CN106633544B - A kind of high temperature high voltage resistant sealing element fluorubber material and preparation method thereof - Google Patents
A kind of high temperature high voltage resistant sealing element fluorubber material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to polymer rubber composite material, a kind of high temperature high voltage resistant sealing element fluorubber material and preparation method thereof is disclosed.A small amount of carbon nanotubes is added in fluorubber polymer, reasonably optimizing filler and vulcanizing system, the high temperature high voltage resistant sealing element are prepared with fluorubber material by the processing aid of the gadolinium oxy-sulphide system fluorubber polymer of 100 parts by weight, the carbon nanotube of 1-15 parts by weight, 1-3 parts of crosslinking agent, 1-6 parts of promotor, the acid absorbent of 0-5 parts by weight, the filler of 5-40 parts by weight and 0-2 parts by weight simultaneously.Rationally, simple process substantially increases the sealing of downhole tool and valve valve seat and pressure-bearing effect under high temperature and pressure to the invention formula.
Description
Technical field
The present invention relates to polymer rubber composite material, in particular to a kind of high temperature high voltage resistant sealing element fluorubber material
And preparation method thereof.
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 technology for drilling, transmission and processing technology relevant device.In high temperature height
Under pressure corrosive conditions, rubber material even more proposes high rigidity, high tensile, high shearing resistance other than being resistant to complex dielectrics
Shear deformation, explosion-proof (ED, Explosive Decompression) or the Quick Depressurization of resistance to gas (RGD, Rapid Gas
) and the performance requirements such as the anti-extrusion deformation of rubber material (ER, Extrusion Resistance) Decompression.
In oil-gas pipeline transmission process, valve is very important component.In the nonmetallic field of sealing technology of valve, non-gold
Belong to material and refers generally to plastics, rubber and soft graphite etc., and rubber material is since its elasticity is excellent, tolerance balancing effect is bright
It is aobvious, it is low to metalwork requirement on machining accuracy the features such as, a large amount of design and use in terms of valve seal.But existing rubber material
At high temperature under high pressure, sealing effect is undesirable, and mainly since wearability is poor, hardness is low, and intensity is low, and anti-extrusion deformation is big,
It fails vulnerable to high shear, while under high temperature high pressure liquid or gaseous environment, rubber seal is easy to produce the fast quick-release of gas
Pressure failure.Therefore, a kind of anti-extrusion deformation of high rigidity, anti-shearing and anti-gas Quick Depressurization high-performance rubber material are researched and developed
It is very necessary, in particular for valve valve base sealing high durometer rubber material, hardness requirement 90Shore A or more.
In oil-gas mining technique, packer is a kind of oil gas field underground commonly key tool, is widely used in oil field
The several work purposes such as dispensing, separate zone stimulation, pressure break, oil production by layer, mechanical pipe water blockoff need.Rubber packing element is as packer
Chief component, its quality directly affects the normal use effect of packer, and service life etc. plays in packer
Conclusive effect.When rubber packing element bears higher differential pressure in the high temperature environment, packing element is easy by pressure break, so that entire packer
Tool seal failure, to cause that the resistance to pressure difference of packer is low, service life is short.Packer rubber cylinder material used at present has fourth
Nitrile rubber, hydrogenated nitrile-butadiene rubber, fluorine-containing rubber etc. have substantially met requirement in the case where pressure difference is not very high situation, but with
The further raising of pressure difference, but all due under room temperature and high temperature shear strength it is low, be easy to cause packing element to damage.Therefore, it grinds
Send out the anti-extrusion deformation of high rigidity a kind of, the rubber material of high shear deformation it is very necessary, hardness requirement 85Shore A or more.
