CN116178847B - High-temperature-resistant and liquid-resistant ethylene propylene rubber compound and preparation method thereof - Google Patents

High-temperature-resistant and liquid-resistant ethylene propylene rubber compound and preparation method thereof Download PDF

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CN116178847B
CN116178847B CN202211580511.6A CN202211580511A CN116178847B CN 116178847 B CN116178847 B CN 116178847B CN 202211580511 A CN202211580511 A CN 202211580511A CN 116178847 B CN116178847 B CN 116178847B
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ethylene propylene
resistant
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rubber compound
liquid
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CN116178847A (en
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李志俊
胡国华
姚能品
陈奕杰
张宁君
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Ningguo Secos Rubber Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
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    • C08K2003/222Magnesia, i.e. magnesium oxide
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02TCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
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Abstract

The invention provides a high-temperature-resistant and liquid-resistant ethylene propylene rubber compound and a preparation method thereof, wherein the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound comprises the following raw materials in parts by weight: 20-100 parts of ethylene propylene diene monomer, 0-80 parts of ethylene propylene diene monomer, 6-14 parts of an activating agent, 0.5-2 parts of a release agent, 2-8 parts of an anti-aging agent, 1-3 parts of a dispersing agent, 30-70 parts of a reinforcing filler, 0-10 parts of a plasticizer, 5-10 parts of dicumyl peroxide DCP and a double-five composite cross-linking agent and 0-5 parts of an auxiliary cross-linking agent. The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound rubber and the preparation method thereof provided by the invention have the advantages of good hardness, breaking strength, breaking elongation, pressure change, processing and other performances, and particularly have excellent high-temperature resistance and liquid resistance.

Description

High-temperature-resistant and liquid-resistant ethylene propylene rubber compound and preparation method thereof
Technical Field
The invention relates to the technical field of rubber materials, in particular to a high-temperature-resistant and liquid-resistant ethylene propylene rubber compound and a preparation method thereof.
Background
With the rapid development of the domestic automobile industry, the requirements of meeting high standard performance are also paid special attention, in particular to an automobile radiator and a cooling sealing system; the automobile radiator is an indispensable important component in an automobile water-cooled engine cooling system, and is developing towards light, efficient and economical directions; the automobile radiator structure is also continuously suitable for new development, so the requirements of long-term high temperature resistance and small liquid change resistance of the ethylene propylene rubber product meeting the public standard TL52316 are also more urgent.
At present, under actual use conditions, the product manufactured by the common ethylene propylene rubber can not meet the standard requirements of the product, and the main surfaces are as follows: the ethylene propylene rubber product has large change under long-term high-temperature working condition; liquid leakage occurs under long-term liquid-resistant working conditions.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-temperature-resistant and liquid-resistant ethylene propylene rubber compound and a preparation method thereof, wherein the compound has good performances of hardness, breaking strength, breaking elongation, pressure change, processing and the like, and particularly has excellent high-temperature resistance and liquid resistance.
The invention provides a high-temperature-resistant and liquid-resistant ethylene propylene rubber compound, which comprises the following raw materials in parts by weight:
20-100 parts of ethylene propylene diene monomer, 0-80 parts of ethylene propylene diene monomer, 6-14 parts of an activating agent, 0.5-2 parts of a release agent, 2-8 parts of an anti-aging agent, 1-3 parts of a dispersing agent, 30-70 parts of a reinforcing filler, 0-10 parts of a plasticizer, 5-10 parts of dicumyl peroxide DCP and a double-five composite cross-linking agent and 0-5 parts of an auxiliary cross-linking agent.
In the invention, the ethylene propylene diene monomer EPDM containing the third monomer and the ethylene propylene diene monomer EPM with high ethylene content are combined, so that the ageing resistance of the obtained ethylene propylene rubber compound is improved, and the processability of the obtained ethylene propylene rubber compound is further improved due to widening of the molecular weight distribution; furthermore, the ethylene propylene diene monomer and ethylene propylene diene monomer are co-vulcanized by adjusting a vulcanization system, so that the obtained rubber material has low compression set and good heat resistance and chemical stability while the high temperature resistance is obtained.
