Low compression set peroxide vulcanized fluorine rubber and preparation method thereof
A technology of vulcanizing fluororubber and peroxide, applied in the field of fluororubber synthesis, can solve the problems of inability to use movable or fixed seals, narrow relative molecular weight distribution, large compression set value, etc., and achieve excellent mechanical and dielectric properties, The effect of shortening the vulcanization time and reducing the compression set value
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Embodiment 1
[0057] This embodiment relates to a preparation method of peroxide vulcanized fluororubber with low compression set, comprising the following steps:
[0058] 1) In a 50L stainless steel vertical reaction kettle, add 33.3L of deionized water, blow nitrogen and deoxygenate three times, evacuate until the oxygen content is less than or equal to 25ppm, add 80g of fluorine-containing compound emulsifier microemulsion, 20g of dipotassium hydrogen phosphate, 40g of three Bromofluoroethylene;
[0059] 2) Turn on stirring at a speed of 200rpm, heat up to 60°C, add vinylidene fluoride, tetrafluoroethylene and HFP mixed monomers to 2MPa according to the ratio of the amount of substances 70 / 10 / 20, and after the system is stable, pass 10g through the metering pump Potassium sulfate was added to the reactor to start the polymerization reaction. Simultaneously add mixed monomer constantly to keep reactor pressure 2MPa, after conversion rate reaches 15%, add 40g of 1,4-diiodoperfluorobutane ...
Embodiment 2
[0062] This embodiment relates to a preparation method of peroxide vulcanized fluororubber with low compression set, comprising the following steps:
[0063] 1) In a 50L stainless steel vertical reaction kettle, add 33.3L of deionized water, blow nitrogen and deoxygenate three times, evacuate until the oxygen content is less than or equal to 25ppm, add 80g of fluorine-containing compound emulsifier microemulsion, 20g of dipotassium hydrogen phosphate, 40g of three Bromofluoroethylene;
[0064] 2) Turn on stirring at a speed of 200rpm, heat up to 60°C, add VDF / HFP=55 / 45 (molar ratio) mixed monomer, increase the pressure to 2MPa at 80°C, and press in 10g of 15% (wt) through a metering pump Aqueous ammonium persulfate solution was used to initiate the polymerization reaction, and then a mixed monomer of VDF / HFP=82 / 18 (molar ratio) was added to maintain the reaction pressure at 2.0 MPa. When the conversion rate reaches 20%, add 40g of 1,4-diiodoperfluorobutane to the reactor;
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Embodiment 3
[0067] This embodiment relates to a preparation method of peroxide vulcanized fluororubber with low compression set, comprising the following steps:
[0068] 1) In a 50L stainless steel vertical reaction kettle, add 33.3L of deionized water, blow nitrogen and deoxygenate three times, evacuate until the oxygen content is less than or equal to 25ppm, add 80g of fluorine-containing compound emulsifier microemulsion, 20g of dipotassium hydrogen phosphate, 40g of three Bromofluoroethylene;
[0069] 2) Start stirring at a speed of 200rpm, heat up to 60°C, add a mixed monomer of TFE / VDF / HFP=4 / 60 / 36 (molar ratio), increase the pressure to 2MPa at 80°C, and press in 10g of 15 % (wt) ammonium persulfate aqueous solution to initiate the polymerization reaction, and then add a mixed monomer of TFE / VDF / HFP=6.3 / 77.2 / 16.5 (molar ratio) to maintain the reaction pressure at 2.0 MPa. When the conversion rate reaches 30%, add 40g of 1,4-diiodoperfluorobutane to the reactor;
[0070] 3) Stop th...
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Abstract
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