Carbon nanotube (CNTs) is the coaxial hollow tubulose formed that flocked together under certain condition by a large amount of carbon atoms
Nanometer materials, with good mechanical property, CNTs tensile strength reaches 50~200Gpa, is 100 times of steel, density
But there was only the 1/6 of steel, an order of magnitude at least higher than ordinary graphite fiber, the elasticity modulus of carbon nanotube is up to 1TPa, with gold
The elasticity modulus of hard rock is suitable, about the 5 of steel times.With reaching its maturity for the carbon nanotubes commercialization of production, material cost is also big
Width decline, carbon nanotubes is used as reinforcing filler also gradually to be increased.Chinese patent (publication number: CN1615336A), which discloses, to be contained
There is rubber composition and preparation method thereof of the carbon nanotubes as reinforcing agent, provides a kind of natural rubber, butadiene-styrene rubber and poly-
Synthetic rubber or natural gum including butadiene rubber enhance rubber using carbon nanotubes or graphite fibre, improve rubber product
Mechanical property, physical property and chemical property.This rubber-like materials applies in general to rubber tyre manufacture, is not suitable for resistance to
The high voltage bearing industrial gas oil of high temperature.Chinese patent (publication number: CN101613495A) is disclosed containing carbon nanotubes
Rubber composition is provided comprising the curable of a kind of special hydrogenated butyronitrile, at least one crosslinking agent and carbon nanotubes
Composition, display curing rubber have excellent thermal, oil resistance and mechanical strength.Chinese patent (Authorization Notice No.:
CN103242609B multidimensional number composite inorganic particles/tetrapropanate fluorine rubber composite material) is disclosed, based on tetrapropanate fluorine rubber
Material adds the composite inorganic particles of different dimensions, by surface modification make surface of inorganic particles with can participate in be crosslinked instead
The double bond answered, the compound particle of addition can effectively improve the heatproof of tetrapropanate fluorine rubber, resistance to hydrogen sulfide and resistance to carbon dioxide performance.
But the composite rubber material of these prior arts is under high temperature and pressure deep-etching operating condition, in addition to not being resistant to complexity
Outside medium, high rigidity, high tensile, high shear deformation, explosion-proof (ED, Explosive can not be met
Decompression) or the Quick Depressurization of resistance to gas (RGD, Rapid Gas Decompression) and rubber material are anti-squeezes
Performance requirements such as (ER, Extrusion Resistance) are deformed out, and the present invention is by comparing and screening repeatedly, by gadolinium oxy-sulphide
System fluorubber polymer and carbon nanotube combine, and prepare high temperature high voltage resistant sealing element fluorubber material in conjunction with auxiliary material,
But originally find, carbon nanotube is added in fluorubber polymer, and not every composite rubber material is in high temperature and pressure
There are high rigidity, high tensile and high elongation rate under environment, or even was once abandoning and preparing high temperature high voltage resistant sealing element fluorine
The initial effort of rubber material,
However as the progress of test, we are had surprisingly found that, are added to specific ratio using the carbon nanotube of a small amount of ratio
In the fluorubber of example, and at the same time reasonably optimizing filler and vulcanizing system, entire formula system guarantees the feelings of higher gum content
Under condition, hardness, stretching strength, anti-extrusion deformation and the anti-shear performance of fluorubber composite material, while material are substantially increased
Material have excellent anti-gas Quick Depressurization performance, in conclusion the present invention provides it is a kind of formula rationally, simple process it is resistance to
High temperature and pressure sealing element fluorubber material and preparation method thereof substantially increases downhole tool and valve valve seat under high temperature and pressure
Sealing and pressure-bearing effect.
Summary of the invention
In order to solve the fluorubber material under high temperature and pressure in the prior art as sealing element used time, sealing and pressure-bearing effect
Difference, the present invention provides a kind of high temperature high voltage resistant sealing element fluorubber materials.
