CN110218405A - A kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its application - Google Patents
A kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its application Download PDFInfo
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- CN110218405A CN110218405A CN201910386804.2A CN201910386804A CN110218405A CN 110218405 A CN110218405 A CN 110218405A CN 201910386804 A CN201910386804 A CN 201910386804A CN 110218405 A CN110218405 A CN 110218405A
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- 229920001973 fluoroelastomer Polymers 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 35
- 238000005260 corrosion Methods 0.000 title claims abstract description 30
- 230000007797 corrosion Effects 0.000 title claims abstract description 30
- 229920001971 elastomer Polymers 0.000 claims abstract description 59
- 239000005060 rubber Substances 0.000 claims abstract description 58
- 239000007789 gas Substances 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 18
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 18
- 238000007789 sealing Methods 0.000 claims abstract description 15
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 8
- 239000011593 sulfur Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000002250 absorbent Substances 0.000 claims abstract description 5
- 230000002745 absorbent Effects 0.000 claims abstract description 5
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229920003249 vinylidene fluoride hexafluoropropylene elastomer Polymers 0.000 claims description 20
- 239000006229 carbon black Substances 0.000 claims description 18
- 229920000642 polymer Polymers 0.000 claims description 18
- 239000000178 monomer Substances 0.000 claims description 13
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 9
- 229920002449 FKM Polymers 0.000 claims description 9
- -1 perfluoromethylvinyl Chemical group 0.000 claims description 7
- 229920001774 Perfluoroether Polymers 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical group CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 239000002109 single walled nanotube Substances 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 claims 5
- 229920002554 vinyl polymer Polymers 0.000 claims 4
- IYABWNGZIDDRAK-UHFFFAOYSA-N allene Chemical group C=C=C IYABWNGZIDDRAK-UHFFFAOYSA-N 0.000 claims 1
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 35
- 230000000694 effects Effects 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 description 17
- 239000000203 mixture Substances 0.000 description 13
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 10
- 239000011737 fluorine Substances 0.000 description 10
- 229910052731 fluorine Inorganic materials 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 238000011056 performance test Methods 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 238000007792 addition Methods 0.000 description 4
- 238000004073 vulcanization Methods 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- UJNVTDGCOKFBKM-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)hexane Chemical compound CCCCCC(OOC(C)(C)C)OOC(C)(C)C UJNVTDGCOKFBKM-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 2
- 229920005560 fluorosilicone rubber Polymers 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- BLTXWCKMNMYXEA-UHFFFAOYSA-N 1,1,2-trifluoro-2-(trifluoromethoxy)ethene Chemical compound FC(F)=C(F)OC(F)(F)F BLTXWCKMNMYXEA-UHFFFAOYSA-N 0.000 description 1
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 1
- 229920006169 Perfluoroelastomer Polymers 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229920006172 Tetrafluoroethylene propylene Polymers 0.000 description 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical class C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009778 extrusion testing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004643 material aging Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The present invention relates to High-molecular rubber material, fluoro-rubber composite and its application of a kind of hydrogen sulfide corrosion-resistant are disclosed.The fluoro-rubber composite is prepared by the raw material of following parts by weight: 100 parts of fluorubber, 1-3 parts of crosslinking agents, 1-8 parts of promotors, 1-5 parts of acid absorbents, 0-15 parts of carbon nanotubes, 1-60 parts of fillers, 1-3 parts of processing aids.Fluoro-rubber composite of the invention has excellent high-concentration hydrogen sulfide corrosion resistance, and low temperature seal performance, fluoro-rubber composite formula of the invention rationally, substantially increases the sealing effect of sealing element used in the high sulfur-bearing operating condition in industrial gas oil underground.
Description
Technical field
The present invention relates to High-molecular rubber materials, and in particular to a kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its answers
With.