Preferably, the comonomer of the ethylene propylene diene monomer comprises at least one of 5-ethylidene-2-norbornene, 5-vinyl-2-norbornene, dicyclopentadiene or 1, 4-hexadiene in addition to ethylene and propylene;
Preferably, the weight ratio of the ethylene propylene diene monomer to the ethylene propylene diene monomer is 1-3:1.
In the invention, when the ethylene propylene diene monomer and the ethylene propylene diene monomer meet the mass ratio of 1-3:1, the crosslinking density of the obtained rubber compound is increased, and the performances such as high temperature resistance, compression deformation and the like are continuously improved.
Preferably, the activator is at least one of zinc oxide, magnesium oxide or calcium oxide;
preferably, the activator comprises zinc oxide and magnesium oxide in a mass ratio of 1-1.5:1.
In the invention, when the zinc oxide and the magnesium oxide are compounded to be used as an activating agent, the high temperature resistance of the obtained mixed rubber can be further improved, and the heat conduction effect can be realized on the vulcanization and the application of products.
Preferably, the release agent is at least one of stearic acid, zinc stearate or calcium stearate.
Preferably, the release agent is zinc stearate.
Preferably, the anti-aging agent is at least one of zinc salt of 2-mercaptomethyl benzimidazole, 4' -bis (phenylisopropyl) diphenylamine or 2, 4-trimethyl-1, 2-dihydroquinoline polymer;
Preferably, the anti-aging agent comprises zinc salt of 2-mercaptomethyl benzimidazole, 4 '-di (phenylisopropyl) diphenylamine and 2, 4-trimethyl-1, 2-dihydroquinoline polymer, and the mass ratio of the zinc salt to the 4,4' -di (phenylisopropyl) diphenylamine to the 2, 4-trimethyl-1, 2-dihydroquinoline polymer is 1:1-2.
In the invention, when the 2-thiol methyl benzimidazole zinc salt is compounded with 4,4' -di (phenyl isopropyl) diphenylamine and the 2, 4-trimethyl-1, 2-dihydroquinoline polymer, the crosslinking characteristic of the obtained rubber compound can be further improved, and the obtained rubber compound has the best temperature resistance and aging resistance.
Preferably, the reinforcing filler is at least one of carbon black, white carbon black, calcium carbonate or talcum powder;
preferably, the reinforcing filler is at least one of carbon black N330, carbon black N375, carbon black N339 or carbon black N550.
Preferably, the dispersant is a fatty acid derivative; preferably, the dispersant is at least one of dispersant WB42, dispersant WB212 or dispersant RDP-100;
preferably, the plasticizer is at least one of paraffin oil, pine tar, naphthenic oil or paraffin oil; preferably, the plasticizer is paraffin oil.
Preferably, the dicumyl peroxide DCP and the bibiwu composite cross-linking agent are supported composite cross-linking agents, which are obtained by using carbon nanotubes as carriers and adsorbing the dicumyl peroxide DCP and the biwu on the carriers;
preferably, the surface of the carbon nano tube is grafted with acrylic ester;
Preferably, the dicumyl peroxide DCP and the biwurtzite composite cross-linking agent are prepared by the following method: acidifying the carbon nanotube to obtain a carboxylated carbon nanotube, and reacting hydroxyethyl acrylate or hydroxypropyl acrylate with the carboxylated carbon nanotube to obtain a carbon nanotube with acrylate grafted on the surface; and dispersing the carbon nano tube with the acrylic ester grafted on the surface, dicumyl peroxide DCP and biwurtzite in an organic solvent, and stirring and mixing completely to obtain the dicumyl peroxide DCP and biwurtzite composite cross-linking agent.
