CN104497189A - Preparation method of thermally-stable raw fluorubber - Google Patents
Preparation method of thermally-stable raw fluorubber Download PDFInfo
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- CN104497189A CN104497189A CN201410587149.4A CN201410587149A CN104497189A CN 104497189 A CN104497189 A CN 104497189A CN 201410587149 A CN201410587149 A CN 201410587149A CN 104497189 A CN104497189 A CN 104497189A
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Abstract
The invention discloses a preparation method of thermally-stable raw fluorubber. The preparation method comprises the following steps that 100 parts by weight of water, 0.02-0.2 parts by weight of perfluorocapylic acid, 0.1-0.2 parts by weight of a pH conditioning agent, 0.06-0.2 parts by weight of a molecular weight conditioning agent, 0.01-0.02 parts by weight of an initiator and 25-50 parts by weight of mixed monomers of vinylidene fluoride, tetrafluoroethene and perfluoropropylene are put into a reactor, the mixture undergoes a polymerization reaction at a reaction temperature of 20-80 DEG C under reaction pressure of 0.5-0.8MPa, after the reaction, the mixed monomers are recovered, and the produced emulsion is subjected to refrigeration coacervation, washing, extrusion dehydration, vacuum drying and plastication molding to form a thermally-stable raw fluorubber product. The preparation method has simple processes. The thermally-stable raw fluorubber obtained by the preparation method has the advantages of high temperature resistance and excellent elasticity.
Description
Technical field
The present invention relates to the preparation method of viton, be specifically related to a kind of preparation method of thermally-stabilised crude fluororubber.
Background technology
Viton has excellent high-low temperature resistant, oil resistant and chemical-resistant, has been widely used in various sealing member goods.Although common viton all has good resistance to elevated temperatures, its resistance to elevated temperatures cannot be compared with the fluoro-resin of identical type, and more than 300 DEG C, during life-time service, its physical and chemical performance is decayed very block, easy decomposes.Therefore there is the problem how ensureing its good resistance to elevated temperatures while keeping rubber superior elasticity.Prior art mainly carries out study on the modification from post-treatment aspect to the resistance to elevated temperatures of viton.
As China Patent Publication No. CN103613886A, denomination of invention: fluoroelastomer glue stock of a kind of high temperature high voltage resistant and preparation method thereof and application.Fluoroelastomer glue stock of a kind of high temperature high voltage resistant of this disclosure of the invention and preparation method thereof and application.The fluoroelastomer glue stock of described high temperature high voltage resistant comprises the viton of 100 mass parts, the acid-acceptor of 3 ~ 15 mass parts, the filler of 0 ~ 30 mass parts, the processing aid of 0 ~ 3 mass parts, the vulcanizing agent of 0.1 ~ 0.6 mass parts, the aramid pulp of 1 ~ 6 mass parts and 1 ~ 6 mass parts spray carbon black.The viton material that this invention obtains, has good heat-resistant stability and high voltage performance.
And for example China Patent Publication No. CN101307165A, denomination of invention: heat resisting fluororubber composition and sulfidization molding products thereof.A kind of heat resisting fluororubber composition of this disclosure of the invention and sulfidization molding products thereof.This fluoro-rubber composite, it comprises 100 weight part viton, 0.1 ~ 10 weight part rare-earth oxide and 0.05 ~ 10 weight part vulcanizing agent.After the fluoro-rubber composite sulfidization molding of this invention, there is good resistance toheat.
Above prior art is all the post-processing stages such as compounding rubber in the later stage, the resistance to elevated temperatures of viton is improved by adding various auxiliary agent, its weak point is that technique is loaded down with trivial details, various auxiliary agent add the processing characteristics and mechanical property that have impact on viton, cause tensile strength and elongation at break to decline more.
