CN107778733B - Composite material of isobutene/alkylstyrene polymer and fluororubber and preparation method thereof - Google Patents

Composite material of isobutene/alkylstyrene polymer and fluororubber and preparation method thereof Download PDF

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CN107778733B
CN107778733B CN201610719960.2A CN201610719960A CN107778733B CN 107778733 B CN107778733 B CN 107778733B CN 201610719960 A CN201610719960 A CN 201610719960A CN 107778733 B CN107778733 B CN 107778733B
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fluororubber
isobutylene
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CN107778733A (en
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梁滔
李振昊
魏绪玲
燕鹏华
张华强
赵洪国
邵卫
龚光碧
李晶
胡海华
伍一波
郭文莉
李树新
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Petrochina Co Ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00Crosslinking
    • C08L2312/04Crosslinking with phenolic resin

Abstract

The invention provides a composite material of isobutene/alkylstyrene polymer and fluororubber and a preparation method thereof, the composite material prepared by the method has the advantages that the Shore A is 50-70, the tensile strength is 9.0-18.0 MPa, the elongation at break is 250-400%, the ASTM3# standard oil resistance change rate is 6-13% in mass change rate, 8-15% in volume change rate, 13-20% in compression permanent deformation (× 70h at 120 ℃), the aging coefficient is K less than or equal to 0.135, the composite material has good oil resistance and aging resistance, and the service life of a sealing material is prolonged.