According to the invention, after dicumyl peroxide DCP and bibiwu are adsorbed on a carrier of a carbon nano tube, the high specific surface area of the carbon nano tube and the specific dispersion characteristic of the carbon nano tube in an ethylene propylene rubber matrix can be utilized to effectively optimize the dispersion uniformity of a solid phase crosslinking agent of dicumyl peroxide and a biwu liquid phase crosslinking agent in the ethylene propylene rubber, so that the crosslinking degree of the crosslinking agent on the ethylene propylene rubber is improved, and the excellent high temperature resistance and liquid resistance of the obtained rubber compound are endowed; meanwhile, acrylic ester is grafted on the surface of the carbon nano tube, unsaturated double bonds contained in the acrylic ester are crosslinked to a rubber network through a crosslinking reaction, so that the effect of the carbon nano tube serving as reinforcing filler is more obvious, and the mechanical property of the obtained rubber compound is further improved.
According to the invention, after acidification of the carbon nanotube, a carboxylated carbon nanotube is obtained, carboxyl contained on the surface of the carboxylated carbon nanotube can be subjected to an ester bond condensation method with hydroxyl of hydroxyethyl acrylate or hydroxypropyl acrylate to obtain the carbon nanotube with acrylate grafted on the surface, and the dicumyl peroxide DCP and the bibipenta are adsorbed in the carbon nanotube by utilizing a lumen structure of the carbon nanotube with acrylate monomer grafted on the surface to obtain the dicumyl peroxide DCP and the bipenta-compound cross-linking agent.
Preferably, the auxiliary crosslinking agent is at least one of triallyl isocyanate, trimethylolpropane trimethacrylate or ethylene glycol dimethacrylate.
The invention also provides a preparation method of the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound, which comprises the following steps: uniformly mixing ethylene propylene diene monomer and ethylene propylene diene monomer, adding an activating agent, a release agent, an anti-aging agent, a dispersing agent, a reinforcing filler and a plasticizer, uniformly mixing, and discharging rubber to obtain a section of rubber compound; after the primary rubber compound is stood, adding dicumyl peroxide DCP, a bi-di-penta compound cross-linking agent and a co-cross-linking agent, uniformly mixing, and discharging rubber to obtain final rubber compound; and vulcanizing the final rubber compound to obtain a finished product, namely the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound.
Compared with the traditional ethylene propylene rubber compound, the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound has better tensile strength, low-pressure change performance and high-temperature resistance and elasticity performance, and meets the long-term high-temperature-resistant and liquid-resistant requirements of sizing materials.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is prepared from the following raw materials in parts by weight: 60 parts of ethylene propylene diene monomer (5-ethylidene-2-norbornene, 5.0 wt%) ethylene propylene diene monomer 40 parts, zinc oxide 5 parts, magnesium oxide 4 parts, zinc stearate 1 parts, zinc salt of 2-mercaptomethylbenzimidazole 1.5 parts, 4' -bis (phenylisopropyl) diphenylamine 1.5 parts, 2 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, a dispersant WB421.5 parts, carbon black N33050 parts, paraffin oil 6 parts, dicumyl peroxide DCP and a bis-penta composite cross-linking agent 8 parts, and triallyl isocyanate (TAIC) 3 parts;
The dicumyl peroxide DCP and the biwurtzite composite cross-linking agent are prepared by the following method: adding the carbon nano tube into concentrated nitric acid according to the weight-to-volume ratio of 1:10 (g/mL), heating and refluxing for reaction overnight after uniform ultrasonic dispersion, filtering, washing with water, and drying to obtain carboxylated carbon nano tube; adding the carboxylated carbon nanotube and hydroxyethyl acrylate into acetone according to the mass ratio of 12:1, adding DMAP accounting for 0.5wt% of the mass of the carboxylated carbon nanotube and DCC accounting for 1wt% of the mass of the carboxylated carbon nanotube, and stirring and reacting for 3 hours to obtain the carbon nanotube with the surface grafted with acrylic ester; and (3) dissolving dicumyl peroxide DCP and bibiwu in absolute ethyl alcohol according to a mass ratio of 3:1, adding 1 times of dicumyl peroxide DCP and biwu mass of the carbon nano tube with the surface grafted with acrylic ester under stirring, stirring and mixing for 3 hours at 30 ℃, distilling under reduced pressure to remove the solvent, and drying in an oven completely to obtain the dicumyl peroxide DCP and biwu composite cross-linking agent.