Summary of the invention
Instant invention overcomes the defect of prior art, provide the preparation method of the thermally-stabilised crude fluororubber of simple, the obtained product resistance to elevated temperatures of a kind of technique and excellent spring.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions: a kind of preparation method of thermally-stabilised crude fluororubber, comprises the following steps:
A () adds water in reactor, the add-on of described water is 50 ~ 70% of reactor volume, by weight, the water added in reactor is counted 100 parts, 0.02 ~ 0.2 part of Perfluorocaprylic Acid is added by every 100 parts of water, 0.1 ~ 0.2 part of pH adjusting agent, raw material for standby chosen by 0.06 ~ 0.2 part of molecular weight regulator and 0.01 ~ 0.02 part of initiator;
B () adds the Perfluorocaprylic Acid aqueous solution and the pH adjusting agent aqueous solution by the composition by weight determined in reactor;
C () is warming up to 20 ~ 80 DEG C by after reactor deoxygenation;
D () adds vinylidene, tetrafluoroethylene and perfluoro propylene mix monomer to reactor pressure in reactor is 0.5 ~ 0.8MPa, then adds initiator solution by the composition by weight determined and molecular weight regulator starts polyreaction;
E (), in polymerization process, is added vinylidene, tetrafluoroethylene and perfluoro propylene mix monomer separately and is maintained reactor constant voltage;
F () terminates to react when component reaches 25-50 part with the ratio of the water of 100 parts by weight when the amount of the vinylidene added, tetrafluoroethylene and perfluoro propylene mix monomer, reclaim mix monomer, by the emulsion obtained through freeze agglomeration, washing, extruding dehydration, vacuum-drying and plasticating shapingly obtains thermally-stabilised crude fluororubber product.
Further:
Described vinylidene, tetrafluoroethylene and perfluoro propylene mix monomer composition is preferably: the vinylidene of 30 ~ 50mol%, the perfluoro propylene of 15 ~ 40mol%, the tetrafluoroethylene of 10 ~ 50mol%.
Described initiator is preferably one or both the mixture in S-WAT, sodium phosphate, ammonium persulphate.
Described molecular weight regulator is preferably the one in methyl alcohol, ethanol, diethyl malonate.
Described pH adjusting agent is preferably the one in dipotassium hydrogen phosphate, sodium carbonate, sodium bicarbonate, Sodium Tetraborate.
The present invention is using water as dispersion medium, and free-radical emulsion polymerization mode under employing low-temp low-pressure, obtains the viton with excellent resistance to elevated temperatures.In the present invention, the add-on of water medium will make to leave in reactor the vapour space being enough to receive gaseous state mix monomer, and therefore in the present invention, the add-on of water is 50 ~ 70% of reactor volume, is preferably 60% of reactor volume.
Through free-radical emulsion polymerization mode, the polymerized emulsion obtained need carry out postprocessing working procedures.In last handling process, prior art generally adopts and adds electrolytical mode and condense, but requires that its foreign matter content is low in use due to the viton of preparation, adopts to add electrolytical method and carry out the purity that aftertreatment can reduce rubber, thus affects its performance.Therefore the present invention adopts the mode of freeze agglomeration; by low temperature, by emulsion, water congeals into ice; the formation of ice limits the pedesis of material particles; destroy the protective membrane of particle surface; rubber grain after thawing, flocking settling and water stratification under gravity, thus decrease the foreign matter content caused because adding ionogen; ensure the purity of rubber, for post-production and use provide good base mateiral.
Rubber after washing is the conventional drying mode in this area by putting into oven drying after centrifugal, but the preparation of rubber item needs water-content lower to prevent the end group in mixing process to be hydrolyzed.Therefore, the rubber washed is undertaken extruding free water a large amount of in dry removal rubber by twin screw extruder by the present invention, then makes water-content below 0.01% by vacuum drying oven drying, can effectively prevent the end group in mixing process to be hydrolyzed.
Of the present invention plasticate shaping can on opening rubber mixing machine, adopt the conventional processing conditions in this area to carry out.
1, preparation method's technique is simple, and environmental protection, is suitable for large-scale industrial production;
2, the product good mechanical performance prepared, tensile strength is at more than 11MPa, and elongation at break is more than 200%;
3, the product resistance to elevated temperatures prepared is good, and heat decomposition temperature is more than 400 DEG C.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but the present invention is not only confined to following examples.
