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Method for producing vulcanizable fluorine-containing elastomer

A manufacturing method and elastomer technology, which is applied in the field of manufacturing fluoroelastomers, can solve the problems of poor productivity, residual sealing, and no special improvement of elastomers, etc., and achieve high productivity, less branched polymer chains, and superior balance Effect

Active Publication Date: 2006-02-22
DAIKIN IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, although it is not necessary to make major changes to the existing emulsion polymerization equipment, uniform particle size can be formed and its original characteristics can be maintained, and the polymerization rate can be shortened by more than 2 times. The productivity is still poor compared to the polymerization method
In addition, compared with the conventional iodine transfer polymerization method, the elastomer obtained by this polymerization method has no special improvement, and the above-mentioned problem of sealing performance remains.
[0011] There is no such manufacturing method for iodine-containing fluoroelastomers that combines productivity and maintenance properties

Method used

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  • Method for producing vulcanizable fluorine-containing elastomer
  • Method for producing vulcanizable fluorine-containing elastomer
  • Method for producing vulcanizable fluorine-containing elastomer

Examples

Experimental program
Comparison scheme
Effect test

reference example 1

[0216] (polymerization of seed polymer particles)

[0217] In a polymerization tank having an electromagnetic induction stirring device as a stirring device with an internal volume of 1.8 liters, add 720 g of pure water, 290 g of 10% by weight of ammonium perfluorooctanoate aqueous solution and 0.6 g of diethyl malonate, and fully replace the system with nitrogen To decompress. This operation was repeated 3 times, 20 g of VdF and 51 g of HFP were added under reduced pressure, and the temperature was raised to 80° C. while stirring. Next, 0.02 g of ammonium persulfate (APS) dissolved in 0.6 g of pure water was blown in with nitrogen to start polymerization. The polymerization pressure was set at 2 MPa, and VdF / HFP mixed monomer (78 / 22 (mol %)) was continuously supplied to compensate for the pressure drop during polymerization, and the polymerization was carried out under stirring. Until the end of the polymerization, 215 g of monomers were supplied into the tank.

[0218] Th...

reference example 2

[0220] (Aggregation of Seed Aggregation Particles)

[0221] In a polymerization tank with an inner volume of 1.8 liters having an electromagnetic induction stirring device as a stirring device, 809 g of pure water and 200 g of a 10% by weight ammonium perfluorooctanoate aqueous solution were added, and the system was fully replaced with nitrogen before depressurization. Repeat this operation 3 times, add 0.5mL isopentane under reduced pressure, and then add each monomer, so that the phase composition at 80°C is VdF / TFE / HFP=29.0 / 13.0 / 58.0 mol%, and the pressure in the tank is 1.4MPa. After the completion of the temperature rise, 0.67 g of ammonium persulfate (APS) dissolved in 20 g of pure water was injected with nitrogen pressure to start polymerization. The polymerization pressure was set at 1.4 MPa, and VdF / TFE / HFP mixed monomer (50 / 20 / 30 (mol %)) was continuously supplied to compensate for pressure drop during polymerization, and polymerization was carried out under stirri...

Embodiment 1

[0224] Add 1324g of pure water, 33.5g of the aqueous dispersion of polymer particles produced in Reference Example 1 and 19.1g of 10% by weight of The aqueous solution of ammonium perfluorooctanoate was decompressed after fully replacing the inside of the system with nitrogen. This operation was repeated three times, 171 g of VdF and 729 g of HFP were added under reduced pressure, and the temperature was raised to 80° C. while stirring. Next, 2.98 g of octafluoro-1,4-diiodobutane and 0.068 g of APS dissolved in 15 g of pure water were injected with nitrogen pressure to initiate polymerization and continue under the conditions of (a), (b) and (c) The polymerization was carried out, and after 4.3 hours, the stirring was stopped, the monomer was released, and the polymerization was stopped.

[0225] (a) Use Aspen Plus Ver.11.1 to calculate the critical temperature and critical pressure by the Peng-Robinson equation for the composition VdF / HFP=36 / 64 (mol %) in the polymerization ...

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Abstract

The present invention provides a process for preparing a fluorine-containing elastomer in a high productivity comparable to that of non-iodine transfer polymerization process by carrying out an iodine transfer polymerization at high pressure. The present invention also provides a fluorine-containing elastomer prepared by this process, and fluorine-containing molded articles. The process is a batch copolymerization process conducted under conditions that the reduced temperature of the critical constant is at least 0.95 and the reduced pressure of the critical constant is at least 0.80 wherein the reduced temperature and the reduced pressure are calculated using the Peng-Robinson formula from the critical temperature, the critical pressure and the composition ratio of each of the monomers in the gaseous phase in a reaction vessel, in which ethylenically unsaturated compounds containing at least one fluoroolefine are copolymerized in the presence of a compound having the formula: Rf<1>.Ix wherein Rf<1> is a saturated or unsaturated fluorohydrocarbon or chlorofluorohydrocarbon group having 1 to 16 carbon atoms, and x is the number of bonds of Rf<1> and an integer of 1 to 4.

Description

technical field [0001] The present invention relates to a process for the manufacture of fluoroelastomers by iodine transfer polymerization at high pressure. Furthermore, it relates to a fluorine-containing elastomer having few elastomer branches and a high terminal iodine content produced by the method, and a fluorine-containing elastomer having an excellent balance of compression set and tensile elongation at break obtained by vulcanizing the elastomer. moldings. Background technique [0002] Vinylidene fluoride-hexafluoropropylene (VdF-HFP) and tetrafluoroethylene (TFE)-perfluoroethylene ether fluoroelastomers exhibit excellent chemical resistance, solvent resistance, and heat resistance, so they are Made of O-rings, gaskets, hoses, rod seals, shaft seals, diaphragms, etc. used in harsh environments, widely used in the automotive industry, semiconductor industry, chemical industry and other fields. [0003] As a fluoroelastomer used for these applications, there is an i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/18
Inventor 西村洋介入江正树入江贞成藤泽学德野敏岸根充
Owner DAIKIN IND LTD
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