Nitrosofluoro rubber solution polymerization process

A technology of nitrosofluororubber and polymerization process, which is applied in the field of organic fluorine chemistry, can solve the problems of inconvenient preparation of irregularly shaped sealing parts, single product form, single molding method, etc., and achieve the effect of superior synthesis effect

Active Publication Date: 2013-07-24
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the fluororubber in the solid form must be vulcanized into pre-designed parts through the process of kneading in an open mill (or internal mixer)-mould forming, the molding metho

Method used

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  • Nitrosofluoro rubber solution polymerization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1 Synthesis of solid-state nitrosofluororubber

[0044] Replace the stainless steel polymerization kettle with nitrogen and then evacuate it, and circulate the ethanol of -60°C as a cold medium in the jacket, and cool the empty kettle to -60°C; use the vacuum state of the polymerization kettle to add γ-nitroso in sequence by suction Base perfluorobutyric acid 100g, dichloromethane 3.5 liters; Start the polymerization kettle to stir, continue to circulate the cold medium in the jacket, and control the temperature of the kettle below -45°C, add 3.0 nitrosotrifluoromethane in the gas phase kg, add 3.1 kg of tetrafluoroethylene in the gas phase when the kettle temperature is lower than -50°C.

[0045] After the feeding was completed, the temperature of the polymerization kettle was allowed to rise naturally. When the temperature in the kettle rose to -45°C, the polymerization reaction started and released heat, and the initial pressure reached 0.62MPa. The reactio...

Embodiment 2

[0046] Example 2 Synthesis of semi-solid nitrosofluororubber

[0047] Replace the stainless steel polymerization kettle with nitrogen and then evacuate it, and circulate the ethanol as a cold medium at -70°C in the jacket, and cool the empty kettle to -60°C; use the vacuum state of the polymerization kettle to add γ-nitroso in sequence by suction Base perfluorobutyric acid 100g, molecular chain transfer agent ethyl ether 68g, dichloromethane 3.5 liters; start the polymerization kettle to stir, continue to circulate the cold medium in the jacket, and control the temperature of the kettle below -45°C, and add 1.6 kg of nitrosotrifluoromethane; 1.93 kg of tetrafluoroethylene was added in the gas phase when the kettle temperature was lower than -50°C.

[0048] After the feeding was completed, the temperature of the polymerization kettle was allowed to rise naturally. When the temperature inside the kettle rose to -45°C, the polymerization reaction started and released heat, and ...

Embodiment 3

[0049] Example 3 Synthesis of liquid nitrosofluororubber

[0050] Basically the same as Example 2, on this basis, sequentially add 100 g of γ-nitroso perfluorobutyric acid, 175 g of molecular chain transfer agent ether, and 3.5 liters of methylene chloride; Add 1.95 kg of nitrosotrifluoromethane; add 2.38 kg of tetrafluoroethylene in the gas phase under the condition that the temperature of the kettle is lower than -50°C.

[0051] After 18 hours of polymerization reaction, the solvent dichloromethane and the liquid polymer were taken out by liquid separation. After the polymer is washed with water, dehydrated, and low-molecular weight is removed, 2.48 kg of raw rubber is obtained as a light yellow transparent liquid. After testing, its intrinsic viscosity is 0.06 / dLg -1 , the acid content is 1.36% (mol), and the dynamic viscosity is 61Pa.s.

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Abstract

The invention provides a nitrosofluoro rubber solution polymerization process which comprises the following steps: performing low-temperature copolymerization on nitroso trifluoromethane, tetrafluoroethylene and a vulcanization point monomer in a dichloromethane solvent, and regulating the polymerization reaction through a molecular chain transfer agent so as to synthesize the fluororubber. The amount of the molecular chain transfer agent is changed, the regulation action of the molecular chain transfer agent is utilized, and nitrosofluoro rubber from a solid form to a liquid form with different dynamic viscosities can be polymerized. In the presence of the dichloromethane solvent, the mass transfer and heat transfer conditions of the polymerization reaction are greatly improved, so that the reaction is stably performed in an easily controlled state, the explosion hazard is avoided, the polymer and the solvent are easily and conveniently separated, and the efficiency is high.

Description

technical field [0001] The invention relates to a polymerization method, in particular to a solution polymerization process of nitroso fluorine rubber polymer (raw rubber), belonging to the technical field of organic fluorine chemistry. Background technique [0002] Nitroso fluororubber (Nitroso Rubber, referred to as NR) is produced by copolymerization of nitrosotrifluoromethane (one monomer), tetrafluoroethylene (two monomers) and vulcanization point monomer (three monomers) at low temperature. Rubber, and then vulcanized and cross-linked to become an elastomer (rubber). Half of the main chain of NR polymer is a carbon-carbon bond (-C-C-), the other half is a nitrogen-oxygen bond (-N-O-), and the carbon atoms are all connected to fluorine atoms, which has good chemical stability; a large number of main chains The nitrogen-oxygen chain link endows rubber with excellent low-temperature resistance; NR has high fluorine content and does not contain C-H bonds. The gas released...

Claims

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Application Information

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IPC IPC(8): C08F214/26C08F2/38C08F2/06
Inventor 邓清田周楠杨晓勇吴勇徐亭罗凯黎爽沈佶原华宋升
Owner CHINA BLUESTAR CHENGRAND CO LTD
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