Background technique
As oil gas drilling depth gradually increases, oily gas ingredients and pressure condition become increasingly complex, as a result, oil gas
More stringent requirements are proposed to related rubber packing material for drilling, transmission and processing technology relevant device.In recent decades, contain
The oil gas field of hydrogen sulfide corrosion medium occurs in succession, and corrosion not only causes huge economic loss to the exploitation of oil gas field, production,
Environmental pollution is also resulted in simultaneously, since hydrogen sulfide is toxic, also threatens personal safety.In recent years in China's investigation and prospecting constantly
It was found that high Oil & gas field in sulfur, such as the general light in southwest, the gas field Yuan Ba, the concentration of hydrogen sulfide in work condition environment is even close
20%.High sulfur-bearing operating condition can constantly corrode rubber packing material, and then lead to the seal failure of rubber material, lead to sulfur-bearing
Change the serious accident that hydrogen natural gas leaks.As it can be seen that under high sulfur-bearing operating condition, the reliable rubber material of resistance to hydrogen sulfide and sealing
Part is particularly significant.
Fluorubber (FPM) is fluorine rubber polymer, and it is poly- that U.S.'s ASTM D1418 standard divides this kind of fluorine-containing rubber
Conjunction object is FPM, is a kind of common rubber material for oil gas field sealing.Yang Xiaolu et al. (acid-resisting medium of rubber o-ring
Corrosive nature, China Synthetic Rubber Industry, 2012,35 (6): 420-424) have studied fluorocarbon rubber, fluorine silicone rubber and tetrapropanate fluorine rubber
Hydrogen sulfide corrosion-resistant performance, the results showed that tetrapropanate fluorine rubber have good acid gas corrosive nature, fluorocarbon rubber and
Fluorine silicone rubber corrosion is serious.Lu Shaojie et al. (influence of the vulcanizing system to fluororubber 26 ageing-resistant performance in hydrogen-sulfide environmental,
Synthesis material aging and application, 2013,42 (2): 1-3) have studied 3# vulcanizing agent, bisphenol AF/tri- kinds of BPP, DCP/TAIC vulcanization
The corrosive nature of the resistance to hydrogen sulfide of fluororubber 26 of system vulcanization, the results showed that the fluororubber 26 material volume of three kinds of vulcanizing systems becomes
Rate is all larger than 20%, is difficult to meet under high-concentration hydrogen sulfide environment and uses.Chinese patent CN102250437B discloses one kind
Acidproof, alkaline-resisting and hydrogen sulfide corrosion-resistant tetrapropanate fluorine rubber (FEPM) composition, the composition can be used for preparing hydrogen-sulfide environmental
Used in rubber product.Chinese patent CN102140189B discloses a kind of hydrogenated nitrile-butadiene rubber combination of hydrogen sulfide corrosion-resistant
Object uses the rubber product of the composition in 100 DEG C, pressure to there is in the hydrogen-sulfide environmental of 6.9MPa preferable resistance to hydrogen sulfide rotten
Corrosion energy.
In terms of the above-mentioned published patent and document report, the rubber material of resistance to sulfidation corrosion is substantially with tetrapropanate fluorine rubber, hydrogen
Change based on nitrile rubber or expensive perfluoroelastomers, fluorubber does not have reliable technology path and method to be made and can expire
The fluorubber material and product used under sufficient high-concentration hydrogen sulfide operating condition.But tetrapropanate fluorine rubber is due to the poor (glass of resistance to low temperature
Changing transition temperature is -3 DEG C or so), the characteristics such as compression set is larger, using limited；Although hydrogenated nitrile-butadiene rubber highest makes
With temperature up to 180 DEG C, but long-term use temperature is only 150 DEG C, and the another corrosivity such as resistance to oil gas and organic solvent are general, using
It is limited；Fluorubber has excellent resistance to oil gas and chemical solvent, also more broad using -60 DEG C~230 DEG C of temperature, is oil gas
The common rubber material in field.In view of the current people understanding bad to fluorubber hydrogen sulfide corrosion-resistant performance, our also never phases
It hopes and develops the fluorubber material of hydrogen sulfide corrosion-resistant, however we are during study lower temperature resistance fluorubber, in surprise
It was found that the low form fluorubber containing perfluoro methyl vinyl ether monomer or perfluoroalkoxy methylene vinyl ether monomers not only has
There is excellent resistance to low temperature, and resisting high-concentration hydrogen sulfide corrosion performance is also very excellent.
