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Preparation method of perfluoro-3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride

A technology of octenesulfonyl and dioxa, applied in the field of preparation of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride, can solve the problem of many reaction steps and many by-products , long reaction time and other problems, to achieve the effect of short reaction route, less by-products, high yield and purity

Pending Publication Date: 2021-01-22
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has more reaction steps, longer reaction time and more by-products

Method used

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  • Preparation method of perfluoro-3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride
  • Preparation method of perfluoro-3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride
  • Preparation method of perfluoro-3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) synthesis

[0033] In a 1L reactor, add ethylene glycol dimethyl ether 200ml, sodium fluoride 3.6g, tetrafluoroethane-β-sultone 180g (1mol), then import 300g (1.8mol) according to the flow rate of 0.25kg / h ) hexafluoropropylene oxide for addition reaction, the reaction temperature is controlled at 10°C, and the reaction pressure is controlled at 0.2MPa. After the introduction of hexafluoropropylene oxide is completed, the reaction is continued for 1h. After the reaction is completed, the reaction solution is rectified to obtain 478g ( 0.93mol) intermediate, the yield is 92%, and the purity is 99.3%;

[0034] (2) PSVE synthesis

[0035]In the moving bed reactor (volume 2L, material 316L, produced by Suzhou Newmt Technology Co., Ltd.), the mixture of 450g (0.87mol) of the intermediate obtained in step (1) and 400g of sodium carbonate (3.77mol) was passed through the moving The salt-forming zone and decarboxylation zone of the bed reactor (the salt-forming temperatur...

Embodiment 2

[0037] (1) Synthesis of intermediates

[0038] In a 1L reactor, add 50ml of diethylene glycol dimethyl ether, 10g of lithium fluoride, 200g (1.2mol) of tetrafluoroethane-β-sultone, and then import 250g (1.5mol) at a flow rate of 0.2kg / h. mol) of hexafluoropropylene oxide for addition reaction, the reaction temperature is controlled at 15°C, and the reaction pressure is controlled at 0.3MPa. After the introduction of hexafluoropropylene oxide is completed, the reaction is continued for 1h. After the reaction is completed, the reaction liquid is rectified to obtain 522g (1.01mol) intermediate, the yield is 91%, and the purity is 99.2%;

[0039] (2) PSVE synthesis

[0040] In the moving bed reactor (volume 2L, material 316L, produced by Suzhou Newmt Technology Co., Ltd.), the mixture of 500g (0.97mol) of the intermediate obtained in step (1) and 500g (4.71mol) of sodium carbonate is passed through the moving The salt-forming zone and decarboxylation zone of the bed reactor (the...

Embodiment 3

[0042] (1) Synthesis of intermediates

[0043] In a 1L reactor, add 300ml of dimethylformamide, 15.4g of calcium fluoride, 220g (1.22mol) of tetrafluoroethane-β-sultone, and then import 415g (2.5mol) at a flow rate of 0.1kg / h ) hexafluoropropylene oxide for addition reaction, the reaction temperature is controlled at 5°C, and the reaction pressure is controlled at 0.1MPa. After the introduction of hexafluoropropylene oxide is completed, the reaction is continued for 1h. After the reaction is completed, the reaction liquid is rectified to obtain 587g ( 1.15mol) intermediate, the yield is 93%, and the purity is 99.1%.

[0044] (2) PSVE synthesis

[0045] In a moving bed reactor (volume 2L, material 316L, produced by Kunshan Fuxi Engineering Technology Co., Ltd.), a mixture of 540g (1.05mol) of the intermediate obtained in step (1) and 550g (3.98mol) of potassium carbonate was passed through the moving The salt-forming zone and decarboxylation zone of the bed reactor (the salt-...

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Abstract

The invention discloses a synthesis method of perfluoro-3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride (PSVE), which comprises the following steps: (1) reacting tetrafluoroethane beta sultone with hexafluoropropylene oxide in an organic solvent under the action of a catalyst, and rectifying the reaction solution to obtain an intermediate after the reaction is finished; and (2) mixing alkali carbonate and the intermediate obtained in the step (1) according to a molar ratio of (1-8): 1, carrying out a salt forming reaction at 50-250 DEG C, wherein the contact time of the reaction is 5-10 min, then carrying out a decarboxylation reaction at 260-500 DEG C, wherein the contact time of the reaction is 10-30 min, collecting a decarboxylation reaction product, and carrying out condensation and rectification to obtain the 3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride product. The method has the advantages of simple process, short reaction route, safety, environmental protection, high yield andhigh purity.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride (PSVE). Background technique [0002] Perfluoro 3,6-dioxa-4-methyl-7-octenesulfonyl fluoride (PSVE) is an important comonomer for a wide range of polymers and organic fluorine materials. It can be copolymerized with other monomers to prepare materials such as fluororesins and fluororubbers with special functions used under specific conditions; it can also prepare fluorinated polymers with excellent heat resistance and high proton conductivity, and through The fluorinated polymer can give a solid polymer electrolyte membrane having excellent heat resistance. [0003] PSVE is one of the main monomers for the preparation of perfluorosulfonic acid ion exchange resins. The main function is to introduce functional sulfonic acid group chains into the polymer, which can be copolymerized with TFE ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/82C07C303/02C07C303/44
CPCC07C303/02C07C303/44
Inventor 刘华平马利勇叶立峰郑佳
Owner JUHUA GROUP TECH CENT
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