Embodiment 1: first add 30kg (volume 30L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 500g10wt%, 500g10wt% sodium hydrogen carbonate solution, then the deoxygenation of reactor nitrogen is warming up to 80 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 45mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 40mol%, perfluoro propylene 15mol%) to reactor pressure be 0.8MPa, open to stir and mix monomer is fully mixed, add the ammonium persulfate solution of 500g1wt% again, 20g ethanolic soln starts reaction.Reactor pressure is kept to be 0.8MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 15kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 2: first add 30kg (volume 30L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 400g10wt%, 500g10wt% sodium carbonate solution, then the deoxygenation of reactor nitrogen is warming up to 60 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 40mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 45mol%, perfluoro propylene 15mol%) to reactor pressure be 0.7MPa, open to stir and mix monomer is fully mixed, add the S-WAT of 500g1wt% and the mixing solutions of sodium phosphate again, 20g methanol solution starts reaction.Reactor pressure is kept to be 0.7MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 12kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 3: first add 30kg (volume 30L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 300g10wt%, 500g10wt% dipotassium hydrogen phosphate solution, then the deoxygenation of reactor nitrogen is warming up to 40 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 45mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 40mol%, perfluoro propylene 15mol%) to reactor pressure be 0.6MPa, open to stir and mix monomer is fully mixed, add the potassium persulfate solution of 500g1wt% again, 20g methanol solution starts reaction.Reactor pressure is kept to be 0.6MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 15kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 4: first add 25kg (volume 25L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 200g10wt%, 500g10wt% dobell's solution, then the deoxygenation of reactor nitrogen is warming up to 20 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 45mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 40mol%, perfluoro propylene 15mol%) to reactor pressure be 0.5MPa, open to stir and mix monomer is fully mixed, add the S-WAT of 500g1wt% and the mixing solutions of sodium phosphate again, 50g ethanolic soln starts reaction.Reactor pressure is kept to be 0.5MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 12kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 5: first add 25kg (volume 25L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 100g10wt%, 500g10wt% dobell's solution, then the deoxygenation of reactor nitrogen is warming up to 80 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 30mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 50mol%, perfluoro propylene 20mol%) to reactor pressure be 0.5MPa, open to stir and mix monomer is fully mixed, add the S-WAT of 500g1wt% and the mixing solutions of sodium phosphate again, 50g ethanolic soln starts reaction.Reactor pressure is kept to be 0.5MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 12kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 6: first add 25kg (volume 25L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 400g10wt%, 500g10wt% sodium hydrogen carbonate solution, then the deoxygenation of reactor nitrogen is warming up to 70 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 35mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 40mol%, perfluoro propylene 25mol%) to reactor pressure be 0.8MPa, open to stir and mix monomer is fully mixed, add the S-WAT of 500g1wt% and the mixing solutions of sodium phosphate again, 50g ethanolic soln starts reaction.Reactor pressure is kept to be 0.8MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 12kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 7: first add 35kg (volume 35L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 300g10wt%, 500g10wt% sodium carbonate solution, then the deoxygenation of reactor nitrogen is warming up to 50 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 40mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 30mol%, perfluoro propylene 30mol%) to reactor pressure be 0.7MPa, open to stir and mix monomer is fully mixed, add the S-WAT of 500g1wt% and the mixing solutions of sodium phosphate again, 50g diethyl malonate solution starts reaction.Reactor pressure is kept to be 0.7MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 10kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 8: first add 35kg (volume 35L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 200g10wt%, 500g10wt% dipotassium hydrogen phosphate solution, then the deoxygenation of reactor nitrogen is warming up to 40 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 45mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 20mol%, perfluoro propylene 35mol%) to reactor pressure be 0.6MPa, open to stir and mix monomer is fully mixed, add the potassium persulfate solution of 500g1wt% again, 50g diethyl malonate solution starts reaction.Reactor pressure is kept to be 0.6MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 12kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
Embodiment 9: first add 35kg (volume 35L) water in the reactor of 50L, the Perfluorocaprylic Acid solution of 100g10wt%, 500g10wt% dobell's solution, then the deoxygenation of reactor nitrogen is warming up to 30 DEG C after oxygen level is less than 50ppm, then (mix monomer consists of: vinylidene 50mol% in reactor, to add mix monomer with membrane compressor, tetrafluoroethylene 10mol%, perfluoro propylene 40mol%) to reactor pressure be 0.5MPa, open to stir and mix monomer is fully mixed, add the potassium persulfate solution of 500g1wt% again, 50g diethyl malonate solution starts reaction.Reactor pressure is kept to be 0.5MPa by adding mix monomer continuously in reaction process.The stopped reaction when mix monomer total feed reaches 10kg, reclaim mix monomer, wash after the emulsion obtained is carried out freeze agglomeration in-35 DEG C of freezing alcohol troughs, after again the rubber washed being undertaken extruding dehydration by twin screw extruder, put into baking oven vacuum-drying to water-content below 0.01%, last plasticating on opening rubber mixing machine shapingly obtains thermostability crude fluororubber product, and performance is in table 1.
