Method for recovering perfluoro-2-(2-sulfuryl fluoride ethyoxyl) propyl vinyl ether in polymer

A technology of sulfuryl fluoride ethoxy and propyl vinyl ether, which is applied in the field of perfluoro-2-propyl vinyl ether in recycled polymers, can solve the problems of lower yield, separation failure, and generation of impurities. Achieve the effect of reducing production cost, reducing the difficulty of post-processing, and operating flexibility

Pending Publication Date: 2021-11-02
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the polymerization system contains a large amount of fluorine surfactants and initiators, etc., and the air stripping method to recover PSVE will easily lead to separation failure due to the generation of a large amount of foam, and the steam stripping method generally needs to be carried out at a higher temperature. PSVE encounters high temperature and no In the state of protective measures, it is easy to decompose, produce impurities, and reduce the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Add 10.0 kg of perfluorosulfonic acid resin powder with a particle size of 100 mesh and 10 wt% (wt%, mass percentage) of PSVE in the reaction kettle, add 1,1,2,2-tetrafluoroethyl -2,2,2-Trifluoroethyl ether and n-hexane with a mass ratio of 1:8 mixed extractant 12kg, control the temperature of the kettle at 10°C, stir at 50 rpm for 0.5h, release the material and filter, Obtain the extracted resin and filtrate (I);

[0036] (2) the filtrate (I) that step (1) obtains is put into another reaction kettle, stirs, slowly adds the sodium carbonate aqueous solution of 10wt%, regulates solution pH=5, then pours into filter and filters, obtains Filtrate (II), static layering, obtains organic layer;

[0037] (3) The organic layer obtained in step (2) is packed into a rectification device, and the rectification device drives away the air in the device through high-purity nitrogen, opens the cooling system, turns on the heater, and carries out rectification under normal pressur...

Embodiment 2

[0040] (1) Add 10.0 kg of perfluorosulfonic acid resin powder with a particle size of 100 mesh and 10 wt% PSVE in the reaction kettle, add 1,1,2,2-tetrafluoroethyl-2,2,2-trifluoro The mass ratio of ethyl ether and n-hexane is 15kg of mixed extractant, control the temperature of the kettle at 20°C, stir at 80 rpm for 1h, release the material and filter to obtain the extracted resin and filtrate (I) ;

[0041] (2) the filtrate (I) that step (1) obtains is put into another reaction kettle, stirs, slowly adds the sodium carbonate aqueous solution of 10wt%, regulates solution pH=5.5, then pours into filter and filters, obtains Filtrate (II), static layering, obtains organic layer;

[0042](3) The organic layer obtained in step (2) is packed into a rectification device, and the rectification device drives away the air in the device through high-purity nitrogen, opens the cooling system, turns on the heater, and carries out rectification under normal pressure. Obtain the mixed extr...

Embodiment 3

[0045] (1) Add 10.0 kg of perfluorosulfonic acid resin powder with a particle size of 100 mesh and 10 wt% PSVE in the reaction kettle, add 1,1,2,2-tetrafluoroethyl-2,2,2-trifluoro 10kg of mixed extractant with a mass ratio of ethyl ether and n-hexane of 1:3, control the temperature of the kettle at 30°C, stir at 100 rpm for 2h, release the material and filter to obtain the extracted resin and filtrate (I) ;

[0046] (2) put the filtrate (I) that step (1) obtains into another reactor, stir, slowly add 10wt% sodium carbonate aqueous solution, adjust solution pH=6, then pour into filter and filter to obtain Filtrate (II), static layering, obtains organic layer;

[0047] (3) The organic layer obtained in step (2) is packed into a rectification device, and the rectification device drives away the air in the device through high-purity nitrogen, opens the cooling system, turns on the heater, and carries out rectification under normal pressure. Obtain the mixed extractant that recla...

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Abstract

The invention discloses a method for recovering perfluoro-2-(2-sulfuryl fluoride ethyoxyl) propyl vinyl ether in a polymer, which comprises the following steps: (1) stirring and mixing the polymer containing the perfluoro-2-(2-sulfuryl fluoride ethyoxyl) propyl vinyl ether with an extracting agent, extracting, and filtering to obtain an extracting solution; (2) adjusting the pH value of the extraction solution to 5-8 by using an alkaline solution, filtering to obtain filtrate, and standing and layering the filtrate to obtain an organic layer; (3) carrying out normal-pressure rectification on the organic layer under the protection of nitrogen to obtain the recovered extracting agent and tower bottoms; and (4) carrying out reduced pressure rectification on the tower bottoms under the protection of a stabilizer to obtain the perfluoro-2-(2-sulfuryl fluoride ethyoxyl) propyl vinyl ether. The method has the advantages of simple process, high efficiency, economy and environmental protection.

Description

technical field [0001] The invention relates to a technology for recovering monomers in the polymerization industry, in particular to a method for recovering perfluoro-2-(2-sulfuryl fluoride ethoxy) propyl vinyl ether in polymers. Background technique [0002] Perfluoro-2-(2-sulfuryl fluoride ethoxy) propyl vinyl ether, alias: perfluorovinyl ether sulfonyl fluoride, abbreviation: PSVE, boiling point is 135 ℃, is an important perfluoromonomer , can be used to develop perfluororubber, perfluororesin, functional resin and other products, and the market price is high. [0003] When PSVE is used as raw material to produce perfluoropolymers such as perfluorosulfonic acid resin, not all PSVE raw materials participate in the reaction, and 20% to 40% remain in the polymerization system because they do not participate in the reaction. The residual monomer affects Product quality brings great difficulty to the resin post-treatment process. The PSVE-containing waste liquid generated du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J11/02C08F16/30C07C303/44C07C309/82
CPCC08J11/02C08F16/30C07C303/44C07C309/82
Inventor 童闻亮王宗令徐益宾
Owner JUHUA GROUP TECH CENT
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