Description

Composite material of isobutene/alkylstyrene polymer and fluororubber and preparation method thereof
Technical Field
The invention relates to the field of fluororubber composite materials and preparation thereof, in particular to an isobutylene/alkylstyrene polymer and fluororubber composite material and a preparation method thereof.
Background
The fluorine rubber (FKM) is a special synthetic polymer elastomer containing fluorine atoms on carbon atoms of a main chain or a side chain, has excellent high temperature resistance, oil resistance and chemical resistance, good physical and mechanical properties, weather resistance, electric insulation, radiation resistance and the like, is widely applied to the fields of aerospace, aviation, military industry, national defense, automobiles, petrochemical industry and the like, wherein 75% of the yield is used for manufacturing O-rings, sealing elements, oil pipes, electric circuit sheath gaskets and gasket materials. Although fluororubbers have many excellent properties, they have disadvantages such as poor molding flowability, easy compression set, poor compatibility between the raw rubber processing technique and the physical properties of vulcanized rubber, and the like. Therefore, composite materials were studied.
The lubricating material is prepared by adding 0.1-5 parts by weight of fatty acid monoamide to 100 parts by weight of fluororubber to prepare a fluororubber composition, the fluororubber composition has good mold release performance, the molded product obtained by vulcanizing and molding the composition is prepared by adding 100 parts by weight of a flame retardant, a sealing material, a vehicle.
JP19870107743 describes a new coating for a new fluoroelastomer material consisting of an organic substance (such as vegetable oil, polyvinyl chloride plasticizer, rubber blend or silicone oil process oil) mixed with borax (for example, except borax; hydrated alumina, magnesia, natural sand, quartz powder, fluorite, perlite) and the like. JP2011063133(a) describes a luminescent sheet comprising a fluorine-containing rubber, which has a good luminescent effect over a long period of time, mainly by blending a luminescent material with or depositing a luminescent material on the rubber or plastic, and making the mixture into a sheet. JP2011063133(a) and JP5336313(B2) design a new rubber product by improving the interaction between organic molecules and inorganic compounds, and the raw material comprises fluorine rubber. GB1438404(A) describes gypsum containing fluororubber and possibly inorganic fillers, such as bauxite, fluorite, cryolite, graphite, quartz, flint, sand, sulphur, boron, aluminium profiles, borax, fine shale, aluminium, sillimanite, agalmatolite and the like. KR20100029345(a) provides a far infrared ray radiation pad which maintains infrared cushioning. The structure is as follows: 35-40 w% of silicon oxide, 23-28 w% of feldspar oxide, 25-29 w% of borax, 0.2-0.8 w% of boric acid, 0.4-0.8 w% of cobalt, 1.5-2 w% of magnesium, 0.7-1.2 w% of selenium, 0.14-cryolite alumina, 0.19 w% of lithium, 1.5-2 w% of zircon, 0.3-0.8 w% of fluorite, 0.2-0.9 w% of porcelain color and the like, and the components are mixed, melted, solidified and crushed. The infrared powder-discharging mixed softening agent is selected from soft synthetic resin and silicon rubber or the ratio of 1:4 to 1: 8. Thereafter, the mixture is injection molded.
Disclosure of Invention
The invention aims to provide a composite material of an isobutene/alkylstyrene polymer and fluororubber and a preparation method thereof, and the prepared composite material has excellent sealing performance.
The composite material of the isobutene/alkylstyrene polymer and the fluororubber comprises the following components in parts by weight based on 100 parts of the total mass of the isobutene/alkylstyrene polymer and the fluororubber: 30-45 parts of isobutene/alkylstyrene polymer, 55-70 parts of fluororubber, 2.5-8.0 parts of vulcanizing agent, 1-4 parts of vulcanization accelerator, 0.5-2 parts of silane coupling agent, 6-14 parts of plasticizer, 2-9 parts of activating agent and 30-60 parts of filler.
The invention also provides a preparation method of the composite material of the isobutene/alkylstyrene polymer and the fluororubber, which comprises the following steps: adding isobutene/alkylstyrene polymer, fluororubber, filler and silane coupling agent into an open mill, open milling for 3-10 min at 20-40 ℃, heating to 40-80 ℃, adding plasticizer, activator and vulcanizing agent, mixing for 2-10 min, adding vulcanization accelerator, continuously mixing for 2-6 min, thinly passing through a lower sheet to obtain a mixed material, and vulcanizing for 20 min-1 h under the vulcanization condition of 150-180 ℃ and 9-15 MPa to obtain the isobutene/alkylstyrene polymer and fluororubber composite material.
According to the preparation method of the isobutylene/alkylstyrene polymer and fluororubber composite material, the filler can be added again before the sheet is thin-passed, the added filler is preferably graphene oxide, and the adding amount is 5-10 parts.
The isobutene/alkylstyrene polymer is an isobutene/(C3-C12) styrene polymer, such as an isobutene/o-methylstyrene polymer, an isobutene/m-methylstyrene polymer, an isobutene/p-methylstyrene polymer, an isobutene/o-ethylstyrene polymer, an isobutene/m-ethylstyrene polymer, an isobutene/p-ethylstyrene polymer and the like.
The vulcanizing agent, the vulcanization accelerator, the silane coupling agent, the plasticizer, the activator and the filler are all common auxiliary agents in the field, and specific varieties and dosage can be selected according to common general knowledge of technicians in the field.
The vulcanizing agents are 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and phenolic resin, and the dosage of the vulcanizing agents is 0.5-1 part and 2-7 parts respectively.
The vulcanization accelerator is TETD or CZ or a mixture thereof.
The silane coupling agent is one or a mixture of KH-560 and KH-602.
The plasticizer is one or more of polytetrafluoroethylene, phthalate, isophthalate and citrate.
The activating agent is one or more of zinc stearate, zinc oxide and triethanolamine.
The filler is one or more of spray carbon black, graphene oxide and carbon nano tubes.
