Perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride and preparation method thereof

A technology of dioxa and sulfonyl fluoride, which is applied in the field of perfluorosulfonyl fluoride and its preparation, can solve problems such as unfavorable industrial production, increased amount of "three wastes" and complicated procedures, so as to avoid advanced treatment and reduce Production volume, cost, and effect of simplification of operation process

Pending Publication Date: 2022-07-22
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Complicating the process, increasing the cost and energy consumption, and increasin

Method used

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  • Perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride and preparation method thereof
  • Perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride and preparation method thereof
  • Perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Intermediate preparation - in a 0.5L autoclave, add 90g of ethylene glycol dimethyl ether and 18g of KF, turn on stirring, cool down to 0°C, then slowly add 180g (1mol) of tetrafluorosultone dropwise, and control the internal temperature to 0°C ~10°C, after the dropwise addition was completed, stirring was continued for 0.5 h, followed by the addition of 0.09 g of dimethylethylenediamine. After the addition was completed, the temperature was lowered to -25°C, and 282.2 g (1.7 mol) of hexafluoropropylene oxide was slowly introduced into the normal pressure. After the reaction was completed, the stirring was stopped and the layers were allowed to stand. Pure intermediate, yield 85%.

[0030] Preparation of intermediate carboxylate solution—in a 1L autoclave, add 256 g of diethylene glycol dimethyl ether, 116.59 g (1.1 mol) of sodium carbonate, stir and heat up to 50 ° C, slowly add 512 g (1 mol) of intermediate dropwise, dropwise After the addition was completed, stirrin...

Embodiment 2

[0033]Intermediate preparation - in a 0.5L autoclave, add 126g of tetrahydrofuran and 18g of KF, turn on stirring, cool down to 0°C, then slowly add 180g (1mol) of tetrafluorosultone dropwise, control the internal temperature from 0°C to 10°C, dropwise After the addition was completed, stirring was continued for 0.5 h, followed by the addition of 0.36 g of tri-n-butylamine. After the addition was completed, it was cooled to -5°C, and 332.0 g (2.0 mol) of hexafluoropropylene oxide was slowly introduced into the normal pressure. After the reaction was completed, the stirring was stopped and the layers were allowed to stand. The upper solvent continued to be applied mechanically, and the lower intermediate was purified by rectification to obtain Pure intermediate, yield 86%.

[0034] Preparation of intermediate carboxylate solution—in a 1L autoclave, add 307g of tetraethylene glycol dimethyl ether, 138g (1.3mol) of sodium carbonate, stir and heat up to 60°C, slowly add 512g (1mol...

Embodiment 3

[0037] Intermediate preparation-in a 0.5L autoclave, add 108g of tetraethylene glycol dimethyl ether and 18g of KF, turn on stirring, cool down to 0°C, then slowly add 180g (1mol) of tetrafluorosultone dropwise, and control the internal temperature to 0 ℃~10℃, continue stirring for 0.5h after the dropwise addition, and then add 0.15g of sodium hydride. After the addition was completed, it was cooled to -15°C, and 298.8 g (1.8 mol) of hexafluoropropylene oxide was slowly introduced into the normal pressure. After the reaction was completed, the stirring was stopped and the layers were allowed to stand. The upper layer solvent continued to be applied mechanically, and the lower layer intermediate was purified by distillation to obtain Pure intermediate, yield 82%.

[0038] Preparation of intermediate carboxylate solution—in a 1L autoclave, add 358 g of tetrahydrofuran and 159 g (1.5 mol) of sodium carbonate, stir and heat up to 55°C, slowly add 512 g (1 mol) of intermediate drop...

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Abstract

The invention discloses perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride for preparing perfluorinated sulfonic acid resin and a preparation method of the perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride. The preparation method comprises the following steps: 1) by taking tetrafluorosultone and hexafluoropropylene oxide as raw materials, preparing an intermediate pure product through KF catalytic isomerization/addition and the like under the condition of a solvent A and an auxiliary agent; 2) adding a solvent A, sodium carbonate, the intermediate and an auxiliary agent to obtain an intermediate carboxylate solution; and 3) treating the intermediate carboxylate solution with a solvent B to obtain the perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride. According to the method, industrial operation is greatly simplified, and the method has a good application prospect; more importantly, the content of the impurity H-PSVE can be controlled within a small range (the purity of the PSVE is greater than or equal to 99.9%, and the impurity H-PSVE is less than or equal to 20ppm), so that the average molecular weight of the prepared perfluorosulfonic acid resin can be well controlled within the optimal range of the perfluorosulfonic acid resin, and various downstream applications are met.

Description

technical field [0001] The invention relates to a perfluoro(4-methyl-3,6-dioxa-7-octene)sulfonyl fluoride for preparing perfluorosulfonic acid resin and a preparation method thereof, belonging to the field of organic fluorine chemistry. The method greatly reduces the process operation requirements and better matches the industrialization. Background technique [0002] Perfluoro(4-methyl-3,6-dioxa-7-octene)sulfonyl fluoride (referred to as PSVE), colorless transparent liquid. It is an important comonomer for a wide range of polymer organic fluorine materials. It can be copolymerized with other monomers to prepare fluorine resins, fluorine rubber and other materials with special functions under specific conditions. The main monomer necessary for acid ion exchange resin, the main function is to introduce functional sulfonic acid group chain into the polymer. The functional membrane material was first developed and widely used in the 1970s. The material has excellent heat resi...

Claims

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Application Information

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IPC IPC(8): C07C309/82C07C303/02C07C303/22C08F16/30
CPCC07C309/82C07C303/02C07C303/22C08F16/30
Inventor 吕杨李宏峰叶文强肖艳茹
Owner JUHUA GROUP TECH CENT
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