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Process for producing elastic fluorocopolymer and crosslinked fluororubber

A manufacturing method and a technology for copolymers, applied in the field of cross-linked fluororubber, can solve problems such as easily hindering cross-linking, and achieve the effects of good cross-linking reactivity, good compression set, and reduced phosphorus content

Inactive Publication Date: 2010-09-22
ASAHI GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if a vinylidene fluoride / hexafluoropropylene-based copolymer is mixed with the copolymer or an acidic filler such as silica is incorporated, there is a problem that crosslinking is easily hindered.

Method used

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  • Process for producing elastic fluorocopolymer and crosslinked fluororubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] (acid polymerization - acid coagulation)

[0108] A stainless steel pressure vessel having an internal volume of 3200 mL having an anchor fin for stirring was degassed, and then a homogeneous mixed solution of 1600 g of ion-exchanged water, 97 g of tert-butanol, and 9 g of sodium lauryl sulfate was added. The pH of this homogeneous mixture was 7.0. Next, the temperature of the solution in the reactor was raised to 80° C., and the pre-prepared monomer mixed gas of TFE / P=85 / 15 (molar ratio) was injected to make the internal pressure of the reactor 2.50 MPaG. The fins were rotated at 300 rpm, and 25 g of a 10% by mass aqueous solution of ammonium persulfate was added to start the polymerization reaction.

[0109] The pressure decreases with the progress of polymerization, so when the internal pressure of the reactor drops to 2.49MPaG, the mixed gas of TFE / P=56 / 44 (molar ratio) prepared in advance is pressed into the internal pressure of the reactor by self-pressure, so th...

Embodiment 2

[0113] (Basic Polymerization-Acidic Coagulation)

[0114] After degassing a stainless steel pressure vessel with an inner volume of 3200 mL having anchor fins for stirring, 1600 g of ion-exchanged water, 97 g of tert-butanol, 9 g of sodium lauryl sulfate, 1.5 g of sodium hydroxide, and 42 g of sodium hydrogenphosphate were added. The pH is 11.5. Next, a monomer mixed gas of TFE / P=85 / 15 (molar ratio) was pressurized at 80° C. so that the internal pressure of the reactor was 2.50 MPaG. The fins were rotated at 300 rpm, and 25 g of a 10% by mass aqueous solution of ammonium persulfate was added to start the polymerization reaction.

[0115] Other than that, it carried out similarly to Example 1, and obtained the TFE / P / crotonate vinyl ester copolymer latex of 20 mass % of solid content concentration. The pH of the obtained latex was 9.5. The polymerization time was about 3.5 hours.

[0116] After adjusting the pH of 2205 g of the latex to 2.0 with sulfuric acid, it was added t...

Embodiment 3

[0119] (neutral aggregation-neutral agglutination)

[0120] After degassing a stainless steel pressure vessel with an inner volume of 3200 mL having anchor fins for stirring, 1600 g of ion-exchanged water, 97 g of tert-butanol, 9 g of sodium lauryl sulfate, and 8.0 g of ammonium sulfite were added. At this point the pH of the solution was 7.0. Next, a monomer mixed gas of TFE / P=85 / 15 (molar ratio) was pressurized at 40° C. so that the internal pressure of the reactor was 2.50 MPaG. The fins were rotated at 300 rpm, and a 10% by mass aqueous solution of ammonium persulfate was added to start the polymerization reaction. Then, a 10% by mass aqueous solution of ammonium persulfate was continuously added using a high-pressure pump.

[0121] The pressure decreases with the progress of polymerization, so when the internal pressure of the reactor drops to 2.49MPaG, the mixed gas of TFE / P=56 / 44 (molar ratio) prepared in advance is pressed into the internal pressure of the reactor by...

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Abstract

A process for producing an elastic fluorocopolymer, which comprises emulsion-polymerizing at least one fluoromonomer (a) selected from the group consisting of tetrafluoroethylene, hexafluoropropylene, vinylidene fluoride and a perfluorovinyl ether represented by CF2-CF-O-R<f >(wherein R<f >is a C1-8 perfluoroalkyl group or a perfluoro(alkoxyalkyl) group), a vinyl ester monomer (b) represented by the formula CR<1>R<2>-CR<3>COOCH-CH2 (wherein each of R<1 >and R<2 >which are independent of each other, is a hydrogen atom, a C1-10 alkyl group or a C1-10 alkoxyalkyl group containing an etheric oxygen atom, and R<3 >is a hydrogen atom, a fluorine atom or a methyl group), and as the case requires, at least one hydrocarbon monomer (c) selected from the group consisting of ethylene, propylene and avinyl ether represented by CH2-CH-O-R<4 >(wherein R<4 >is a C1-8 alkyl group or an alkoxyalkyl group), in an aqueous medium to produce an elastic fluorocopolymer latex, adjusting the pH of the elastic fluorocopolymer latex to from 1 to 9, and coagulating the elastic fluorocopolymer latex to isolate an elastic fluorocopolymer.

Description

technical field [0001] The present invention relates to a method for producing a fluorine-containing elastic copolymer, a fluorine-containing elastic copolymer obtained by the production method, and a crosslinked fluorine-containing rubber obtained by crosslinking the fluorine-containing elastic copolymer. Background technique [0002] Vinylidene fluoride / hexafluoropropylene-based copolymers, tetrafluoroethylene / propylene-based copolymers, tetrafluoroethylene / perfluoro(alkyl vinyl ether)-based copolymers, and the like are known as fluorine-containing elastic copolymers. [0003] These fluorine-containing elastic copolymers have good heat resistance and chemical resistance, so they can be used in severe environments that cannot be tolerated by ordinary materials. However, these fluorine-containing elastic copolymers lack reactivity and have insufficient crosslinking reactivity and adhesiveness with other materials, and a method of introducing reactive functional groups to imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08F214/26C08F2/22C08F210/06
CPCC08F214/267C08F214/265C08F214/18C08F214/20C08F218/04C08F210/00C08F214/22
Inventor 野村顺平舟木宙神谷浩树
Owner ASAHI GLASS CO LTD
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