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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.

Pending Publication Date: 2021-09-03
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that carbon tetrachloride is an internationally prohibited reagent, does not meet the requirements of green production, and cannot be used for industrialized production;
[0007] The third method: gas-phase ethylene carbonate is prepared by high-temperature cracking. The disadvantage of this method is that the reaction conditions are harsh, the yield is low, and the requirements for equipment are very high, which is not conducive to industrial production;
[0008] The fourth type: gas-phase ethylene carbonate is prepared by oxidation at high temperature. The disadvantages of this method are low yield, high equipment requirements, poor controllability and repeatability

Method used

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preparation example Construction

[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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Abstract

The invention belongs to the field of synthesis of vinylene carbonate, and particularly relates to a preparation method of vinylene carbonate. The method comprises the following steps: 1) carrying out hydrogen chloride elimination reaction on chloroethylene carbonate and excessive triethylamine in the presence of a polymerization inhibitor without a solvent, and carrying out solid-liquid separation to obtain a reaction solution containing triethylamine; and 2) distilling the reaction solution containing triethylamine, and separating out unreacted triethylamine and vinylene carbonate in sequence. According to the preparation method of the vinylene carbonate, the hydrogen chloride elimination reaction is carried out under the solvent-free condition, so that the subsequent solvent removal is reduced; the reaction solution containing triethylamine is a vinylene carbonate crude product, the unreacted triethylamine and the product can be obtained through distillation, rectification is not needed, and the yield and the purity of the product are high. The whole process is low in environmental pollution, high in operability, high in production safety, low in input cost and very suitable for industrial production.

Description

technical field [0001] The invention belongs to the synthesis field of vinylene carbonate, and in particular relates to a preparation method of vinylene carbonate. Background technique [0002] Vinylene carbonate, also known as 1,3-dioxol-2-one or ethylene carbonate, is a colorless and transparent liquid, an important intermediate in organic synthesis, and an electrolyte for lithium-ion batteries Additives can significantly prolong the cycle life of lithium-ion batteries and improve the storage resistance of batteries. [0003] At present, the main methods of producing vinylene carbonate are as follows: [0004] The first: take ethylene carbonate and thionyl chloride as raw materials, carbon tetrachloride as a solvent, trigger under light to prepare chloroethylene carbonate, and then use chloroethylene carbonate and triethylamine as raw materials, Ester solvents are used as solvents to prepare vinylene carbonate. The disadvantage of this method is that carbon tetrachlorid...

Claims

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Application Information

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IPC IPC(8): C07D317/40C01B7/01C01B11/06
CPCC07D317/40C01B7/012C01B11/06
Inventor 李云峰薛旭金张照坡杨华春薛峰峰辛婉婉李喜毋文彦
Owner DO FLUORIDE CHEM CO LTD
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