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Method for preparing perfluoromethyl isobutyrate by electrochemical fluorination

A perfluoromethyl isobutyrate, electrochemical technology, applied in the direction of electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of difficult operation, complicated distillation and purification process, large proportion of by-products, etc., and achieve reaction selection The effect of good performance, high yield, and no isomer by-products

Active Publication Date: 2018-08-24
昊华气体有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrochemical fluorination reaction with isobutyric anhydride as the substrate has poor selectivity, large proportion of by-products, complex distillation and purification process, difficult operation, and directly affects the product yield of methyl perfluoroisobutyrate

Method used

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  • Method for preparing perfluoromethyl isobutyrate by electrochemical fluorination
  • Method for preparing perfluoromethyl isobutyrate by electrochemical fluorination

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Put 800g of methacrylic anhydride into an electrochemical reactor containing 10kg of anhydrous hydrogen fluoride at 0°C, control the operating voltage of the electrochemical reactor to 4.5V-5.0V, and the current density at 5-10mA / cm 2 , the system temperature was maintained at 0-5°C. During the reaction process, the gaseous product generated was passed through the gas phase outlet of the reactor, and slowly passed into a reaction kettle containing 1L of methanol and 530g of anhydrous sodium fluoride, and fully reacted for 3 hours at room temperature. After the reaction was finished, the reaction solution was filtered, and the unreacted methanol was removed by distillation from the obtained filtrate, leaving 1055 g of colorless and transparent liquid methyl heptafluoroisobutyrate. The product was characterized by gas chromatography and no methyl heptafluoro-n-butyrate by-product was detected. The purity of methyl heptafluoroisobutyrate is 90.41%, the reaction selectivity...

Embodiment 2

[0022] Put 1kg of methacrylic acid into the electrochemical reactor containing 17kg of anhydrous hydrogen fluoride at 0°C, control the operating voltage of the electrochemical reactor to 5.0V-10V, and the current density at 25-30mA / cm 2 , the system temperature was maintained at 0-5°C. During the reaction process, the gaseous product produced was passed through the gas phase outlet of the reactor, and slowly passed into a reaction kettle containing 1L of methanol and 595g of anhydrous sodium fluoride, and fully reacted for 3 hours at room temperature. After the reaction, the reaction liquid was filtered, and the unreacted methanol was removed by distillation from the obtained filtrate, leaving 1105g of colorless and transparent liquid methyl heptafluoroisobutyrate, and the product was characterized by gas chromatography without detecting the by-product of methyl heptafluorobutyrate , purity 91.22%, reaction selectivity 38.05%, product yield 38.05%. 1 H NMR (500 MHz, CDCl 3 )...

Embodiment 3

[0024] Put 500g of methacryloyl chloride into an electrochemical reactor containing 5kg of anhydrous hydrogen fluoride at 0°C, control the operating voltage of the electrochemical reactor to 6.0V-10V, and the current density at 15-30mA / cm 2 , the system temperature was maintained at -10 to 1°C. During the reaction process, the gaseous product generated was passed through the gas phase outlet of the reactor, and slowly passed into a reaction kettle containing 1L of methanol and 250g of anhydrous sodium fluoride, and fully reacted for 2 hours at room temperature. After the reaction, the reaction liquid was filtered, and the obtained filtrate was distilled to remove unreacted methanol, leaving 458g of colorless and transparent liquid methyl heptafluoroisobutyrate, and the product was characterized by gas chromatography without detecting methyl heptafluoro-n-butyrate as a by-product , purity 93.03%, reaction selectivity 39.06%, product yield 39.06%. 1 H NMR (500 MHz, CDCl 3 )δ4....

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Abstract

The invention discloses a method for preparing perfluoromethyl isobutyrate by electrochemical fluorination. The method comprises the following steps: taking methylacrylic acid and a derivative thereofas a starting material; carrying out electrochemical fluoridation on the starting material and hydrogen fluoride in an electrochemical reactor to obtain a gaseous product; feeding the obtained gaseous product in a methanol solution and fully reacting and esterifying; and distilling reaction liquid to collect the product. Methacrylic anhydride and the derivative thereof are used as the raw material, and the problem that isobutyric anhydride is isomerized in an electrochemical fluorination process is solved. The method has the characteristics of good reaction selectivity, zero isomer by-productand high yield.

Description

technical field [0001] The invention relates to a preparation method of methyl perfluoroisobutyrate, in particular to an electrochemical fluorination method. Background technique [0002] Methyl perfluoroisobutyrate is a key intermediate in the synthesis of perfluoroisobutyronitrile. Perfluoroisobutyronitrile is a new type of environmentally friendly insulating gas material, which can be used as a dielectric composition for electrical equipment insulators. In recent years, it has attracted extensive attention from major electrical companies and research institutions around the world. [0003] [0004] Methyl perfluoroisobutyrate is not available commercially, and needs to be synthesized by itself. 3M’s patented US 2015 / 0083979Al process for preparing methyl perfluoroisobutyrate is as follows: use isobutyric anhydride as the starting material, and prepare perfluoroisobutyryl fluoride by electrochemical fluorination with hydrogen fluoride in an electrochemical reactor , a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/08C25B3/28
CPCC25B3/28
Inventor 宋新巍黄晓磊任章顺牛鹏飞张金彪牛学坤鲍金强吴旭飞苏镇西刘伟张松林
Owner 昊华气体有限公司
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