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A method of preparing fluororubber through microemulsion polymerization

A technology of microemulsion polymerization and fluororubber, which is applied in the field of preparation of fluororubber by microemulsion polymerization, can solve problems such as application research blanks, and achieve the effects of avoiding gel, improving vulcanization, and improving production efficiency

Inactive Publication Date: 2017-05-10
江苏梅兰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, a few foreign companies have developed substitutes for perfluorooctanoate for the production of fluorine rubber, such as 3M’s perfluorobutane sulfonic acid (C4), DuPont’s C6-based products containing hydrocarbon chain segments, and Japan’s Daikin Corporation’s C6 products, while the application research in this area in my country is still blank

Method used

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  • A method of preparing fluororubber through microemulsion polymerization
  • A method of preparing fluororubber through microemulsion polymerization
  • A method of preparing fluororubber through microemulsion polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In this example, fluoroether carboxylate and fluoroether oil are used as raw materials to prepare microemulsion surfactants:

[0025] Add 4kg of deionized water to a 10L container, and 1.8kg of structural formula is CF 3 O(CF(CF 3 ) CF 2 O) 3 (CF 2 CF 2 O) 5 COONH 4The fluoroether carboxylate, 1.0kg structural formula is CF 3 O(CF(CF 3 ) CF 2 O) 12 (CF 2 CF 2 O) 2 CF 3 The fluoroether oil is stirred uniformly under normal temperature and pressure to obtain an aqueous solution of a microemulsion surfactant with a concentration of 41.2%.

Embodiment 2

[0027] Add 4kg of deionized water to a 10L container, and 3.8kg of structural formula is CF 3 O(CF(CF 3 ) CF 2 O) 8 COONH 4 The fluoroether carboxylate, 1.6kg structural formula is CF 3 O(CF(CF 3 ) CF 2 O) 10 (CF 2 CF 2 O) 4 CF 3 The fluoroether oil is stirred uniformly under normal temperature and pressure to obtain a concentration of 57.4% in the aqueous solution of the microemulsion surfactant.

Embodiment 3

[0029] Taking a 100L polymerization kettle as an example, add 60kg of ion-free water and 1.2kg of the microemulsion surfactant prepared in Example 1 into the reaction kettle; after nitrogen replacement and vacuum treatment, the oxygen content in the kettle is ≤ 20ppm; Add vinylidene fluoride and hexafluoropropylene mixed monomers with a mass ratio of 60:40, until the pressure of the kettle is 2.1 Mpa; stir, heat up to 92°C, add 1.2Kg of potassium persulfate initiator with a concentration of 5% to start the reaction, and the reaction During the process, the monomer mixture is continuously added to keep the pressure at 2.1Mpa; when a certain amount of reaction is stopped, the reaction is stopped, and the unreacted mixed monomer is recovered after cooling; Obtain binary fluorine rubber raw rubber.

[0030] See Table 1. The fluororubber prepared in Example 3 is compared with the fluororubber prepared by using perfluorooctanoic acid as an emulsifier, and the rest of the operations ...

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Abstract

A method of preparing fluororubber through microemulsion polymerization is disclosed. The method includes (1) compounding fluoroether carboxylic acid or carboxylate polymer the molecular formula of which is CF3O(CF(CF3)CF2O)(CF2CF2O)COOX and a fluoroether oil polymer the molecular formula of which is CF3O(CF(CF3)CF2O)<c>(CF2CF2O)<d>CF3 according to a certain ratio to obtain an aqueous solution having a certain concentration; (2) subjecting one or a plurality of fluoroolefin monomers, a cure site monomer, a perfluoroether functional monomer and other olefin monomers according to a ratio to microemulsion polymerization in a polymerization kettle under actions of a fluorine-containing microemulsion surfactant, an initiator, and other auxiliary agents; and (3) subjecting the emulsion obtained through polymerization to coacervation, washing and drying for dehydration, and then preparing a fluororubber sheet resistant to low temperature through an open mill. Vulcanization, mechanical and low-temperature resistant properties of the fluororubber are effectively improved, the polymerization time is greatly shortened, and the production efficiency is increased.

Description

technical field [0001] The invention relates to a method for preparing fluorine rubber by microemulsion polymerization. Background technique [0002] In the process of producing fluororubber by traditional emulsion polymerization, perfluorooctanoic acid and its derivatives are widely used as emulsifiers due to their excellent surface activity and emulsifying properties. Due to the impact of the "Teflon incident", the United States and the European Union have legislated The import and use of products containing perfluorooctanoate will be completely prohibited in the next year. Therefore, it is of great significance to develop a clean production process for fluororubber without perfluorooctanoate. At present, a few foreign companies have developed substitutes for perfluorooctanoate for the production of fluorine rubber, such as 3M’s perfluorobutane sulfonic acid (C4), DuPont’s C6-based products containing hydrocarbon chain segments, and Japan’s Daikin Corporation’s C6 product...

Claims

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Application Information

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IPC IPC(8): C08F214/22C08F214/28C08F214/26C08F216/14C08F2/26C08F2/30
CPCC08F214/22C08F2/26C08F2/30C08F214/282
Inventor 钱厚琴程爱峰吴玉勋王昌尧
Owner 江苏梅兰化工有限公司
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