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Preparation method for preparing type 26 fluororubber from fluoroether sulfonate

A technology of fluoroethersulfonate and fluororubber, which is applied in the field of preparation of 26-type fluororubber by using fluoroethersulfonate, which can solve the problems of poor strength of fluororubber, difficult degradation of perfluorooctanoic acid, uneven vulcanization, etc.

Active Publication Date: 2015-02-18
ZHEJIANG FLUORINE CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, scientists have found that perfluorooctanoic acid and its derivatives are difficult to degrade from the environment and will affect the growth and development of organisms. Therefore, perfluorooctanoic acid and its derivatives are gradually banned from being used in the production of fluoropolymers, and green PFOA substitutes are developed to become fluoropolymers. The inevitable task of the enterprise
In order to avoid the use of perfluorooctanoic acid, domestic fluororubber manufacturers have been researching and developing perfluorooctanoic acid substitutes, but there are also problems such as too fast polymerization reaction speed, too small molecular weight of fluororubber, poor strength of fluororubber produced by polymerization, uneven vulcanization, affecting the performance of the final product, etc. question

Method used

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  • Preparation method for preparing type 26 fluororubber from fluoroether sulfonate
  • Preparation method for preparing type 26 fluororubber from fluoroether sulfonate
  • Preparation method for preparing type 26 fluororubber from fluoroether sulfonate

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Experimental program
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Effect test

Embodiment 1

[0027] Add 6kg of deionized water into the 10L polymerization reactor, and then replace the oxygen in the reactor with nitrogen to make the oxygen content in the reactor lower than 10ppm, then add 20g of fluoroether sulfonate, 10g of disodium hydrogen phosphate, and 0.5kg of six Fluoropropene, 2kg vinylidene fluoride, turn on the stirring paddle at a speed of 250r / min, heat up to 90°C, pour 10g of potassium persulfate into the reaction kettle with a metering pump to initiate the polymerization reaction, and continuously add mass to the reaction kettle through the middle tank Hexafluoropropylene / vinylidene fluoride mixed gas with a ratio of 5 / 12, maintain the reaction pressure at 4MPa, add 10g of diethyl malonate to the reaction kettle after 30 minutes, complete the polymerization reaction after 2.5 hours, and recover unreacted mixed monomers , the emulsion in the reactor is transported to the emulsion tank through the pressure control valve, 6g of calcium chloride powder is add...

Embodiment 2

[0029] Add 5.5kg of deionized water to a 10L polymerization reactor, then add 3.5g of fluoroether sulfonate, 3.5g of disodium hydrogen phosphate, 0.7kg of hexafluoropropylene, 2.5kg of vinylidene fluoride, and turn on the stirring paddle at a speed of 350r / min, heat up to 50°C, pour 3.2g of potassium persulfate into the reaction kettle with a metering pump to initiate the polymerization reaction, and continuously add hexafluoropropylene / vinylidene fluoride mixture with a mass ratio of 7 / 25 to the reaction kettle through the middle tank gas, maintain the reaction pressure to be 3MPa, add diethyl malonate 5g in the reactor after 10min, finish the polymerization reaction after 1 hour, reclaim a small amount of unreacted mixed monomer, and the emulsion in the reactor is delivered to In the emulsion tank, add 10g of calcium chloride powder for coagulation, and then the solid matter enters the washing tank for washing. After washing, the block-shaped finished product is placed in a ...

Embodiment 3

[0031]Add 6kg of deionized water to a 10L polymerization reactor, add 42.5g of fluoroether sulfonate, 8.5g of disodium hydrogen phosphate, 0.7kg of hexafluoropropylene, and 1kg of vinylidene fluoride to ensure that the oxygen content in the kettle is lower than 10ppm, and then open Stirring paddle, the rotating speed is 700r / min, the temperature is raised to 120°C, inject 34g of potassium persulfate into the reaction kettle with a metering pump to initiate the polymerization reaction, and continuously add hexafluoropropylene with a mass ratio of 7 / 10 to the reaction kettle through the middle tank / vinylidene fluoride mixed gas, maintain the reaction pressure at 7MPa, add 39g of diethyl malonate to the reactor after 20min, end the polymerization reaction after 2.5 hours, recover a small amount of unreacted mixed monomer, and turn the reactor to The emulsion in the emulsion is transported to the emulsion tank, and 9.4g of calcium chloride powder is added for coagulation, and then...

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Abstract

The invention provides a preparation method for preparing type 26 fluororubber from a fluoroether sulfonate and belongs to the technical field of synthesis of the high polymer material fluoroelastomers. The preparation method comprises the following steps: 1) blowing nitrogen into an airtight polymerization reaction kettle to remove oxygen, and adding deionized water, an emulsifier, disodium hydrogen phosphate, potassium persulfate, diethyl malonate, vinylidene fluoride and hexafluoropropylene, wherein the emulsifier is the fluoroether sulfonate; 2) reacting under the pressure of 3.0-7.0Mpa and at a temperature ranging from 50 to 120 DEG C, starting a mixing propeller at a rotating speed of 300-700r / min, and ending the reaction after 0.5-2.5 hours, thereby obtaining fluororubber latex; 3) coagulating by use of calcium chloride, washing the coagulated solid particles by use of deionized water until the bubble disappears, and drying in vacuum to obtain the finished product. The preparation method for preparing the type 26 fluororubber from the fluoroether sulfonate has the advantages of increasing the molecular weight of the fluororubber, improving the molecular weight distribution and the mechanical properties of the fluororubber, and protecting the environment.

Description

technical field [0001] The invention belongs to the technical field of polymer material fluoroelastomer synthesis, in particular to a method for preparing 26-type fluororubber by using fluoroether sulfonate. Background technique [0002] Type 26 fluoroelastomer refers to a binary polymer fluoroelastomer formed by copolymerization of vinylidene fluoride (VDF) and hexafluoropropylene (HFP) mixed monomers in a certain proportion under the action of an emulsifier. It has excellent chemical resistance , heat resistance and physical and mechanical properties, are widely used in sealing rings, gaskets, oil seals and other fields. [0003] At present, perfluorooctanoic acid and its derivatives are used as emulsifiers in the production of 26-type fluororubber. Its main function is to uniformly disperse the primary particles of fluororubber to ensure the stability of the fluororubber emulsion. It is a necessary additive for the industrial production of 26-type fluororubber. However, ...

Claims

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Application Information

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IPC IPC(8): C08F214/22C08F214/28C08F2/26C08F6/22
Inventor 苗国祥
Owner ZHEJIANG FLUORINE CHEM NEW MATERIAL
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