Low-temperature resistant fluorubber, and preparation method thereof

A fluororubber and low temperature resistant technology, applied in the field of low temperature resistant fluororubber and its preparation, can solve the problems of extremely high safety requirements, expensive raw materials, low brittle temperature, etc. The effect of improving low temperature resistance

Active Publication Date: 2014-04-30
江苏梅兰化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But fluorine rubber also has a prominent disadvantage: its low temperature performance is too poor (generally Tg is only -20°C), which is far from meeting the market's requirements for its performance, especially in aviation and aerospace, because of its high-speed flight in high altitude, The temperature of the working parts is extremely low and extremely high, and these parts are often subject to strong corrosion, and because the aerospace industry has extremely high safety requirements, it is only possible to find a breakthrough in fluorine rubber, that is to say, find a way to make fluorine Rubber has a low brittle temperature
Before the present invention was made, the Chinese invention patents with publication numbers CN85109162 and CN1152583A disclosed several novel monomers capable of improving the low-temperature performance of rubber, but the raw materials required for this technical solution were expensive, and sometimes used in the preparation process containing Fluoroalkyl iodide, therefore, complex processing

Method used

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  • Low-temperature resistant fluorubber, and preparation method thereof
  • Low-temperature resistant fluorubber, and preparation method thereof
  • Low-temperature resistant fluorubber, and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0017] In this embodiment, tetrafluoropropanol is used as raw material to prepare tetrafluoropropyl pentafluoropropenyl ether through condensation reaction:

[0018] In a reactor equipped with stirring, thermometer, and condenser, by weight, 24 parts of tetrafluoropropanol, 8 parts of pentafluorobromopropene and 1 part of tetrabutylammonium bromide were dissolved in 20 parts of CH 2 Cl 2 Add 7.5 parts of aqueous solution of 5 parts of NaOH dropwise, heat up to 50°C and react for 24 hours, cool the reaction solution, filter out insoluble salts, separate the oil layer, pickle with 4% hydrochloric acid once, wash with distilled water 3 times to medium properties, after drying with anhydrous sodium sulfate, the product tetrafluoropropyl pentafluoropropenyl ether was obtained by fractional distillation with a yield of 83.5%.

[0019] Re-synthesis of branched fluorine rubber containing tetrafluoropropyl pentafluoropropenyl ether:

[0020] to 3m 3 Add 1500Kg of deionized water to ...

Embodiment 2

[0022] In this example, octafluoropentyl pentafluoropropenyl ether was prepared by condensation reaction according to the preparation method of Example 1, and the yield was 76.4%.

[0023] Re-synthesis of branched fluorine rubber containing octafluoropentyl pentafluoropropenyl ether:

[0024] to 3m 3 Add 1500Kg of deionized water to the polymerization kettle, replace with nitrogen and vacuumize, and then add 0.9Kg of ammonium perfluorooctanoate, 1.5Kg of disodium hydrogen phosphate, and 7.5Kg of diethyl malonate into the polymerization kettle after the oxygen content in the kettle is qualified. Then, a monomer mixture composed of 1,1-difluoroethylene, hexafluoropropylene, and octafluoropentylpentafluoropropenyl ether in a molar ratio of 75:22:3 is added into the reaction kettle through a compressor to make the pressure in the kettle When it reaches 2.0Mpa, heat the reaction mixture to 85°C, add 0.9Kg potassium persulfate to start the reaction, and continuously add monomer mix...

Embodiment 3

[0026] to 3m3 Add 1500Kg of deionized water into the polymerization kettle, replace with nitrogen and vacuumize, and after the oxygen content in the kettle is qualified, add 12Kg of ammonium perfluorooctanoate, 6Kg of disodium hydrogen phosphate, and 3Kg of diethyl malonate into the polymerization kettle, and then add 1 , 1- difluoroethylene, hexafluoropropylene, tetrafluoropropyl pentafluoropropenyl ether in a molar ratio of 78:12:10 into the reaction kettle through the compressor, so that the pressure in the kettle reaches 2.4Mpa , the reaction mixture was heated to 75°C, and 1.5Kg potassium persulfate was added to start the reaction. During the reaction, the monomer mixture was continuously added to keep the pressure at 2.6Mpa, while maintaining a stirring rate of 500r / min to maintain the reaction rate; Finally, stop adding the monomer mixture, and recover the unreacted mixed monomer after cooling; the latex obtained by polymerization is coagulated, washed, dried and dehydra...

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Abstract

The invention relates to a low-temperature resistant fluorubber, and a preparation method thereof, and belongs to the field of fluorine chemical industry and high molecular material technology. The preparation method comprise following steps: 1) alcohols containing fluorine, such as tetrafluoro-1-Propanol, octafluoropentyl alcohol, and H,1H,7H-dodecafluoro-1-heptanol are taken as initial fluorine-containing materials, and are subjected to condensation with pentafluoro bromopropylene in the presence of a phase transfer catalyst so as to obtain a fluorine-containing ether containing carbon-carbon double bonds; 2) a monomer mixture is prepared from 1,1-difluoroethylene, hexafluoropropylene, and fluorine-containing alkyl pentafluoropropene ether according to a certain molar ratio, and is stored for further treatment; and 3) the monomer mixture is delivered into a polymerization vessel, and is subjected to emulsion polymerization in the presence of an emulsifier, an initiator, and a chain transferring agent, and latex obtained via polymerization is subjected to coacervation, washing, and drying, and is made into low-temperature resistant fluorubber sheets using a open mill. The preparation method is capable of improving low-temperature resistance of fluorubber effectively, so as to satisfy requirements on low-temperature sealing; the raw materials are easily available; preparation processes are easy to realize; and the preparation method is beneficial for popularization and application.

Description

technical field [0001] The invention relates to a low temperature resistant fluorine rubber and a preparation method thereof. Background technique [0002] Fluorine rubber has a series of excellent properties such as oil resistance, high temperature resistance, solvent resistance, strong acid resistance, strong oxidant resistance, flame retardancy, aging resistance, etc. field has been widely applied. Especially in recent years, with the rapid development and technological progress of the above-mentioned related industries, fluororubber, as an irreplaceable high-performance elastomer, not only has a substantial increase in demand, but also continues to expand in use. But fluorine rubber also has a prominent disadvantage: its low temperature performance is too poor (generally Tg is only -20°C), which is far from meeting the market's requirements for its performance, especially in aviation and aerospace, because of its high-speed flight in high altitude, The temperature of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F214/28C08F216/14C08F2/24
Inventor 王昌尧吴玉勋钱厚琴
Owner 江苏梅兰化工有限公司
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