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Method for preparing fluoro-carbonate ester by means of phase-transfer catalysis

A technology of phase transfer catalysis and fluorocarbonate, which is applied in the direction of organic chemistry, can solve the problems of high tar, low yield, low conversion rate and selectivity, and achieve easy-to-use, high reaction yield and stable catalyst Effect

Active Publication Date: 2013-01-16
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN101210005 has reported that adopt crown ether and polyethylene glycol compound as phase transfer catalyst, chloroethylene carbonate and sodium fluoride carry out halogen exchange reaction in solvent-free condition, generate fluoroethylene carbonate product, but this reaction produces More tar, resulting in very low yield, below 60%
Chinese patent CN101870687 has reported that adopting 18-crown-6 as phase transfer catalyst, chloroethylene carbonate carries out halogen exchange reaction with potassium fluoride in aprotic polar solvent, generates fluoroethylene carbonate product, but the conversion of this reaction The efficiency and selectivity are relatively low, only 80-85% of the raw materials react, the selectivity of the formed product is 75-85%, and the yield of the fluorination reaction is within 75%.
Chinese patent CN101597275 reports that quaternary ammonium salt compounds are used as phase transfer catalysts, and chlorocarbonate compounds and sodium fluoride undergo fluorination reaction to generate fluorocarbonate products, but the yield of this reaction is low, below 70%.

Method used

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  • Method for preparing fluoro-carbonate ester by means of phase-transfer catalysis
  • Method for preparing fluoro-carbonate ester by means of phase-transfer catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 700g of chloroethylene carbonate and 1200g of dimethyl carbonate to a 3000ml four-necked round bottom flask equipped with mechanical stirring, thermometer and reflux condenser, stir and mix well, then add 398g of solid KF and 18g of p-tert-butyl cup [4] Aromatics. Heating in an oil bath, the temperature was raised to 70° C. for 8 hours. The gas chromatography monitoring reaction result shows that 97.3% of chloroethylene carbonate reacts, the selectivity of fluoroethylene carbonate is 92.8%, and the yield of target product fluoroethylene carbonate reaches 90.3%.

Embodiment 2

[0029] Add 750g of chloroethylene carbonate and 1300g of diethyl carbonate to a 3000ml four-necked round-bottomed flask equipped with mechanical stirring, thermometer and reflux condenser. After mixing evenly, add 427g of solid KF and 29g of p-tert-butyl cup [6] Aromatics. Heated in an oil bath, and the temperature was raised to 110°C for 10 hours of reaction. The gas chromatography monitoring reaction results showed that 99.3% of the chloroethylene carbonate reacted, the selectivity of the fluorination reaction was 95.9%, and the yield of the target product fluoroethylene carbonate reached 95.2%.

Embodiment 3

[0031] In the four-neck round bottom flask that 2000ml is furnished with mechanical stirring, thermometer, reflux condenser, add 550g 4-chloro-5-methyl-1,3-dioxolan-2-ketone and 800g diethyl carbonate, After stirring and mixing, 315g of solid KF and 25g of p-hydrocalix[6]arene were added. Heated in an oil bath, and the temperature was raised to 100°C for 7 hours of reaction. The gas chromatography monitoring reaction result shows that 98.6% of 4-chloro-5-methyl-1,3-dioxolan-2-ketone reacts, and the selectivity of fluorination reaction is 96.2%, and target product 4-fluoro- The yield of 5-methyl-1,3-dioxolan-2-one reached 94.9%.

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Abstract

The invention discloses a method for preparing fluoro-carbonate ester by means of phase-transfer catalysis. The method includes the steps: taking chloro-carbonate ester as reaction raw materials; taking calixarene and derivatives as phase-transfer catalysts, wherein the mass ratio of the calixarene to the raw materials is 0.01-50%; and performing phase-transfer catalysis reaction in organic solvent and metal and ammonium fluorinating agent at the temperature ranging from 20 to 150 DEG C to generate the fluoro-carbonate ester. The method is simple in reaction process, high in reaction yield and easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fluorination reaction and relates to a method for preparing fluorocarbonate by phase transfer catalysis. Background technique [0002] The rapid development of lithium-ion secondary battery technology has occupied the largest market share in the fields of mobile phones, notebook computers, digital imaging equipment, and hand-held electric tools, and is expected to show explosive growth in the fields of electric bicycles and electric vehicles. With the expansion of lithium-ion battery application fields, users have also put forward higher requirements for its performance. Improving the safety and stability of batteries has become one of the current scientific research problems that need to be solved urgently. [0003] Fluorocarbonate compounds are a class of electrolyte additives with excellent performance, which can increase the boiling point and flash point of the solvent, reduce the freezing point an...

Claims

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Application Information

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IPC IPC(8): C07D317/42
Inventor 刘红光周立山叶学海郭西凤张洪源吴巍
Owner CHINA NAT OFFSHORE OIL CORP
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