The roll spacing of the open mill is 0.5-1 mm.
The number of the thin pass is 3-5.
The parts are all parts by mass.
The molecular chain of the isobutylene/alkylstyrene polymer is saturated, the isobutylene/alkylstyrene polymer is not easy to vulcanize in the processing process, and the carbon atoms of the main chain or the side chain of the fluororubber contain fluorine atoms, so that the fluororubber is compounded with the isobutylene/alkylstyrene polymer, the processing and vulcanizing characteristics of the polymer are greatly improved.
Detailed Description
The present invention is further described below with reference to examples. It should be noted that the following examples are not intended to limit the scope of the present invention, and any modifications made on the basis of the present invention do not depart from the spirit of the present invention.
The required medicines are all commercial industrial products.
Test methods and standards: mooney viscosity: SH/T1232.1-2000 roll-through method; 300% stress at definite elongation, tensile strength, elongation at break: SH/T1600-2004, procedure 1ASTM IRB NO7 carbon Black, GB/T528-2009, type 1 cutter; oil resistance: GB/T1690-2006.
Example 1
The temperature of an open mill is raised to 20 ℃, the roller distance is adjusted to lmm, 30 parts of isobutylene/o-methylstyrene polymer, 70 parts of fluororubber, 40 parts of spray carbon black and graphene oxide (the mass ratio of the spray carbon black to the graphene oxide is 1:1) and 1 part of KH-560 silane coupling agent are added for open milling for 6min, the temperature is raised to 70 ℃, 6 parts of polytetrafluoroethylene and 3 parts of phthalate are added, 5 parts of zinc stearate, 2 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 24023 parts of phenolic tackifying resin, mixing for 5min, adding 1 part of vulcanization accelerator TETD, continuing to mix for 6min, finally adding 1 part of graphene oxide, mixing for 8min, 3 times respectively for a left 3/4 cutter and a right 3/4 cutter, adjusting the roller distance to 0.5mm, thinly passing through for 5 times to obtain a mixed material, and vulcanizing for 30min under the vulcanization condition of 170 ℃ and 15MPa to obtain the composite material of the isobutylene/o-methylstyrene polymer and the fluororubber.
Comparative example 1
The test formulation and conditions were the same as in example 1 except that 30 parts of isobutylene/o-methylstyrene polymer was not added.
Example 2
The temperature of an open mill is raised to 40 ℃, the roller distance is adjusted to lmm, 35 parts of isobutylene/m-methylstyrene polymer, 65 parts of fluororubber, 50 parts of spray carbon black and carbon nano tube (the mass ratio of the spray carbon black to the carbon nano tube is 1:1) and 2 parts of KH-560 silane coupling agent are added for open milling for 3min, the temperature is raised to 50 ℃, 6 parts of polytetrafluoroethylene and 4 parts of zinc stearate are added, 3 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 24024 parts of phenolic tackifying resin, mixing for 6min, adding 2 parts of accelerator TETD, continuing mixing for 6min, finally adding 1.5 parts of graphene oxide, mixing for 4min, 3 times respectively for a left 3/4 cutter and a right 3/4 cutter, adjusting the roller distance to 0.5mm, thinly passing for 5 times to obtain a mixed material, and vulcanizing for 30min under the vulcanization condition of 160 ℃ and 12MPa to obtain the composite material of the isobutylene/m-methylstyrene polymer and the fluororubber.
Comparative example 2
The test formulation and conditions were the same as in example 2 except that 35 parts of isobutylene/m-methylstyrene polymer was not added.
Example 3
The temperature of an open mill is raised to 30 ℃, the roller distance is adjusted to lmm, 40 parts of isobutylene/p-methylstyrene polymer, 60 parts of fluororubber, 50 parts of spray carbon black, 50 parts of graphene oxide and carbon nano tube (the mass ratio of the spray carbon black, the graphene oxide and the carbon nano tube is 1:1:1) and 2 parts of KH-560 silane coupling agent are added for open milling for 5min, the temperature is raised to 60 ℃, 7 parts of polytetrafluoroethylene are added, 5 parts of zinc stearate, 3 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 24026 parts of phenolic tackifying resin, mixing for 10min, adding 1 parts of accelerator TETD, continuing mixing for 2min, finally adding 0.5 part of graphene oxide, mixing for 3min, mixing 3 times respectively by a left 3/4 cutter and a right 3/4 cutter, adjusting the roller distance to 0.5mm, thinly passing through for 5 times to obtain a mixed material, and vulcanizing for 1h under the vulcanization condition of 150 ℃ and 10MPa to obtain the composite material of the isobutylene/p-methylstyrene polymer and the fluororubber.
Comparative example 3
The test formulation and conditions were the same as in example 3 except that 40 parts of isobutylene/para-methylstyrene polymer was not added.
Example 4
The temperature of an open mill is raised to 40 ℃, the roller distance is adjusted to lmm, 45 parts of isobutylene/p-methylstyrene polymer, 55 parts of fluororubber, 50 parts of spray carbon black, 50 parts of graphene oxide and carbon nano tube (the mass ratio of the spray carbon black to the graphene oxide to the carbon nano tube is 1:2:1) and 1 part of KH-560 silane coupling agent are added for open milling for 3min, the temperature is raised to 80 ℃, 8 parts of polytetrafluoroethylene are added, 3 parts of zinc stearate, 3 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 24025 parts of phenolic tackifying resin, mixing for 5min, adding 2 parts of accelerator TETD, continuing mixing for 5min, finally adding 1.0 part of graphene oxide, mixing for 5min, respectively 3 times by a left cutter and a right cutter 3/4 cutter, adjusting the roller distance to 0.5mm, thinly passing through for 5 times to obtain a mixed material, and vulcanizing for 30min under the vulcanization condition of 170 ℃ and 12MPa to obtain the composite material of the isobutylene/p-methylstyrene polymer and the fluororubber.
Comparative example 4
The test formulation and conditions were the same as in example 4 except that 45 parts of isobutylene/para-methylstyrene polymer was not added.
Example 5