In order to solve the above-mentioned technical problem, the invention adopts the following technical scheme:
A kind of high temperature high voltage resistant sealing element fluorubber material, is prepared by the supplementary material of following parts by weight:
Preferably, the gadolinium oxy-sulphide system fluorubber polymer is biasfluoroethylene-hexafluoropropylene-tetrafluoroethene-sulphur
Change point monomer fluorubber or vinylidene-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer fluorubber one kind；More
For preferably, the biasfluoroethylene-hexafluoropropylene-tetrafluoroethene-cure site monomer fluorubber is fluorubber Viton GF；Institute
Stating vinylidene-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer fluorubber is fluorubber Viton GLT.
Preferably, the carbon nanotube is that single-walled carbon nanotube or multi-walled carbon nanotube are one or two kinds of.
Preferably, the crosslinking agent is that (101XL-45 has 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane
Imitate ingredient 45%).
Preferably, the promotor is Triallyl isocyanurate (TAIC-S70, effective component 70%).
Preferably, the acid absorbent is zinc oxide；The carbon black is the one or more of N990, N774 or N550；
The processing aid is WS280 or HT290.
The present invention also provides simultaneously is made high-temperature and high-presure resistent sealing element using fluorubber material provided by the invention；It will
The sealing element is sealed for industrial gas oil downhole tool or valve seal, or pump and compressor seal.
It is a further object to provide a kind of preparation methods of high temperature high voltage resistant sealing element fluorubber material, and
The fluorubber material being prepared by the preparation method.The preparation method specifically includes:
(1) by the gadolinium oxy-sulphide system fluorubber polymer of 100 parts by weight plasticate on the double roll mill uniformly and packet roller,
Then by the carbon nanotube of 1-15 parts by weight, the suction of the crosslinking agent of 1-3 parts by weight, the promotor of 1-6 parts by weight, 0-5 parts by weight
The processing aid auxiliary material of sour agent, the filler of 5-40 parts by weight and 0-2 parts by weight is pre-mixed uniformly, and is gradually added open mill
In, gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on into each 5-10
It is secondary, open mill roll spacing is adjusted to minimum, clot or is beaten triangle packet mode 10 times, and entire mixing time was controlled in 15-20 minute
Between, slice after being kneaded rubber composite material uniformly obtains fluororubber compounded rubber.
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
High temperature high voltage resistant sealing element fluorubber material provided by the invention and preparation method thereof, the present invention receives a small amount of
Rice carbon pipe is added in fluorubber polymer, while reasonably optimizing filler and vulcanizing system, test result show entirely matching
In the case that cube system guarantees higher gum content, high temperature high voltage resistant sealing element provided by the invention is greatly improved with fluorubber material
The hardness of fluorubber composite material, stretching strength, anti-extrusion deformation and anti-shear performance, at the same material have it is excellent anti-
Gas Quick Depressurization performance；From the above technical scheme, rationally, simple process substantially increases height to formula of the present invention
The sealing of downhole tool and valve valve seat and pressure-bearing effect under warm high pressure.
Specific embodiment
The invention discloses a kind of high temperature high voltage resistant sealing element fluorubber material and preparation method thereof, those skilled in the art
Member can use for reference present disclosure, be suitably modified realization of process parameters.In particular, it should be pointed out that all similar substitutions and modifications
Apparent to those skilled in the art, they are considered as including in the present invention.Method of the invention and
Using being described by preferred embodiment, related personnel can obviously not depart from the content of present invention, spirit and scope
It is interior that method described herein and application are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
The formula of 1 gadolinium oxy-sulphide fluorubber material of embodiment
Table 1 is the formula of No. 1 to No. 4 gadolinium oxy-sulphide fluorubber material, and proportion is referring to each component ratio in table in detail.
