Preparation method for difluoroethylene carbonate
A technology of bisfluoroethylene carbonate and vinylene carbonate, which is applied in the field of preparation of bisfluoroethylene carbonate, can solve the problems of high processing cost, cumbersome processing, and low yield, achieve high purity and create economic benefits , the effect of high yield
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[0017] The preparation method of bisfluoroethylene carbonate is described in detail below.
[0018] The preparation method of bisfluoroethylene carbonate comprises the following steps.
[0019] 1. Addition reaction: add the forward distillation of vinylene carbonate and organic solvent in the first reaction kettle, stir so that the forward distillation of vinylene carbonate and the organic solvent are completely miscible, and the vinylene carbonate in the forward distillation of vinylene carbonate The mass fraction of vinyl ester is 30% to 60%. Nitrogen is passed through. The function of nitrogen is to isolate the reactants from air and water, heat to 20-50°C, and add liquid bromine or chlorine gas to carry out the addition reaction. The dropping rate of liquid bromine is 12 drops / minute, and the flow rate of chlorine gas is 0.1 to 0.5 liters / minute when chlorine gas is introduced. After the reaction is completed, solvent removal (recover the solvent for future use), refining...
Embodiment 1
[0025] One, addition reaction: in the first reaction kettle, add the forward distillation of vinylene carbonate and organic solvent, wherein the quality of the forward distillation of vinylene carbonate is 143.42g, the massfraction of vinylene carbonate is 60%, carbonic acid Vinylene is 1 mol; the organic solvent is dimethyl carbonate, the mass is 1000 g, and the water content is 8.2 ppm. Stir to make the forward distillate of vinylene carbonate miscible with the organic solvent completely, pass nitrogen gas, heat to 25°C, add liquid bromine (1.1mol, 175.791g) dropwise, the dropping rate of liquid bromine is 12 drops / min, carry out Addition reaction. After the reaction, precipitation and refining were carried out, and the whole process of refining was under nitrogen protection to obtain pure bisbromoethylene carbonate (239.56 g, yield 97.45%, purity 99.01%). Put the pure product of bisbromoethylene carbonate into the second reaction kettle for subsequent use.
[0026] 2. Sub...
Embodiment 2
[0029] One, addition reaction: in the first reaction kettle, add the forward distillation of vinylene carbonate and organic solvent, wherein the quality of the forward distillation of vinylene carbonate is 172.10g, the massfraction of vinylene carbonate is 50%, carbonic acid Vinylene is 1 mol; the organic solvent is diethyl carbonate, the mass is 500 g, and the water content is 5.3 ppm. Stir to make the front distillation of vinylene carbonate and diethyl carbonate miscible completely, pass nitrogen gas, heat to 30°C, pass chlorine gas (1.3mol, 92.3g), and the flow rate of chlorine gas is 0.3 liters / minute to carry out addition reaction . After the reaction, precipitation and refining were carried out, and nitrogen protection was used throughout the refining process to obtain pure dichloroethylene carbonate (153.50 g, yield 97.80%, purity 99.10%). Put the pure product of dichloroethylene carbonate into the second reaction kettle for standby.
[0030] 2. Substitution reaction...
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