The temperature of an open mill is raised to 30 ℃, the roller distance is adjusted to lmm, 35 parts of isobutylene/o-methylstyrene polymer, 65 parts of fluororubber, 50 parts of spray carbon black and graphene oxide (the mass ratio of the spray carbon black to the graphene oxide is 1:2) and 1.5 parts of KH-560 silane coupling agent are added for open milling for 6min, the temperature is raised to 80 ℃, 8 parts of polytetrafluoroethylene and 5 parts of zinc stearate are added, 2 parts of zinc oxide, 0.8 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 24022 parts of phenolic tackifying resin, mixing for 6min, adding a promoter TETD1 parts, continuing mixing for 3min, finally adding 1.5 parts of graphene oxide, mixing for 8min, 3 times respectively for a left 3/4 cutter and a right 3/4 cutter, adjusting the roller distance to 0.5mm, thinly passing through for 5 times to obtain a mixed material, and vulcanizing for 30min under the vulcanization condition of 160 ℃ and 15MPa to obtain the composite material of the isobutylene/o-methylstyrene polymer and the fluororubber.
Comparative example 5
The test formulation and conditions were the same as in example 5 except that 35 parts of isobutylene and o-methylstyrene polymer were not added.
Example 6
The temperature of an open mill is raised to 20 ℃, the roller distance is adjusted to lmm, 45 parts of isobutylene/m-methylstyrene polymer, 55 parts of fluororubber, 50 parts of spray carbon black and carbon nano tube (the mass ratio of the spray carbon black to the carbon nano tube is 1:2) and 2 parts of KH-560 silane coupling agent are added for open milling for 6min, the temperature is raised to 50 ℃, 10 parts of polytetrafluoroethylene and 3 parts of zinc stearate are added, 3 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 24026 parts of phenolic tackifying resin, mixing for 6min, adding 1 part of accelerator TETD, continuing mixing for 6min, finally adding 1.0 part of graphene oxide, mixing for 8min, 3 times respectively for a left 3/4 cutter and a right 3/4 cutter, adjusting the roller distance to 0.5mm, thinly passing for 5 times to obtain a mixed material, and vulcanizing for 30min under the vulcanization condition of 180 ℃ and 10MPa to obtain the composite material of the isobutylene/m-methylstyrene polymer and the fluororubber.
Comparative example 6
The test formulation and conditions were the same as in example 6 except that no 45 parts of isobutylene/m-methylstyrene polymer was added.
Example 7
The temperature of an open mill is raised to 20 ℃, the roller distance is adjusted to lmm, 35 parts of isobutylene/o-methylstyrene polymer, 65 parts of fluororubber, 40 parts of spray carbon black and graphene oxide (the mass ratio of the spray carbon black to the graphene oxide is 1:1) and 2 parts of KH-560 silane coupling agent are added for open milling for 6min, the temperature is raised to 70 ℃, 6 parts of polytetrafluoroethylene and 3 parts of phthalate are added, 5 parts of zinc stearate, 2 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and 24023 parts of phenolic tackifying resin are mixed for 5min, 1 part of vulcanization accelerator TETD is added to be continuously mixed for 6min, the left and right 3/4 cutters are respectively mixed for 3 times, the roller distance is adjusted to 0.5mm, the materials are thinly passed through for 5 times and are sliced to obtain mixed materials, and then the mixed materials are vulcanized for 30min under the vulcanization condition of 170 ℃ and 15MPa, so that the composite material of the isobutylene/o-methylstyrene polymer and the fluororubber is obtained.
Comparative example 7
The test formulation and conditions were the same as in example 7 except that 35 parts of isobutylene/o-methylstyrene polymer was not added.
Example 8
The temperature of an open mill is raised to 40 ℃, the roller distance is adjusted to lmm, 40 parts of isobutylene/m-methylstyrene polymer, 60 parts of fluororubber, 50 parts of spray carbon black, 50 parts of graphene oxide and carbon nano tube (the mass ratio of the spray carbon black to the graphene oxide to the carbon nano tube is 1:1:1) and 2 parts of KH-560 silane coupling agent are added for open milling for 3min, the temperature is raised to 50 ℃, 6 parts of polytetrafluoroethylene are added, 4 parts of zinc stearate, 3 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and 24024 parts of phenolic tackifying resin are mixed for 6min, 2 parts of accelerator TETD are added to be continuously mixed for 6min, the left and right 3/4 cutters are respectively mixed for 3 times, the roller distance is adjusted to 0.5mm, the mixture is obtained by thin passing for 5 times and then is vulcanized for 30min under the vulcanization condition of 170 ℃ and 12MPa, and the composite material of the isobutylene/m-methylstyrene polymer and the fluororubber is obtained.
Comparative example 8
The test formulation and conditions were the same as in example 8 except that 40 parts of isobutylene/m-methylstyrene polymer was not added.
Example 9
The open mill is heated to 30 ℃, the roller distance is adjusted to lmm, 35 parts of isobutylene/p-methylstyrene polymer, 65 parts of fluororubber, 50 parts of graphene oxide and carbon nano tube (the mass ratio of the graphene oxide to the carbon nano tube is 1:1), 2 parts of KH-560 silane coupling agent are added for open milling for 5min, the temperature is increased to 60 ℃, 7 parts of polytetrafluoroethylene, 5 parts of zinc stearate, 3 parts of zinc oxide, 0.5 part of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and 24026 parts of phenolic tackifying resin are added for mixing for 10min, then the accelerant TETD1 is added for mixing for 2min, 3 times are respectively carried out on a left cutter and a right cutter 3/4, the roller distance is adjusted to 0.5mm, the mixture is obtained by thin passing for 5 times, and then the mixture is vulcanized for 1h under the vulcanization condition of 160 ℃ and 10MPa, and the isobutylene/p-methylstyrene polymer and fluororubber composite is obtained.
Comparative example 9
The test formulation and conditions were the same as in example 9 except that 35 parts of isobutylene/para-methylstyrene polymer was not added.
TABLE 1 Properties of composites obtained in examples and comparative examples
Figure GDA0002431148730000101