The formula of 1 No. 1 to No. 4 gadolinium oxy-sulphide fluorubber materials of table
| Serial number | No. 1 | No. 2 | No. 3 | No. 4 |
| Fluorubber Viton GF | 100.00 | 100.00 | 100.00 | 100.00 |
| Carbon nanotube GTR | 0.00 | 5.00 | 10.00 | 15.00 |
| Promotor TAIC-S70 | 4.00 | 4.00 | 4.00 | 4.00 |
| Crosslinking agent 101XL-45 | 1.50 | 1.50 | 1.50 | 1.50 |
| Zinc oxide META-Z102 | 3.00 | 3.00 | 3.00 | 3.00 |
| Carbon black N 990 | 30.00 | 25.00 | 20.00 | 15.00 |
| Processing aid Struktol HT 290 | 1.00 | 1.00 | 1.00 | 1.00 |
| Total number | 139.50 | 139.50 | 139.50 | 139.50 |
The performance test of 2 gadolinium oxy-sulphide fluorubber material of embodiment
Each component is weighed to No. 4 formula (parts by weight) ratios according to No. 1 in embodiment 1, gadolinium oxy-sulphide fluorubber is existed
Double rods are begun to pratise packet rod on machine, and the auxiliary materials such as carbon nanotube, crosslinking agent, promotor, acid absorbent zinc oxide, carbon black and processing aid are added
Enter in open mill and fluorubber mixes, is kneaded uniform and slice in the case where roller temperature is lower than 80 DEG C, obtains fluororubber compounded rubber.It will be kneaded
Glue, at a temperature of 180 DEG C, under the conditions of 10 minutes one step cures, molding is sulfided into standard rubbers test piece, at a temperature of 200 DEG C again
Post vulcanization 12 hours, rubber test piece by the sample preparation of standard testing batten and is tested, the performance ginseng of 1-4 gadolinium oxy-sulphide fluorubber
Number is 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 measurement of GB/T 529-2008 vulcanized rubber or thermoplastic elastomer tearing strength；
4, the anti-gas Quick Depressurization test method of NORSOK M710 rubber packing material and requirement；
5, 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 1-4 gadolinium oxy-sulphide fluorubber performance test parameter of table
| Fluorubber number | No. 1 | No. 2 | No. 3 | No. 4 |
| Gum content, % | 71.68 | 71.68 | 71.68 | 71.68 |
| Hardness, Shore A | 77 | 88 | 94 | 98 |
| Tensile strength, MPa | 18.10 | 28.50 | 34.10 | |
| Elongation, % | 256 | 208 | 179 | |
| 50% modulus, MPa | 2.29 | 6.51 | 10.56 | |
| 100% modulus, MPa | 5.00 | 13.97 | 21.69 | |
| Right-angle tearing, KN/m | 60.20 | 74.60 | 94.90 | |
| Pants type tearing, KN/m | 20.86 | 32.60 | 49.79 | |
| The anti-extrusion measurement of API | Difference | Generally | It is excellent | |
| NORSOK M710 measurement | Do not pass through | Pass through | Pass through |
2 data of table are shown, add a certain amount of carbon nanotubes, rubber for the fluorubber of Viton GF peroxidating vulcanizing system
Material hardness improves quickly, and 5 parts of carbon nanotubes of such as No. 2 additions are corresponding simultaneously to reduce carbon black number, keeps being formulated total gum content not
Become, hardness increases to 88Shore A from 77Shore A；When 10 parts of carbon nanotubes of No. 3 additions, hardness substantially increases from 77Shore A
It is added to 94Shore A, and is formulated gum content and still maintains constant, up to 71.68%, therefore, suitable carbon nanotubes is added to
High durometer rubber product obtained in fluorubber still has excellent caoutchouc elasticity.It can also be seen that addition from 2 data of table
50% modulus of carbon nanotubes fluorubber composite material, 100% modulus are multiplied, and tensile strength also greatly improves, tearing strength
Raising is also particularly evident, and anti-extrusion performance is also obviously improved with hardness increase, and anti-gas Quick Depressurization is functional；But nano-sized carbon
Pipe additive amount is more than 10 parts (parts by weight), and such as No. 4 too high with side elastomeric material hardness, material becomes fragile, and unsuitable sealed elastic is wanted
It asks.Therefore, the additive amount of carbon nanotubes of the invention, and fluorine rubber can be made with the proportion of the fluorubber of peroxidating vulcanizing system
Each performance of the synthesis of glue material is the most excellent.