Summary of the invention
In order to solve the problems, such as that fluorubber hydrogen sulfide corrosion-resistant performance is bad in the prior art, the present invention provides a kind of resistance to
The fluoro-rubber composite of hydrogen sulfide corrosion.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant, is prepared by the raw material of following parts by weight:
Fluorubber is that vinylidene fluoride (VDF)-tetrafluoroethene (TFE)-perfluoro methyl vinyl ether (PMVE)-vulcanization point is single
Body (CSM) polymer, vinylidene fluoride (VDF)-hexafluoropropene (HFP)-tetrafluoroethene (TFE)-ethylene (E)-perfluoro-methyl second
Alkene ether (PMVE)-cure site monomer (CSM) polymer, vinylidene fluoride (VDF)-perfluoroalkoxy methylene vinyl ethers
(PMOVE)-cure site monomer (CSM) polymer.
Preferably, the vinylidene fluoride (VDF)-tetrafluoroethene (TFE)-perfluoro methyl vinyl ether (PMVE)-sulphur
Changing point monomer (CSM) polymer is Viton GLT600S, Viton GLT200S, Tecnoflon PL855 or Tecnoflon
One of PL455；The vinylidene fluoride (VDF)-hexafluoropropene (HFP)-tetrafluoroethene (TFE)-ethylene (E)-perfluor first
Base vinyl ethers (PMVE)-cure site monomer (CSM) polymer is Tecnoflon BR9151；The vinylidene fluoride
(VDF)-perfluoroalkoxy methylene vinyl ethers (PMOVE)-cure site monomer (CSM) polymer is Tecnoflon
One of VPL85540, Tecnoflon VPL55540, Tecnoflon VPLX75545 or Tecnoflon VPLX65455.
Preferably, the crosslinking agent is 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane.
Preferably, the promotor is Triallyl isocyanurate (TAIC).
Preferably, the acid absorbent is high-active zinc oxide.
Preferably, the carbon nanotube is that single-walled carbon nanotube or multi-walled carbon nanotube are one or two kinds of.
Preferably, the filler is carbon black N990, carbon black N774, carbon black Ensaco 250G or carbon black Austin
325 one or more.
Preferably, the processing aid is HT290 or WS280.
The present invention provides a kind of above-mentioned fluoro-rubber composites to use in preparing the high sulfur-bearing operating condition of industrial gas oil
Rubber product in application.
The present invention provides above-mentioned fluoro-rubber composites to prepare industrial gas oil downhole tool sealing element, well head dress
Application in standby sealing element, pipeline valve sealing element, pump and compressor seal part.
The present invention provides a kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its applications, pass through reasonably optimizing composition
Formula, test result show that fluoro-rubber composite of the invention has excellent high-concentration hydrogen sulfide corrosion resistance and low
Warm sealing performance, fluoro-rubber composite formula of the invention rationally, substantially increase the high sulfur-bearing work in industrial gas oil underground
The sealing effect of sealing element used in condition.
Specific embodiment
The invention discloses a kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its application, those skilled in the art can be with
Present disclosure is used for reference, realization of process parameters is suitably modified.In particular, it should be pointed out that all similar substitutions and modifications are to ability
It is it will be apparent that they are considered as including in the present invention for field technique personnel.Method and application of the invention is
Through being described by preferred embodiment, related personnel obviously can not depart from the content of present invention, in spirit and scope to this
Methods and applications described in text are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
A kind of embodiment 1: fluoro-rubber composite of hydrogen sulfide corrosion-resistant
Table 1 is the formula of No. 1 to No. 8 fluoro-rubber composite, wherein the detailed weight ratio of each component is referring to table in raw material
1。
1 1-8 fluoro-rubber composite formula of table
Embodiment 2:
(1) performance test of fluoro-rubber composite
Each component is weighed to No. 8 formula (parts by weight) ratios according to No. 1 in embodiment 1, fluorubber is begun to pratise in double rods
Packet roller on machine, by the auxiliary materials such as carbon nanotube, crosslinking agent, promotor, acid absorbent, carbon black and processing aid be added open mill in and fluorine
Rubber mixes, and after fluorubber is mixed with auxiliary material, the rubber composition or so of packet roller is operated on each 5 times, adjusts open mill roll spacing
It to minimum, clot or beats triangle packet mode 10 times, between 15 minutes, open mill roller temperature is controlled 80 for entire mixing time control
DEG C hereinafter, make rubber material be kneaded uniformly after slice, obtain fluororubber compounded rubber, this fluororubber compounded rubber displayed 16 hours
Afterwards, then back mixing slice is stand-by.
