reaction time
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Embodiment 1
[0022] Add 120 g of sulfolane and 10 g of ethylene glycol dimethyl ether into a 1 L three-neck round bottom flask, then add 61 g of chloroethylene carbonate, and start stirring. After the temperature of the solvent system was raised to 79° C., 1 g of polyethylene glycol with a degree of polymerization of 400 was added to the mixture as a phase transfer catalyst, and the mixture was fully stirred for 10 minutes. Then gradually raise the temperature of the reaction system to 125°C, and add 15g, 10g and 10g of fluorinating agent respectively when reaching this temperature, 1 hour and 2 hours later, then maintain this temperature and continue the reaction for 8 hours to obtain fluorinated ethylene carbonate mixture of esters. The yield of fluoroethylene carbonate was 85.5%.
[0023] The mixture containing fluoroethylene carbonate was recrystallized twice, and then vacuum distillation was carried out under the vacuum condition of about -1.3kPa, and the fraction at 90-110°C was col...
Embodiment 2
[0025] Add 60 g of sulfolane and 70 g of diethylene glycol dimethyl ether into a 1 L three-neck round bottom flask, then add 61 g of chloroethylene carbonate, and start stirring. After the temperature of the solvent system was raised to 76° C., 2 g of polyethylene glycol with a degree of polymerization of 1000 was added to the mixture as a phase transfer catalyst, and the mixture was thoroughly stirred for 10 minutes. Then gradually raise the temperature of the reaction system to 132°C, and add 20g, 12g and 10g of fluorinating agent respectively when reaching this temperature, 1 hour and 2 hours later, then maintain this temperature and continue the reaction for 7 hours to obtain fluorinated ethylene carbonate mixture of esters. The yield of fluoroethylene carbonate was 88.7%.
[0026] The mixture containing fluoroethylene carbonate was recrystallized twice, and then vacuum distillation was carried out under the vacuum condition of about -1.3kPa, and the fraction at 90-110°C ...
Embodiment 3
[0028] Add 178g of triethylene glycol dimethyl ether into a 1L three-neck round bottom flask, then add 61g of chloroethylene carbonate, and start stirring. After raising the temperature of the solvent system to 72° C., 3 g of polyethylene glycol with a degree of polymerization of 800 was added to the mixture as a phase transfer catalyst, and the mixture was thoroughly stirred for 10 minutes. Then gradually raise the temperature of the reaction system to 140° C., and add 15 g, 15 g, and 10 g of fluorinating agent when reaching this temperature, 1 hour, and 2 hours later, and then maintain this temperature to continue the reaction for 6 hours to obtain fluorinated ethylene carbonate. mixture of esters. The yield of fluoroethylene carbonate was 88.5%.
[0029] The mixture containing fluoroethylene carbonate was recrystallized twice, and then subjected to vacuum distillation under a vacuum condition of about -1.3kPa to collect fractions at 90-110°C to obtain pure fluoroethylene c...
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