The formula of 3 gadolinium oxy-sulphide fluorubber material of embodiment
Table 3 is the formula of No. 5 to No. 8 gadolinium oxy-sulphide fluorubber materials, and proportion is referring to each component ratio in table in detail.
The formula of 3 No. 5 to No. 8 gadolinium oxy-sulphide fluorubber of table
4 gadolinium oxy-sulphide fluorubber performance test of embodiment
Each component is weighed to No. 8 formula (parts by weight) ratios according to No. 5 in embodiment 3, gadolinium oxy-sulphide fluorubber is existed
Double rods are begun to pratise packet rod on machine, and the auxiliary materials such as carbon nanotube, crosslinking agent, promotor, acid absorbent zinc oxide, carbon black and processing aid are added
Enter in open mill and fluorubber mixes, is kneaded uniform and slice in the case where roller temperature is lower than 80 DEG C, obtains fluororubber compounded rubber.By this reality
A rubber compound is applied, at a temperature of 180 DEG C, under the conditions of 10 minutes one step cures, molding is sulfided into standard rubbers test piece, at 200 DEG C
At a temperature of post vulcanization 12 hours again, test piece by the sample preparation of standard testing batten and is tested, the performance parameter of 5-8 fluorubber is shown in
Table 4.Wherein, the test method and standard and embodiment 2 being related to are identical.
4 5-8 gadolinium oxy-sulphide fluorubber performance test parameter of table
4 data of table are shown, add a certain amount of carbon nanotubes for the fluorubber of Viton GLT peroxidating vulcanizing system, together
Sample fluorubber material hardness significantly improves, and 5 parts of carbon nanotubes of such as No. 6 additions are corresponding simultaneously to reduce carbon black number, keeps formula total
Gum content 66.58% is constant, and hardness increases to 92Shore A from 86Shore A；When 10 parts of carbon nanotubes of No. 7 additions, hardness from
86Shore A increases to 94Shore A, and increasing degree is slowed down, obvious not as good as Viton GF peroxide fluorubber, formula
Gum content still maintains constant, and up to 66.58%, therefore, suitable carbon nanotubes is added to high rigidity obtained in fluorubber
Rubber product still has excellent caoutchouc elasticity.It can also be seen that addition carbon nanotubes is low to Viton GLT from 2 data of table
Warm fluorubber, 50% modulus of composite material, 100% modulus obviously increase, and tearing strength also significantly improves, anti-extrusion performance with
Hardness increase is also obviously improved, and anti-gas Quick Depressurization is functional；But carbon nanotubes additive amount is more than 10 parts (parts by weight), such as
No. 8 too high with side elastomeric material hardness, material becomes fragile, and is not suitable for sealed elastic requirement.Therefore, carbon nanotubes of the invention adds
Dosage, and each performance of synthesis of fluorubber material can be made the most excellent with the proportion of the fluorubber of peroxidating vulcanizing system.
5 bis-phenol vulcanised fluororubbers material prescription of embodiment and performance test
Table 5 is the formula of No. 9 to No. 12 bis-phenol vulcanizing system fluorubber materials, and proportion is referring to each component ratio in table in detail
, in table 5 in formula, acid absorbent NICC500 is high activity calcium hydroxide, and acid absorbent MA150 is extra light calcined magnesia, vulcanizing agent
AF50 is bisphenol AF (effective component 50%), and promotor is benzyltriphenyl phosphonium phosphate BTPPC (effective component 33%).
Bis-phenol vulcanised fluororubbers material is prepared according to No. 9 to No. 12 formulas, preparation method and embodiment 2 are identical, by this reality
A rubber compound is applied, at a temperature of 180 DEG C, under the conditions of 10 minutes one step cures, molding is sulfided into standard rubbers test piece, at 200 DEG C
At a temperature of post vulcanization 12 hours again, test piece by the sample preparation of standard testing batten and is tested, the performance parameter of 9-12 fluorubber
It is shown in Table 6.Wherein, the test method and standard and embodiment 2 being related to are identical.