The thermally-stabilised crude fluororubber product obtained to embodiment 1-9 carries out performance test, the results are shown in Table 1.Wherein:
Stretching strength determination is pressed GB/T528-2009 and is performed, and extension at break measures presses GB/T528-2009 execution, and heat decomposition temperature adopts thermogravimetry TG; Instrument model: TG 209F1.
The thermally-stabilised crude fluororubber product performance test result that table 1 embodiment 1-9 is obtained
Claims (5)
1. a preparation method for thermally-stabilised crude fluororubber, is characterized in that comprising the following steps:
A () adds water in reactor, the add-on of described water is 50 ~ 70% of reactor volume, by weight, the water added in reactor is counted 100 parts, 0.02 ~ 0.2 part of Perfluorocaprylic Acid is added by every 100 parts of water, 0.1 ~ 0.2 part of pH adjusting agent, raw material for standby chosen by 0.06 ~ 0.2 part of molecular weight regulator and 0.01 ~ 0.02 part of initiator;
B () adds the Perfluorocaprylic Acid aqueous solution and the pH adjusting agent aqueous solution by the composition by weight determined in reactor;
C () is warming up to 20 ~ 80 DEG C by after reactor deoxygenation;
D () adds vinylidene, tetrafluoroethylene and perfluoro propylene mix monomer to reactor pressure in reactor is 0.5 ~ 0.8MPa, then adds initiator solution by the composition by weight determined and molecular weight regulator starts polyreaction;
E (), in polymerization process, is added vinylidene, tetrafluoroethylene and perfluoro propylene mix monomer separately and is maintained reactor constant voltage;
F () terminates to react when component reaches 25-50 part with the ratio of the water of 100 parts by weight when the amount of the vinylidene added, tetrafluoroethylene and perfluoro propylene mix monomer, reclaim mix monomer, by the emulsion obtained through freeze agglomeration, washing, extruding dehydration, vacuum-drying and plasticating shapingly obtains thermally-stabilised crude fluororubber product.
2. the preparation method of thermally-stabilised crude fluororubber according to claim 1, it is characterized in that described vinylidene, tetrafluoroethylene and perfluoro propylene mix monomer consist of: the vinylidene of 30 ~ 50mol%, the perfluoro propylene of 15 ~ 40mol%, the tetrafluoroethylene of 10 ~ 50mol%.
3. the preparation method of thermally-stabilised crude fluororubber according to claim 1, is characterized in that described initiator is one or both the mixture in S-WAT, sodium phosphate, ammonium persulphate.
4. the preparation method of thermally-stabilised crude fluororubber according to claim 1, is characterized in that described molecular weight regulator is the one in methyl alcohol, ethanol, diethyl malonate.
5. the preparation method of thermally-stabilised crude fluororubber according to claim 1, is characterized in that described pH adjusting agent is the one in dipotassium hydrogen phosphate, sodium carbonate, sodium bicarbonate, Sodium Tetraborate.
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| CN107868145A (en) * | 2016-09-26 | 2018-04-03 | 中昊晨光化工研究院有限公司 | A kind of fluorine resin F2314 cohesion washing methods |
| CN113501903A (en) * | 2021-07-30 | 2021-10-15 | 浙江巨圣氟化学有限公司 | Preparation method of high-elasticity fluororubber raw rubber |
| CN113736003A (en) * | 2021-09-06 | 2021-12-03 | 浙江巨化股份有限公司氟聚厂 | Method for modifying polytetrafluoroethylene resin by perfluorovinyl ethers |
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| CN113736003A (en) * | 2021-09-06 | 2021-12-03 | 浙江巨化股份有限公司氟聚厂 | Method for modifying polytetrafluoroethylene resin by perfluorovinyl ethers |
| CN113736003B (en) * | 2021-09-06 | 2022-11-25 | 浙江巨化股份有限公司氟聚厂 | Method for modifying polytetrafluoroethylene resin by perfluorovinyl ethers |
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Application publication date: 20150408 |