The performance test of fluoro-rubber composite: at a temperature of 180 DEG C, under the conditions of 10 minutes one step cures, 20MPa mould
Pressure is sulfided into standard rubbers test piece, post vulcanization 16 hours again at a temperature of 200 DEG C, and standard testing batten is pressed in fluorubber test piece
Sample preparation is simultaneously tested, and the performance test data of 1-8 fluoro-rubber composite the results are shown in Table 2.
Wherein, the test method and standard being related to are as follows:
1, GB/T 531.1-2008 vulcanized rubber or thermoplastic elastomer penetration hardness test method first part: shore is hard
Spend meter method；
2, the measurement of GB/T 528-2009 vulcanized rubber or thermoplastic elastomer tensile stress-strain performance；
3, the measuring temperature of GB/T 7758-2002 vulcanized rubber cryogenic property bounces back method (TR test)；
4, GB/T 19466.2-2004 plastics differential scanning calorimetry (DSC) part 2: the survey of glass transition temperature
It is fixed；
5, the quick decompression test method of the anti-gas of NORSOK M710Rev.2 rubber packing material and requirement；
6, it the anti-extrusion test method of API: is surveyed anti-extrusion is placed in a thickness of the permanent deformation test block of the standard compression of 12.7mm
It tries in instrument, test block and pressure column gap are 0.34mm, at a certain temperature, pressurize to pressure column, it is made to press rubber
Deformation, pressure calculate rubber block height change, the height retention rate of rubber block is used as anti-extrusion at this time to after setting test request
The characterization haveing excellent performance；
2 1-8 fluorubber performance test data of table
| Serial number | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 | No. 6 | No. 7 | No. 8 |
| Hardness, Shore A | 76 | 90 | 94 | 81 | 88 | 96 | 98 | 90 |
| Tensile strength, MPa | 23.6 | 21.0 | 13.8 | 15.9 | 18.1 | 21.9 | 19.8 | 20.6 |
| Elongation, % | 286 | 197 | 81 | 200 | 167 | 111 | 88 | 143 |
| 50% modulus, MPa | 2.7 | 5.7 | 9.3 | 3.1 | 5.2 | 11.5 | 13.6 | 7.0 |
| 100% modulus, MPa | 5.9 | 12.4 | 7.4 | 10.8 | 19.8 | 14.4 | ||
| Cold snap-back TR10, DEG C | -29.6 | -29.9 | -31.4 | -40.0 | -40.1 | -41.7 | -41.5 | -7.3 |
| Glass transition temperature Tg, DEG C | -29.2 | -29.4 | -29.6 | -39.4 | -39.6 | -39.8 | -40.1 | -7.1 |
| The anti-extrusion measurement of API | NG | GOOD | BEST | NG | GOOD | BEST | BEST | BEST |
| NORSOK M710 measurement | FAIL | PASS | PASS | FAIL | PASS | PASS | PASS | PASS |
2 data of table are shown, for adding a certain amount of carbon nanotubes, rubber in fluorubber Tecnoflon VPL85540 formula
Material hardness is obviously improved, and carbon black total number remains unchanged 5 parts of carbon nanotubes of such as No. 6 additions simultaneously, and hardness increases from 88Shore A
It is added to 96Shore A；When 10 parts of carbon nanotubes of No. 7 additions, hardness is significantly increased from 86Shore A to 98Shore A.Therefore,
Appropriate amount carbon nanotubes is added in fluorubber, under conditions of keeping corresponding caoutchouc elasticity, available high rigidity rubber
Glue product.It separately can also be seen that addition 50% modulus of carbon nanotubes fluorubber material, 100% modulus also substantially from 2 data of table
Increase.Obvious, such as fluorine of No. 2 Viton GLT600S by conductive black Ensaco 250G addition fluoro-rubber composite reinforcing effect
The conductive black Ensaco 250G that rubber composition adds 25 parts replaces the N990 carbon black of identical weight number, and rubber material is hard
Degree is significantly increased from 76Shore A to 90Shore A, and 50% modulus and 100% modulus also greatly improve nearly 100%, it is seen that mends
Potent fruit is very excellent.
