Preparation method of vinylene carbonate
A technology of vinylene carbonate and chloroethylene carbonate, which is applied in the field of preparation of vinylene carbonate, and can solve the problems of high equipment requirements, non-compliance with green production requirements, and inability to use industrialized production.
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[0022] The present invention relates to the preparation method of vinylene carbonate. Considering the industrial indicators such as yield, it is the most effective production process to prepare vinylene carbonate with (mono) chloroethylene carbonate (CEC) and triethylamine by eliminating hydrogen chloride reaction.
[0023] In the process of eliminating hydrogen chloride, chloroethylene carbonate removes HCl to generate vinylene carbonate (VC), thereby realizing the introduction of double bonds in the carbonate ring. The generated HCl will generate triethylamine hydrochloride with a large amount of triethylamine, which will be precipitated from the reaction solution.
[0024] VC is easily oxidized, even if a polymerization inhibitor is added, some products will be oxidized and deteriorated. In the present invention, triethylamine is used in excess, that is, as a raw material and as a "solvent", and no other solvents are added for the reaction.
[0025] (1) Elimination of hyd...
Embodiment 1
[0043] The preparation method of the vinylene carbonate of the present embodiment may further comprise the steps:
[0044] (1) Synthesis of chloroethylene carbonate (ClEC): Replace the microchannel reactor system with nitrogen, turn on the ultraviolet lamp, and pass ethylene carbonate and chlorine gas (the molar ratio of ethylene carbonate to chlorine gas is 1:1.2) into the microchannel reactor system. In the channel reactor, the reaction temperature is 30°C, and the residence time is 0.5min. The generated chloroethylene carbonate containing hydrogen chloride gas is transferred to the reaction kettle, and nitrogen gas is passed from the bottom of the kettle to replace the residual hydrogen chloride gas. into the synthesis kettle.
[0045] The generated hydrogen chloride gas and excess chlorine gas are absorbed through two-stage water absorption and one-stage sodium hydroxide solution to obtain by-product hydrochloric acid and sodium hypochlorite.
[0046] (2) synthesis of vin...
Embodiment 2
[0050] The preparation method of the vinylene carbonate of the present embodiment may further comprise the steps:
[0051] (1) Synthesis of chloroethylene carbonate (ClEC): Use nitrogen to replace the microchannel reactor system, turn on the ultraviolet lamp, and pass ethylene carbonate and chlorine gas (the molar ratio of ethylene carbonate to chlorine gas is 1:1.5) into the microchannel reactor system. In the channel reactor, the reaction temperature is 50°C, and the residence time is 1min. The generated chloroethylene carbonate containing hydrogen chloride gas is transferred to the reaction kettle, and nitrogen gas is passed from the bottom of the kettle to replace the residual hydrogen chloride gas. After the replacement, it is transferred to in the reactor.
[0052] (2) synthesis of vinylene carbonate (VC): chloroethylene carbonate is fed into the synthesis kettle, 1% of BHT is added, and at 40°C, 220% of triethylamine is added, after the reaction is completed, centrifuge...
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