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Preparation method for special low-temperature-resistant fluororubber

A technology of fluororubber and low temperature resistance, which is applied in the field of special low temperature resistant fluororubber preparation, which can solve the problems of poor emulsion stability, perfluorooctanoic acid environmental pollution, etc., and achieve the effect of improving performance

Inactive Publication Date: 2015-12-02
江苏梅兰化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the surface activity of this fluoroether oligomer liquid is lower than that of perfluorooctanoic acid commonly used in fluoropolymer emulsion polymerization, and the emulsion stability is poor. However, due to the environmental pollution caused by perfluorooctanoic acid, it is urgent to find alternatives to perfluorooctanoic acid
In addition, the surface oil repellency of this kind of fluoroether oligomer is not as good as that of traditional three-proof fluoropolymer, and its surface tension performance still needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0010] The preparation process of the present invention is further described below: in the pressure-resistant reactor, add deionized water and special fluoroether carboxylate as surfactant and special fluoroether oil, after deoxygenation in the reactor, heat and stir, and pass into the gas phase Fluorinated monomers, containing molar ratio (20%-70%) of vinylidene fluoride, (10%-40%) hexafluoropropylene, (0%-70%) tetrafluoroethylene, other optional copolymerized monomers Body (0% ~ 40%) selected from: perfluoromethyl vinyl ether, perfluoroethyl vinyl ether, perfluoropropyl vinyl ether, fluoroethylene, ethylene, propylene, trifluoroethylene, trifluorochloroethylene , difluorodichloroethylene, 3,3,3-trifluoropropylene and perfluoroalkylethylene, any one monomer or a combination of more than one monomer, then add a free radical initiator, and the reaction temperature is controlled At 20 degrees to 140 degrees, the reaction pressure is controlled at 1 atmosphere to 50 atmospheres, ...

Embodiment 1

[0021] Embodiment 1 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0022] In a photochemical reaction kettle with an internal volume of about 10 liters, nitrogen exhaust and dehumidification are first used, the jacket temperature is reduced to minus 70 degrees, and then 9.9 kilograms of fluorine-containing monomer A (90% hexafluoro Propylene, 10% tetrafluoroethylene), 0.1 kg of fluorine-containing monomer B: perfluoropropenyl methyl ether CF2=CFCF2-O-CF3, at this time, the mixed fluorine-containing monomer is basically liquefied, and the stirring is started, and the ultraviolet light is turned on The power of the lamp is about 300 watts. Oxygen (about 3.5 liters / minute) and difluorodichloromethane (about 0.45 liters / minute) are introduced into the bottom of the kettle, and the temperature in the kettle is controlled at about minus 35 to minus 40 degrees Celsius. After about 8 hours of reaction, the stirring was stopped, the unreacted monomers were disch...

Embodiment 2

[0023] Embodiment 2 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0024] In a photochemical reaction kettle with an internal volume of about 10 liters, nitrogen exhaust and dehumidification are first used, the jacket temperature is reduced to minus 70 degrees, and then 9.5 kilograms of fluorine-containing monomer A (80% hexafluoro Propylene, 20% tetrafluoroethylene), 0.5 kg of fluorine-containing monomer B: perfluoropropenyl propyl ether CF2=CFCF2-O-C3F7, at this time, the mixed fluorine-containing monomer is basically completely liquefied, stirring is started, and ultraviolet light is turned on The power of the lamp is about 300 watts. Oxygen (about 3.6 liters / minute) and bromotrifluoromethane (about 0.41 liters / minute) are introduced into the bottom of the kettle, and the temperature in the kettle is controlled at about minus 35 to minus 40 degrees Celsius. After about 8 hours of reaction, the stirring was stopped, the unreacted monomers were dischar...

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Abstract

The present invention discloses a preparation method for special low-temperature resistant fluororubber. The method comprises: in a pressure resistant reactor, adding deionized water and special fluoroether carboxylate as a surfactant; after deoxidation of the reactor, performing heating and stirring; introducing vapor fluorine-containing monomers that comprises the following materials in percentage by weight: 20%-70% of vinylidene fluoride, 10%-40% of hexafluoropropene, 0%-70% of tetrafluoroethylene and 0%-40% of other selectable comonomer that is one of the monomers or a combination of more than one monomers selected from: perfluoro methyl vinyl ether, perfluoro ethyl vinyl ether, perfluoro propyl vinyl ether, fluoroethylene, ethylene, propylene, trifluoroethylene, chlorotrifluoroethylene, difluoro dichloroethylene, 3,3,3-trifluoropropene, and perfluoroalkyl ethylene; and then adding a free radical initiator to prepare the fluororubber, wherein the reaction temperature is controlled at 20-140 DEG C, and the reaction pressure is controlled at 1-50 atmospheric pressure, and the concentration of the special fluoroether carboxylate in the final emulsion product is 0.01%-3%.

Description

technical field [0001] The invention relates to a method for preparing a special low-temperature resistant fluororubber, in particular to the special low-temperature resistant fluororubber prepared by using a special fluoroether oligomer and its derived fluoroether surfactant and fluoroether oil. Background technique [0002] The low temperature resistance of traditional fluorine rubber is not good. Taking fluoride rubber as an example, its low temperature resistance is generally as low as minus 30 degrees and it is easy to be brittle. This is not enough for the development of aerospace materials and needs to be improved. [0003] Fluoroether oils, especially fluoroether oligomers, have excellent physical surface properties, low temperature resistance and chemical stability, and are widely used in chemical materials, mechanical seals, high temperature resistance lubrication, aerospace military industry, new materials and other fields. Applications. Fluorine-containing monom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/28C08F214/26C08F216/14C07C41/30C07C43/17
Inventor 钱厚琴吴慧生
Owner 江苏梅兰化工有限公司
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