Fluorubber Viton GLT600S, Tecnoflon VPL85540 and Tecnoflon BR9151 composite formula 1
Numbers-No. 8, with oil gas field tetrapropanate fluorine rubber comparatively, having excellent low temperature service performance, especially Viton
Reachable -30 DEG C of dynamic sealing low temperature of GLT600S composition, Tecnoflon VPL85540 composition dynamic sealing low temperature is reachable -
40 DEG C, maximum operation (service) temperature is up to 200 DEG C or more.
(2) the resistance to 20% hydrogen sulfide corrosion performance test of fluoro-rubber composite, reference standard are as follows: NACE TM0187-2011 acid
The assessment of property gaseous environment elastomer material, test temperature: 175 DEG C, pressure: 6.9MPa, testing time: 168 hours.1-8
The performance test data of number resistance to 20% hydrogen sulfide corrosion of fluoro-rubber composite the results are shown in Table 3.
The resistance to 20% hydrogen sulfide corrosion performance test of 3 1-8 fluorubber of table
| Serial number | No. 1 | No. 1 | No. 1 | No. 1 | No. 1 | No. 1 | No. 1 | No. 1 |
| Firmness change, Shore A | -7 | -6 | -6 | -7 | -6 | -6 | -6 | -10 |
| Mass change, % | 2.6 | 2.4 | 2.3 | 2.2 | 1.9 | 2.1 | 1.8 | 2.8 |
| Volume change, % | 5.3 | 5.0 | 4.9 | 5.0 | 4.1 | 4.3 | 3.9 | 6.5 |
| 50% modulus change, % | 5.0 | 4.0 | 4.1 | 1.9 | 1.5 | 1.6 | 1.5 | 5.4 |
| 100% modulus change, % | 5.1 | 4.0 | 2.0 | 2.1 | 2.3 | 8.4 | ||
| Tensile strength variation, % | 2.2 | 1.1 | 2.1 | 5.2 | 6.9 | 6.1 | 5.9 | 2.2 |
| Elongation change, % | 3.6 | -2.7 | -2.3 | 3.2 | 3.5 | 3.6 | 3.5 | -2.6 |
3 data of table are shown, according to the test appraisal procedure of NACE TM0187-2011, in 175 DEG C of temperature, 6.9MPa pressure
And under the conditions of 168 hours corrosion tests, fluorubber Viton GLT600S, Tecnoflon VPL85540 and Tecnoflon
BR9151 composite formula No. 1-No. 8, excellent hydrogen sulfide corrosion-resistant performance is all had, volume change, stretches by force mass change
Degree variation and elongation change are respectively less than 10%.As it can be seen that the fluoro-rubber composite of the invention patent has excellent resistance to hydrogen sulfide rotten
Corrosion energy, it may have excellent low temperature seal performance.
The preparation of 3 fluoro-rubber composite of embodiment
(1) the fluorubber polymer Viton GLT200S of 100 parts by weight is plasticated uniformly on the double roll mill and is wrapped
Roller, then by the carbon nanotube of 10 parts by weight, then by 2,5- dimethyl -2,5- of the carbon nanotube of 15 parts by weight, 1 parts by weight
Bis(t-butylperoxy) hexane, the Triallyl isocyanurate of 1 parts by weight, the filler carbon black N990 of 20 parts by weight, 1 weight
The processing aid HT290 of part is pre-mixed uniformly, and is gradually added in open mill, and fluorubber is mixed with auxiliary material；
(2) after mixing fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 5 times, adjusts open mill roller
Away to minimum, clot or beat triangle packet mode 10 times, between 15 minutes, open mill roller temperature, which controls, to exist for entire mixing time control
80 DEG C hereinafter, make rubber material be kneaded uniformly after slice, obtain fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 4 fluoro-rubber composite of embodiment
(1) the fluorubber polymer Tenoflon VPLX75545 of 100 parts by weight is plasticated uniformly on the double roll mill
And packet roller, then by the carbon nanotube of 1 parts by weight, then by dimethyl -2 2,5- of the carbon nanotube of 1 parts by weight, 2 parts by weight,
5- bis(t-butylperoxy) hexane, the Triallyl isocyanurate of 3 parts by weight, 60 parts by weight filler carbon black N990,3 weights
The processing aid HT290 of amount part is pre-mixed uniformly, and is gradually added in open mill, and fluorubber is mixed with auxiliary material；
(2) after mixing fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 10 times, adjusts open mill roller
Away to minimum, clot or beat triangle packet mode 10 times, between 20 minutes, open mill roller temperature, which controls, to exist for entire mixing time control
