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Synthesis method of cycloethane carbonate

A technology of cycloethane carbonate and a synthesis method, applied in the chemical industry, can solve the problems of high price, large amount of catalyst, long reaction time and the like, and achieve the effects of low price, high product yield and good stability

Pending Publication Date: 2022-07-15
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After the catalyst was circulated five times, the catalyst activity dropped from 94.4% to 91.4% in the first reaction. There were problems such as long reaction time, large amount of catalyst, and high price, and the activity of the catalyst still needs to be further improved.

Method used

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  • Synthesis method of cycloethane carbonate
  • Synthesis method of cycloethane carbonate
  • Synthesis method of cycloethane carbonate

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preparation example Construction

[0028] The invention provides a method for synthesizing cycloethane carbonate, and the process flow refers to figure 1 , the method specifically includes the following steps:

[0029] (1) catalyst preparation: the alkali metal alkoxide is dissolved in raw material ethylene glycol or methanol to prepare a catalyst material;

[0030] (2) transesterification reaction: the ethylene glycol material 1 enters the reactive distillation column R1 through the ethylene glycol delivery pump A1 and the ethylene glycol delivery pump outlet pipeline 4, and the dimethyl carbonate material 2 passes through the dimethyl carbonate The delivery pump A2 and the dimethyl carbonate delivery pump outlet pipeline 5 enter the reactive distillation column R1, and the catalyst material passes through the catalyst configuration device outlet pipeline 3, the catalyst and ethylene glycol mixed solution delivery pump A3 and the catalyst delivery pump outlet pipeline 6 enter the reactive distillation column ...

Embodiment 1

[0036] use figure 1 As shown in the synthetic process of cycloethane carbonate, 10g of ethylene glycol and 14.5g of dimethyl carbonate were weighed to form a raw material solution, mixed evenly, and then added to the bottom of the reactive distillation column, raised to 70°C, and then added with 113mg of methanol Potassium began to react for 60 minutes after the reaction, and the liquid phase material was taken for qualitative and quantitative analysis by gas chromatography. The conversion rates of DMC and EG were 66.2% and 64.6%, and the selectivity of EC and ME were 92.2% and 99.8%, respectively.

Embodiment 2

[0038] use figure 1 As shown in the synthetic process of cycloethane carbonate, 10g of ethylene glycol and 14.5g of dimethyl carbonate were weighed to form a raw material solution, mixed evenly, and then added to the bottom of the reactive distillation column, raised to 60°C, and then added with 113mg of methanol Potassium began to react for 15 minutes after the reaction, and the liquid phase material was taken for qualitative and quantitative analysis by gas chromatography. The conversion rates of DMC and EG were 66.8% and 65.2%, and the selectivities of EC and ME were 92.3% and 99.8%, respectively.

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Abstract

According to the synthetic method, a reactive distillation tower is used as a reaction place, dimethyl carbonate and ethylene glycol are continuously subjected to ester exchange in the reactive distillation tower under the action of a catalyst, methanol is obtained at the top of the tower, and a mixture of the ethylene glycol, the cyclohexane carbonate and the catalyst is extracted from the bottom of the tower. And recycling the catalyst, separating and refining the cyclohexane carbonate, and recycling the ethylene glycol. Compared with the prior art, the method provided by the invention has the advantages of simple catalyst and product separation process flow, high production continuity degree, suitability for large-scale production and equipment cost saving.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a method for synthesizing cycloethane carbonate. Background technique [0002] Cycloethane carbonate (EC) is an excellent solvent and organic synthesis intermediate, which is widely used in battery electrolytes, ester intermediates, fibers, pharmaceuticals and organic synthesis industries. The synthesis methods of EC include phosgene method, urea alcoholysis method, ethylene oxide and carbon dioxide addition method, etc. The phosgene method is the earliest industrialized method for preparing cycloethane carbonate, but it has been eliminated due to its high toxicity and serious environmental pollution. The urea alcoholysis method still has problems such as urea decomposition and difficult recovery of catalysts, and it is still in the research stage. In the ethylene oxide method, the atomic utilization rate of ethylene oxide and carbon dioxide reaches 100%, which is the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/38C07C29/128C07C29/80C07C31/04
CPCC07D317/38C07C29/1285C07C29/80C07C31/04Y02P20/10
Inventor 刘成伟迟子怡阎建民李学刚肖文德
Owner SHANGHAI JIAO TONG UNIV
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