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Peroxide vulcanized fluororubber and polymerizing method thereof

A technology of vulcanized fluororubber and polymerization method, which is applied in the field of fluorine chemical industry, which can solve the problems of limited application range, slow polymerization reaction speed, high permanent compression deformation of peroxidized vulcanized fluororubber, and achieve the effect of increasing reaction rate and improving dispersibility

Active Publication Date: 2017-06-30
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent CN201210307846.0 discloses a method for preparing alkali-resistant vulcanized fluororubber. The disadvantage of this method is that the polymerization reaction speed is slow, the polymerization time is long, and the industrial production cost is high.
The permanent compression set of peroxidized vulcanized fluororubber synthesized by this method is relatively high, which limits the scope of application

Method used

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  • Peroxide vulcanized fluororubber and polymerizing method thereof
  • Peroxide vulcanized fluororubber and polymerizing method thereof

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Effect test

Embodiment 1

[0046] A kind of polymerization method of peroxide vulcanized fluororubber, comprises the steps:

[0047] 1) The ionic surface active CF 3 -CF 2 -CF 2 -O-(CF 2 -CF 2 -O) 2 -CF 2 -COOH, polyoxyethylene oleate, fluoroether oil (CF 3 -CF 2 -CF 2 -O-(CF 2 -CF 2 -O) 2 -CF 3 ), water according to the weight ratio (16:14:4:66), gently stirred and heated to 40-45°C and mixed evenly to form a colorless and transparent microemulsion with a weight of 500g.

[0048] 2) Carry out intermittent free radical emulsion polymerization of the present invention in a 50L high-pressure reactor to prepare fluororubber: add 30L deionized water and 50g of pH regulator disodium hydrogen phosphate in the reactor, and the pH of the system is 8~ 9. Replace the air in the reactor with nitrogen first, and then replace the nitrogen with mixed monomers to make the oxygen content less than 20ppm.

[0049] 3) The temperature of the reaction kettle was raised to 95° C., and 250 g of the above-mentio...

Embodiment 2

[0056] Adopt the method for embodiment 1 to prepare peroxide vulcanized fluororubber, difference is: in step (1), described microemulsion is made by following formula:

[0057] Ionic surfactant CF 3 -CF 2 -CF 2 -O-(CF 2 -CF 2 -O) 2 -CF 2 -COOH, polyoxyethylene oleate, fluoroether oil (CF 3 -CF 2 -CF 2 -O-(CF 2 -CF 2 -O) 2 -CF 3 ), water is mixed according to the weight ratio of 20:14:5:61.

Embodiment 3

[0059] Adopt the method for embodiment 1 to prepare peroxide vulcanized fluororubber, difference is: in step (1), described microemulsion is made by following formula:

[0060] Ionic surfactant CF 3 -CF 2 -CF 2 -O-(CF 2 -CF 2 -O) 2 -CF 2 -COOH, polyoxyethylene oleate, fluoroether oil (CF 3 -CF 2 -CF 2 -O-(CF 2 -CF 2 -O) 2 -CF 3 ), water is mixed according to the weight ratio of 11:12:3:74.

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Abstract

The invention relates to peroxide vulcanized fluororubber and a polymerizing method thereof. The polymerizing method comprises the following steps: (1) mixing an emulsifier, hydrofluoroether oil and water and heating to form colorless and transparent microemulsion; (2) adding water and a pH regulator into a reactor until system pH is 8 to 9, firstly utilizing nitrogen to displace air in the reactor, and then introducing mixed gas to displace nitrogen; (3) adding the microemulsion into the reactor, continuing introducing mixed monomer, adding an initiator and a chain transfer agent and starting polymerization reaction; (4) adding a vulcanization point monomer to react continuously when the mixed monomer reacts and reaches certain accumulative reacting weight; (5) agglomerating, washing and drying obtained polymerized emulsion, plastifying and shaping, and packaging to obtain the fluororubber. The polymerizing method disclosed by the invention improves a reaction rate by improving a configuring mode of the emulsifier, adjusting adding time and an adding mode of the vulcanization point monomer and the like, and improves vulcanizing performance of the peroxide vulcanized fluororubber.

Description

technical field [0001] The invention relates to a peroxide vulcanized fluorine rubber and a polymerization method thereof, belonging to the technical field of fluorine chemical industry. Background technique [0002] There are many kinds of fluorine rubber, and their chemical cross-linking is also different, but their cross-linking mechanism can be attributed to the following two types: ionic type and free radical type. Ionic types include amine vulcanization and bisphenol vulcanization, while free radical types include organic peroxide vulcanization and radiation crosslinking vulcanization. Peroxide system fluorine rubber is vulcanized in the form of free radical crosslinking, which includes the following two processes: (1) Decompose peroxide by heating to generate free radicals, and then absorb on the tertiary carbon atoms in the polymer chain H or the active point on the cross-linking point monomer to form a polymer radical; (2) The polymer radical forms a cross-link bon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F214/28C08F214/26C08F2/26C08F2/30C08F4/30
CPCC08F2/26C08F2/30C08F4/30C08F214/22C08F214/28C08F214/26
Inventor 贾如华吴常根朱健全程明
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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