80 DEG C hereinafter, make rubber material be kneaded uniformly after slice, obtain fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 5 fluoro-rubber composite of embodiment
(1) the fluorubber polymer Tenoflon VPLX65455 of 100 parts by weight is plasticated uniformly on the double roll mill
And packet roller, then by the carbon nanotube of 1 parts by weight, then by dimethyl -2 2,5- of the carbon nanotube of 5 parts by weight, 2 parts by weight,
5- bis(t-butylperoxy) hexane, the Triallyl isocyanurate of 5 parts by weight, 5 parts by weight acid absorbent oxide of high activity
Zinc, the filler carbon black N990 of 50 parts by weight, 3 parts by weight processing aid HT290 be pre-mixed uniformly, and be gradually added mill
In machine, fluorubber is mixed with auxiliary material；
(2) after mixing fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 10 times, adjusts open mill roller
Away to minimum, clot or beat triangle packet mode 10 times, between 15 minutes, open mill roller temperature, which controls, to exist for entire mixing time control
80 DEG C hereinafter, make rubber material be kneaded uniformly after slice, obtain fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 6 fluoro-rubber composite of embodiment
(1) the fluorubber polymer Tenoflon PL855 of 100 parts by weight is plasticated uniformly on the double roll mill and is wrapped
Roller, then by the carbon nanotube of 1 parts by weight, then by 2,5- dimethyl -2,5- of the carbon nanotube of 2 parts by weight, 1.5 parts by weight
Bis(t-butylperoxy) hexane, the Triallyl isocyanurate of 4 parts by weight, 30 parts by weight filler carbon black N990,20 weights
The processing aid WS280 for measuring filler carbon black Ensaco 250G of part, the processing aid HT290 of 1 parts by weight and 1 parts by weight is preparatory
It is uniformly mixed, and is gradually added in open mill, fluorubber is mixed with auxiliary material；
(2) after mixing fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 10 times, adjusts open mill roller
Away to minimum, clot or beat triangle packet mode 10 times, between 15 minutes, open mill roller temperature, which controls, to exist for entire mixing time control
80 DEG C hereinafter, make rubber material be kneaded uniformly after slice, obtain fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 7 fluoro-rubber composite of embodiment
(1) the fluorubber polymer Tenoflon PL455 of 100 parts by weight is plasticated uniformly on the double roll mill and is wrapped
Roller, then by the carbon nanotube of 1 parts by weight, then by 2,5- dimethyl -2,5- bis(t-butylperoxy) of 1.5 parts by weight oneself
Alkane, the Triallyl isocyanurate of 5 parts by weight, the filler carbon black N990 of 30 parts by weight, 30 parts by weight filler carbon black N774,
The processing aid HT290 of 2 parts by weight is pre-mixed uniformly, and is gradually added in open mill, and fluorubber is mixed with auxiliary material；
(2) after mixing fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 10 times, adjusts open mill roller
Away to minimum, clot or beat triangle packet mode 10 times, between 15 minutes, open mill roller temperature, which controls, to exist for entire mixing time control
80 DEG C hereinafter, make rubber material be kneaded uniformly after slice, obtain fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The above are the descriptions to the embodiment of the present invention to keep this field special by the foregoing description of the disclosed embodiments
Industry technical staff can be realized or using the present invention.Various modifications to these embodiments carry out those skilled in the art
Saying will be apparent.The general principles defined herein can be the case where not departing from the spirit or scope of the present invention
Under, it realizes in other embodiments.Therefore, the present invention is not intended to be limited to these implementation columns shown in this article, but to accord with
Close the widest scope consistent with principles disclosed herein and novel point.