Claims (11)

1. The composite material of the isobutene/alkyl styrene polymer and the fluororubber is characterized by comprising the following components in parts by weight based on 100 parts of the total mass of the isobutene/alkyl styrene polymer and the fluororubber: 30-45 parts of isobutene/alkyl styrene polymer, 55-70 parts of fluororubber, 2.5-8.0 parts of vulcanizing agent, 1-4 parts of vulcanization accelerator, 0.5-2 parts of silane coupling agent, 6-14 parts of plasticizer, 2-9 parts of activating agent and 30-60 parts of filler,
wherein the isobutylene/alkylstyrene polymer is an isobutylene/o-methylstyrene polymer, an isobutylene/m-methylstyrene polymer, an isobutylene/p-methylstyrene polymer, an isobutylene/o-ethylstyrene polymer, an isobutylene/m-ethylstyrene polymer, or an isobutylene/p-ethylstyrene polymer, and
the vulcanizing agents are 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and phenolic resin, and the using amounts of the vulcanizing agents are 0.5-1 part and 2-7 parts respectively.
2. Composite material according to claim 1, characterized in that the vulcanization accelerator is one of the accelerators TETD, CZ or mixtures thereof.
3. The composite material of claim 1, wherein the silane coupling agent is selected from the group consisting of KH-560, KH-602, and mixtures thereof.
4. The composite material of claim 1, wherein the plasticizer is one or more of polytetrafluoroethylene, phthalate, isophthalate, and citrate.
5. The composite material of claim 1, wherein the activator is one or more of zinc stearate, zinc oxide, and triethanolamine.
6. The composite material of claim 1, wherein the filler is one or more of spray carbon black, graphene oxide, and carbon nanotubes.
7. A method for preparing the isobutylene/alkylstyrene polymer and fluororubber composite according to claim 1, comprising the steps of: adding isobutene/alkylstyrene polymer, fluororubber, filler and silane coupling agent into an open mill, open milling for 3-10 min at 20-40 ℃, heating to 40-80 ℃, adding plasticizer, activator and vulcanizing agent, mixing for 2-10 min, adding vulcanization accelerator, continuously mixing for 2-6 min, thinly passing through a lower sheet to obtain a mixed material, and vulcanizing for 20 min-1 h under the vulcanization condition of 150-180 ℃ and 9-15 MPa to obtain the isobutene/alkylstyrene polymer and fluororubber composite material.
8. The method according to claim 7, wherein the filler is further added and kneaded for 3 to 6 minutes before the sheet is drawn down, and the amount of the filler added is 0.5 to 5 parts by weight based on the total amount of the filler.
9. The method according to claim 8, wherein the filler is graphene oxide.
10. The preparation method of claim 7, wherein the roll gap of the open mill is 0.5-1 mm.
11. The method according to claim 7, wherein the number of thin passes is 3 to 5.
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CN104602911A (en) * 2012-09-06 2015-05-06 埃克森美孚化学专利公司 Construction comprising tie layer
CN104619520A (en) * 2012-09-12 2015-05-13 住友电木株式会社 Tire inner liner sheet and tire
CN104583087A (en) * 2013-02-08 2015-04-29 诺玛科公司 Closure for a product-retaining container

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