Preparing method of high-purity fluoroethylene carbonate
The technology of pure fluoroethylene carbonate and chloroethylene carbonate is applied in the field of preparation of high-purity fluoroethylene carbonate, which can solve the problems of high equipment requirements and low product purity, and achieves the reduction of impurity content, high purity, Process Control Simple Effects
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Embodiment 1
[0030] The preparation method of the high-purity fluoroethylene carbonate of the present embodiment, technological process is as follows figure 1 shown, including the following steps:
[0031] 1) 1 kg of chloroethylene carbonate raw material and anhydrous hydrogen fluoride liquid are passed into the microchannel reactor at the same time in a molar ratio of 1:1 for reaction, the reaction temperature is -15°C, and the reaction time is 7 minutes;
[0032] 2) Step 1) After the reaction is complete, transfer the reaction liquid and reaction gas to the tank reactor, and pass dry high-purity nitrogen gas to replace the hydrogen chloride gas in the tank reactor. The temperature in the reactor is controlled at -15°C, and the nitrogen gas The time is 3min;
[0033] 3) Step 2) After the replacement is complete, feed a fluorine-nitrogen mixed gas with a fluorine-containing gas volume content of 5% and react with unreacted chloroethylene carbonate. In the fluorine-nitrogen mixed gas, fluo...
Embodiment 2
[0041] The preparation method of the high-purity fluoroethylene carbonate of the present embodiment may further comprise the steps:
[0042] 1) Feed 1 kg of chloroethylene carbonate raw material and anhydrous hydrogen fluoride liquid into a microchannel crystallizer at the same time in a molar ratio of 1:1.1 for reaction, the reaction temperature is 0°C, and the reaction time is 10 minutes;
[0043] 2) Step 1) After the reaction is complete, transfer the reaction liquid and reaction gas to the tank reactor, and pass dry high-purity nitrogen gas to replace the hydrogen chloride gas in the tank reactor. The temperature in the reactor is controlled at 0°C, and the nitrogen gas The time is 10 minutes;
[0044] 3) Step 2) After the replacement is complete, feed a fluorine-nitrogen mixed gas with a fluorine-containing gas volume content of 5% and react with unreacted chloroethylene carbonate. In the fluorine-nitrogen mixed gas, fluorine and chloroethylene carbonate The molar ratio ...
Embodiment 3
[0052] The preparation method of the high-purity fluoroethylene carbonate of the present embodiment may further comprise the steps:
[0053] 1) Feed 1 kg of chloroethylene carbonate raw material and anhydrous hydrogen fluoride liquid into a microchannel crystallizer at the same time in a molar ratio of 1:1.15 for reaction, the reaction temperature is 16°C, and the reaction time is 25 minutes;
[0054] 2) Step 1) After the reaction is complete, transfer the reaction liquid and reaction gas to the tank reactor, and pass dry high-purity nitrogen gas to replace the hydrogen chloride gas in the tank reactor. The temperature in the reactor is controlled at 18°C, and the nitrogen gas The time is 10 minutes;
[0055] 3) Step 2) After the replacement is complete, feed a fluorine-nitrogen mixed gas with a fluorine-containing gas volume content of 10% and react with unreacted chloroethylene carbonate. In the fluorine-nitrogen mixed gas, fluorine and chloroethylene carbonate The molar ra...
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