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Preparation method of vinylene carbonate

A technology of vinylene carbonate and chloroethylene carbonate, applied in the field of preparing vinylene carbonate, can solve the problem of low yield of target product vinylene carbonate, low flash point of ether compounds, difficulty in purifying vinylene carbonate, etc. It is beneficial to large-scale industrial production, accelerates the reaction speed, and is easy to separate and purify.

Inactive Publication Date: 2014-05-21
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main defects are: one, the reaction time is long; two, ether compounds have a low flash point, which is easy to form peroxides in the process of transportation and storage, resulting in hidden dangers; three, the yield of the target product vinylene carbonate is too low
However, the melting point of ethylene carbonate is as high as 37°C, which brings great difficulty to the later rectification and purification of vinylene carbonate.

Method used

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  • Preparation method of vinylene carbonate
  • Preparation method of vinylene carbonate
  • Preparation method of vinylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A 250mL there-necked flask equipped with a stirring device was flushed with nitrogen, and 0.2 mol of dry ethylene monochlorocarbonate was added to the there-necked flask under nitrogen protection, and the temperature of the monochloroethylene carbonate in the there-necked flask was controlled at 40°C; Under stirring, 0.3 mol of redistilled triethylamine was added dropwise to ethylene monochlorocarbonate within 15 minutes through a dropping funnel. After the dropwise addition of triethylamine, the temperature was raised to 70°C, and the temperature was kept for 120 minutes. . The reaction was terminated to obtain a reaction solution containing vinylene carbonate.

[0029] The obtained reaction solution containing vinylene carbonate was filtered while hot, and the filter residue was washed three times with ethyl acetate. The filtrate was collected, and ethyl acetate and triethylamine were removed by rotary evaporator under the conditions of bath temperature of 55° C. and...

Embodiment 2

[0041] A 250mL three-necked flask equipped with a stirring device was flushed with nitrogen, and 0.2 mol of dry ethylene monochlorocarbonate (purity greater than 90%) was added to the three-necked flask under nitrogen protection to control the amount of monochloroethylene carbonate in the three-necked flask. The temperature is 43 ° C; under stirring, 1.0 mol of redistilled triethylamine is added dropwise to ethylene monochlorocarbonate within 45 minutes through a dropping funnel, and the temperature is raised to 50 °C after the triethylamine is added dropwise. °C and hold for 20 minutes. The reaction was terminated to obtain a reaction solution containing vinylene carbonate.

[0042] The obtained reaction solution containing vinylene carbonate was filtered while hot, and the filter residue was washed three times with ethyl acetate. The filtrate was collected, and ethyl acetate and triethylamine were removed by rotary evaporator under the conditions of bath temperature of 50° ...

Embodiment 3

[0046] A 250mL three-necked flask equipped with a stirring device was flushed with argon, and 0.2 mol of dry ethylene monochlorocarbonate (purity greater than 90%) was added to the three-necked flask under argon protection to control the amount of monochlorocarbonic acid in the three-necked flask. The temperature of vinyl ester is 45°C; under stirring, 0.6 mol of redistilled triethylamine is added dropwise to ethylene monochlorocarbonate within 30 minutes through a dropping funnel, and the temperature is raised after the addition of triethylamine is completed. to 60°C and held for 40 minutes. The reaction was terminated to obtain a reaction solution containing vinylene carbonate.

[0047] The obtained reaction solution containing vinylene carbonate was filtered while hot, and the filter residue was washed three times with ethyl acetate. The filtrate was collected, and ethyl acetate and triethylamine were removed by rotary evaporator under the conditions of bath temperature of 4...

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Abstract

The invention relates to a preparation method of vinylene carbonate. In the preparation method, monochloroethylene carbonate directly contacts with excessive triethylamine in the protection of inert gas for reaction, and no solvent is involved. In the preparation method of the present invention, triethylamine has two functions: the first one is that triethylamine is used as a dehydrochlorination reagent to participate in elimination reaction; the second one is that triethylamine is used as a solvent of dehydrochlorination reaction. The vinylene carbonate prepared by the preparation method of the invention has a yield of up to 93%, is easy to separate and purify, and has purity of up to more than 99%. The preparation method of the invention does not involve any other reaction solvent, and realizes full contact reaction of monochloroethylene carbonate with triethylamine; therefore, compared with traditional method, the preparation method of the invention is high in reaction speed, high in product yield, and suitable for large-scale industrial production. The vinylene carbonate prepared by the preparation method of the invention is applicable to various fields.

Description

technical field [0001] The invention relates to a method for preparing vinylene carbonate from monochloroethylene carbonate. Background technique [0002] Lithium-ion battery is a green new energy developed in the 1990s. This type of battery has occupied the dominant position in the current battery market due to its high energy density and high cycle performance. Vinylene carbonate is currently the most in-depth and effective organic film-forming additive for lithium-ion battery electrolytes. Since vinylene carbonate can form a polyalkyl lithium carbonate compound on the surface of the carbon negative electrode of the lithium ion battery, it can effectively inhibit the co-insertion reaction of solvent molecules, improve the cycle performance of the battery, and greatly prolong the life of the battery. In addition, vinylene carbonate can be used for the immobilization of biologically active substances such as enzymes after acting on the copolymer carrier, and at the same tim...

Claims

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Application Information

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IPC IPC(8): C07D317/40
CPCC07D317/40
Inventor 李超王雪松程学新张宝文
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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