5 9-12 bis-phenol vulcanised fluororubbers performance test parameter of table
| Serial number | No. 9 | No. 10 | No. 11 | No. 12 |
| Fluorubber Viton AHV | 100.00 | 100.00 | 100.00 | 100.00 |
| Carbon nanotube GTR | 0.00 | 5.00 | 10.00 | 15.00 |
| Acid absorbent NICC5000 | 6.00 | 6.00 | 6.00 | 6.00 |
| Acid absorbent MA150 | 3.00 | 3.00 | 3.00 | 3.00 |
| Vulcanizing agent A F50 | 6.00 | 6.00 | 6.00 | 6.00 |
| Accelerant B P33 | 2.00 | 2.00 | 2.00 | 2.00 |
| Carbon black N 990 | 25.00 | 20.00 | 15.00 | 10.00 |
| Carbon black N774 | 15.00 | 15.00 | 15.00 | 15.00 |
| Processing aid Brazil wax | 1.00 | 1.00 | 1.00 | 1.00 |
| Processing aid WS 280 | 1.00 | 1.00 | 1.00 | 1.00 |
| Total number | 159.00 | 159.00 | 159.00 | 159.00 |
6 9-12 bis-phenol vulcanised fluororubbers performance test parameter of table
| Fluorubber number | No. 9 | No. 10 | No. 11 | No. 12 |
| Gum content, % | 62.89 | 62.89 | 62.89 | 62.89 |
| Hardness, Shore A | 93.00 | 94.00 | 97.00 | 98.00 |
| Tensile strength, MPa | 21.80 | 21.00 | 21.50 | |
| Elongation at break, % | 72.80 | 73.00 | 51.80 | |
| 50% modulus, MPa | 15.32 | 14.90 | 21.05 | |
| 100% modulus, MPa | 0.00 | 0.00 | 0.00 | |
| Right-angle tearing, KN/m | 49.00 | 48.10 | 52.30 | |
| Pants type tearing, KN/m | 28.80 | 30.20 | 46.20 |
6 data of table are shown, under the thinking of high rigidity formula design, for bis-phenol vulcanizing system fluorubber Viton AHV
A certain amount of carbon nanotubes is added, hardness raising is unobvious, and tensile strength decreases almost without improvement, extension at break.
For 50% modulus index, adding 5 parts of carbon nanotubes does not improve, until 10 parts of carbon nanotubes of addition just increase,
But elongation at break reduces obvious at this time.Angle tear strength index, add a certain amount of carbon nanotube improve it is unobvious, for
Pants type tearing strength, improves.Generally, for bis-phenol vulcanizing system fluorubber, especially in high rigidity formula
Under mentality of designing, addition carbon nanotube is ineffective, and material elongation at break is too low, has been not suitable for sealing applications.