Claims (10)
1. a kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant, which is characterized in that be prepared by the raw material of following parts by weight:
The fluorubber is vinylidene fluoride-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer polymer, inclined difluoro
Ethylene-hexafluoropropene-tetrafluoroethylene-Ethylene-perfluoro methyl vinyl ether-cure site monomer polymer, vinylidene fluoride-perfluor
One of alkoxymethylene vinyl ethers-cure site monomer polymer.
2. fluoro-rubber composite as described in claim 1, it is characterised in that: the vinylidene fluoride-tetrafluoroethylene-perfluoro
Methyl vinyl ether-cure site monomer polymer be Viton GLT600S, Viton GLT200S, Tecnoflon PL855 or
One of Tecnoflon PL455；Vinylidene fluoride-hexafluoropropene-tetrafluoroethylene-Ethylene-the perfluoromethylvinyl
Base ether-cure site monomer polymer is Tecnoflon BR9151；The vinylidene fluoride-perfluoroalkoxy methylene ethylene
Base ether-cure site monomer polymer is Tecnoflon VPL85540, Tecnoflon VPL55540, Tecnoflon
One of VPLX75545 or Tecnoflon VPLX65455.
3. fluoro-rubber composite as described in claim 1, it is characterised in that: the crosslinking agent is 2,5- dimethyl -2,5-
Bis(t-butylperoxy) hexane.
4. fluoro-rubber composite as described in claim 1, it is characterised in that: the promotor is triallyl isocyanuric acid
Ester (TAIC).
5. fluoro-rubber composite as described in claim 1, it is characterised in that: the acid absorbent is high-active zinc oxide.
6. fluoro-rubber composite as described in claim 1, it is characterised in that: the carbon nanotube be single-walled carbon nanotube or
Multi-walled carbon nanotube is one or two kinds of.
7. fluoro-rubber composite as described in claim 1, it is characterised in that: the filler be carbon black N990, carbon black N774,
The one or more of carbon black Ensaco 250G or carbon black Austin 325.
8. fluoro-rubber composite as described in claim 1, it is characterised in that: the processing aid is HT290 or WS280.
9. the application of fluoro-rubber composite as described in claim 1-8 any one is prepared in the high sulfur-bearing of industrial gas oil
Rubber product used in operating condition.
10. application as claimed in claim 9, it is characterised in that: prepare industrial gas oil downhole tool sealing element, well head
Equip the application in sealing element, pipeline valve sealing element, pump and compressor seal part.
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| CN111019276A (en) * | 2019-12-31 | 2020-04-17 | 成都晨光博达橡塑有限公司 | Fluorine-containing thermoplastic elastomer and preparation method thereof |
| CN111103421A (en) * | 2019-12-31 | 2020-05-05 | 山东华夏神舟新材料有限公司 | Method for testing fluorine content in fluororubber |
| CN112592548A (en) * | 2020-11-16 | 2021-04-02 | 上海如实密封科技有限公司 | Low-temperature-resistant fluororubber composition and application thereof |
| CN113105703A (en) * | 2021-03-22 | 2021-07-13 | 温州邦欣源科技有限公司 | Modified conductive fluororubber, preparation method and conductive medium-resistant fluororubber sealing ring |
| CN114672116A (en) * | 2022-04-29 | 2022-06-28 | 安徽中鼎密封件股份有限公司 | Low-compression stress relaxation fluororubber for battery sealing element and preparation method thereof |
| CN116769264A (en) * | 2023-08-24 | 2023-09-19 | 江苏中煜橡塑科技有限公司 | Fluororubber material for sealing cold-resistant power battery and preparation method and application thereof |
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| CN113105703A (en) * | 2021-03-22 | 2021-07-13 | 温州邦欣源科技有限公司 | Modified conductive fluororubber, preparation method and conductive medium-resistant fluororubber sealing ring |
| CN114672116A (en) * | 2022-04-29 | 2022-06-28 | 安徽中鼎密封件股份有限公司 | Low-compression stress relaxation fluororubber for battery sealing element and preparation method thereof |
| CN116769264A (en) * | 2023-08-24 | 2023-09-19 | 江苏中煜橡塑科技有限公司 | Fluororubber material for sealing cold-resistant power battery and preparation method and application thereof |
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Application publication date: 20190910 |