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), DuPon

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

Example Embodiment

[0023] Example 1:

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

[0025] Add 4kg of non-ionized water into a 10L container, 1.8kg structure is CF 3 O(CF(CF 3 )CF 2 O) 3 (CF 2 CF 2 O) 5 COONH 4 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 evenly under normal temperature and pressure to obtain an aqueous solution of microemulsion surfactant with a concentration of 41.2%.

Example Embodiment

[0026] Example 2:

[0027] Add 4kg of deionized water into a 10L container, 3.8kg of structure is CF 3 O(CF(CF 3 )CF 2 O) 8 COONH 4 Fluoroether carboxylate, 1.6kg structure 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 evenly under normal temperature and pressure to obtain an aqueous solution of microemulsion surfactant with a concentration of 57.4%.

Example Embodiment

[0028] Example 3:

[0029] Take a 100L polymerization kettle as an example, add 60kg of non-ionized water and 1.2kg of the microemulsion surfactant prepared in Example 1 to the reaction kettle; after nitrogen replacement and vacuum treatment, the oxygen content in the kettle is ≤20ppm; Add the mixed monomer of vinylidene fluoride and hexafluoropropylene with a mass ratio of 60:40 to a kettle pressure of 2.1 Mpa; stir, heat up to 92°C, add a 5% potassium persulfate initiator 1.2Kg to start the reaction, and react During the process, the monomer mixture is continuously added to keep the pressure at 2.1Mpa; the reaction is stopped after a certain amount of reaction, and the unreacted mixed monomer is recovered after cooling; the polymerized latex is coagulated, washed, dried and dehydrated by the mill Get binary fluorine rubber raw rubber.

[0030] See Table 1. The fluororubber prepared in Example 3 is compared with the fluororubber prepared with perfluorooctanoic acid as an emulsifi...

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PUM

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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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