The preparation of 6 fluorubber material of embodiment
(1) biasfluoroethylene-hexafluoropropylene-tetrafluoroethene of 100 parts by weight-cure site monomer fluorubber Viton GF is existed
It plasticates in two-roll mill uniformly and packet roller, then by the single-walled carbon nanotube of 1 parts by weight, dimethyl -2 2,5- of 1 parts by weight,
5- bis(t-butylperoxy) hexane, the Triallyl isocyanurate of 1 parts by weight, the filler carbon black N990 of 5 parts by weight are preparatory
It is uniformly mixed, and is gradually added in open mill, gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 5 times,
Open mill roll spacing is adjusted to minimum, clot or is beaten triangle packet mode 10 times, entire mixing time controlled between 15 minutes, made rubber
Slice after glue composite material is kneaded uniformly, obtains 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 fluorubber material of embodiment
(1) by biasfluoroethylene-hexafluoropropylene-tetrafluoroethene of 100 parts by weight-cure site monomer fluorubber Viton GBL
Plasticate on the double roll mill uniformly and packet roller, then by the multi-walled carbon nanotube of 1 parts by weight, 2, the 5- dimethyl-of 1 parts by weight
2,5- bis(t-butylperoxy) hexane, the Triallyl isocyanurate of 1 parts by weight, the filler carbon black N990 of 5 parts by weight are pre-
It is first uniformly mixed, and is gradually added in open mill, gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 5 times,
Open mill roll spacing is adjusted to minimum, clot or is beaten triangle packet mode 10 times, entire mixing time controlled between 15 minutes, made rubber
Slice after glue composite material is kneaded uniformly, obtains fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 8 fluorubber material of embodiment
(1) by the vinylidene of 100 parts by weight-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer fluorubber
Viton GLT plasticate on the double roll mill uniformly and packet roller, then by the multi-walled carbon nanotube and single wall nano of 15 parts by weight
Carbon pipe, the 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane of 3 parts by weight, 6 parts by weight triallyl isocyanuric acid
Ester, the zinc oxide of 5 parts by weight, the filler carbon black N774 of 40 parts by weight and 2 parts by weight processing aid WS280 be uniformly mixed and by
It gradually is added in open mill, gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 10 times,
Open mill roll spacing is adjusted to minimum, clot or is beaten triangle packet mode 10 times, entire mixing time controlled between 20 minutes, made rubber
Slice after glue composite material is kneaded uniformly, obtains fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 9 fluorubber material of embodiment
(1) by the vinylidene of 100 parts by weight-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer fluorubber
Viton GBLT plasticates uniformly and packet roller on the double roll mill, then by the multi-walled carbon nanotube of 8 parts by weight, 2 parts by weight
2,5- dimethyl -2,5- bis(t-butylperoxy) hexane, 3 parts by weight Triallyl isocyanurate, 2 parts by weight oxidation
The processing aid HT290 of zinc, the filler carbon black N550 and N774 of 22 parts by weight and 1 parts by weight is uniformly mixed and gradually adds
Enter in open mill, gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 8 times,
Open mill roll spacing is adjusted to minimum, clot or is beaten triangle packet mode 10 times, entire mixing time controlled between 22 minutes, made rubber
Slice after glue composite material is kneaded uniformly, obtains fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The preparation of 10 fluorubber material of embodiment
(1) by the vinylidene of 100 parts by weight-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer fluorubber
Viton GFLT plasticates uniformly and packet roller on the double roll mill, then by the single-walled carbon nanotube of 8 parts by weight, 2 parts by weight
2,5- dimethyl -2,5- bis(t-butylperoxy) hexane, 3 parts by weight Triallyl isocyanurate, 2 parts by weight oxidation
The processing aid HT290 of zinc, the filler carbon black N550 of 22 parts by weight and 1 parts by weight is uniformly mixed and is gradually added mill
In machine, gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on each 8 times,
Open mill roll spacing is adjusted to minimum, clot or is beaten triangle packet mode 10 times, entire mixing time controlled between 22 minutes, made rubber
Slice after glue composite material is kneaded uniformly, obtains fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (6)
1. a kind of high temperature high voltage resistant sealing element fluorubber material, which is characterized in that by the supplementary material preparation of following parts by weight
At:
The gadolinium oxy-sulphide system fluorubber polymer is biasfluoroethylene-hexafluoropropylene-tetrafluoroethene-cure site monomer fluorine rubber
Glue or vinylidene-tetrafluoroethylene-perfluoro methyl vinyl ether-cure site monomer fluorubber one kind, the vinylidene-
Hexafluoropropene-tetrafluoroethene-cure site monomer fluorubber is fluorubber Viton GF, the vinylidene-tetrafluoroethylene-perfluoro
Methyl vinyl ether-cure site monomer fluorubber is fluorubber Viton GLT；The carbon nanotube be single-walled carbon nanotube or
Multi-walled carbon nanotube is one or two kinds of；The crosslinking agent is 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane；The rush
It is Triallyl isocyanurate (TAIC) into agent.
2. fluorubber material as described in claim 1, which is characterized in that the acid absorbent is zinc oxide.
3. fluorubber material as described in claim 1, which is characterized in that the filler be carbon black such as N990, N774 or
The one or more of N550.
4. fluorubber material as described in claim 1, which is characterized in that the processing aid is WS280 or HT290.
5. a kind of preparation method of high temperature high voltage resistant sealing element fluorubber material as described in claim 1, which is characterized in that
Specifically includes the following steps:
(1) by the gadolinium oxy-sulphide system fluorubber polymer of 100 parts by weight plasticate on the double roll mill uniformly and packet roller, then
By the carbon nanotube of 1-15 parts by weight, the crosslinking agent of 1-3 parts by weight, the promotor of 1-6 parts by weight, 0-5 parts by weight acid absorbent,
The filler of 5-40 parts by weight and the processing aid auxiliary material of 0-2 parts by weight are pre-mixed uniformly, and are gradually added in open mill, will
Gadolinium oxy-sulphide system fluorubber is mixed with auxiliary material；
(2) after mixing gadolinium oxy-sulphide system fluorubber with auxiliary material, the rubber composition or so of packet roller is operated on to 5-10 times each, tune
Open mill roll spacing is saved to minimum, clot or is beaten triangle packet mode 10 times, entire mixing time controlled between 15-20 minutes, made
Slice after rubber composite material is kneaded uniformly, obtains fluororubber compounded rubber；
(3) after the fluororubber compounded rubber prepared being displayed 16 hours, then back mixing slice is stand-by.
6. a kind of high temperature high voltage resistant sealing element, which is characterized in that be made of fluorubber material described in claim 1；It will
The sealing element is for the sealing of industrial gas oil downhole tool, valve seal or pump and compressor seal.
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| US11084910B2 (en) | 2017-06-06 | 2021-08-10 | Zeon Corporation | Cross-linked rubber and production method therefor |
| US11613612B2 (en) | 2017-07-05 | 2023-03-28 | Nok Corporation | Fluororubber composition, method for producing the same and fluororubber crosslinked molded article |
| CN108410181A (en) * | 2018-03-26 | 2018-08-17 | 山东冬瑞高新技术开发有限公司 | A kind of low temperature resistant fluorine silicone rubber sizing material and preparation method thereof |
| WO2020040221A1 (en) * | 2018-08-24 | 2020-02-27 | 日本ゼオン株式会社 | Seal material |
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| CN109608795B (en) * | 2018-12-27 | 2021-07-30 | 江苏金晟元特种阀门股份有限公司 | Partially-crosslinked special lining material for high-temperature-resistant, creep-resistant and corrosion-resistant valve and preparation method thereof |
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| CN112898705A (en) * | 2019-11-19 | 2021-06-04 | 罗孚橡胶（江苏）有限公司 | Inner layer peroxide fluorine rubber material of rubber tube at high-temperature section of silicon-fluorine composite turbocharging system |
| CN111849094B (en) * | 2020-07-10 | 2022-04-15 | 上海如实密封科技有限公司 | High-strength high-modulus fluororubber composition and preparation method and application thereof |
| CN112457612B (en) * | 2020-11-16 | 2023-03-10 | 上海如实密封科技有限公司 | Low-temperature-resistant perfluoroether rubber composition and preparation method and application thereof |
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| CN115627039B (en) * | 2022-09-26 | 2023-08-01 | 温州大学苍南研究院 | Ternary fluororubber nanocomposite material with double filler systems and preparation method thereof |
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| CN102585402A (en) * | 2012-02-28 | 2012-07-18 | 安徽中鼎密封件股份有限公司 | High-strength fluororubber and preparation method, fluororubber sealing element |
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