The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is prepared by the following method:
(1) And (3) mixing: mixing ethylene propylene diene monomer and ethylene propylene diene monomer in an internal mixer according to the weight parts for 45s, then adding zinc oxide, magnesium oxide, zinc stearate, 2-mercaptomethylbenzimidazole zinc salt, 4' -di (phenylisopropyl) diphenylamine, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, a dispersing agent WB42, carbon black N330 and paraffin oil, mixing for 45s, lifting a bolt, turning over rubber, pressing a bolt, mixing to 150 ℃ and discharging rubber, wherein the bolt is lifted once at 120 ℃ and 135 ℃ respectively, and the time is 20s, thus obtaining a section of mixed rubber;
(2) Two-stage mixing: standing the first-stage rubber compound for 20 hours, adding dicumyl peroxide DCP, a bi-di-penta compound cross-linking agent and triallyl isocyanate, mixing to 115 ℃, and discharging rubber to obtain final rubber compound;
(3) Vulcanizing: and (3) after the final rubber mixture is molded, the final rubber mixture is sent to a vulcanizing machine and vulcanized for 10 minutes at 170 ℃ to obtain a finished product, namely the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound.
Example 2
The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is prepared from the following raw materials in parts by weight: 90 parts of ethylene propylene diene monomer (5-ethylidene-2-norbornene, 5.0 wt%) ethylene propylene diene monomer, 30 parts of ethylene propylene diene monomer, 6 parts of zinc oxide, 4 parts of magnesium oxide, 2 parts of zinc stearate, 2 parts of zinc salt of 2-mercaptomethylbenzimidazole, 2 parts of 4,4' -bis (phenylisopropyl) diphenylamine, 2 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 423 parts of dispersant WB, 33070 parts of carbon black N, 10 parts of paraffin oil, 10 parts of dicumyl peroxide DCP and a compound crosslinking agent of bis (penta) and 5 parts of triallyl isocyanate (TAIC);
The dicumyl peroxide DCP and the biwurtzite composite cross-linking agent are prepared by the following method: adding the carbon nano tube into concentrated nitric acid according to the weight-to-volume ratio of 1:10 (g/mL), heating and refluxing for reaction overnight after uniform ultrasonic dispersion, filtering, washing with water, and drying to obtain carboxylated carbon nano tube; adding the carboxylated carbon nanotube and hydroxyethyl acrylate into acetone according to the mass ratio of 12:1, adding DMAP accounting for 0.5wt% of the mass of the carboxylated carbon nanotube and DCC accounting for 1wt% of the mass of the carboxylated carbon nanotube, and stirring and reacting for 3 hours to obtain the carbon nanotube with the surface grafted with acrylic ester; and (3) dissolving dicumyl peroxide DCP and bibiwu in absolute ethyl alcohol according to a mass ratio of 3:1, adding 1 times of dicumyl peroxide DCP and biwu mass of the carbon nano tube with the surface grafted with acrylic ester under stirring, stirring and mixing for 3 hours at 30 ℃, distilling under reduced pressure to remove the solvent, and drying in an oven completely to obtain the dicumyl peroxide DCP and biwu composite cross-linking agent.
The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is prepared by the following method:
(1) And (3) mixing: mixing ethylene propylene diene monomer and ethylene propylene diene monomer in an internal mixer according to the weight parts for 60s, then adding zinc oxide, magnesium oxide, zinc stearate, 2-mercaptomethyl benzimidazole zinc salt, 4' -di (phenylisopropyl) diphenylamine, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, a dispersing agent WB42, carbon black N330 and paraffin oil, mixing for 60s, lifting a bolt, turning over rubber, pressing a bolt, mixing to 150 ℃ and discharging rubber, wherein the bolt is lifted once at 120 ℃ and 135 ℃ respectively, and the time is 30s, thus obtaining a section of mixed rubber;
(2) Two-stage mixing: standing the first section of rubber compound for 24 hours, adding dicumyl peroxide DCP, a bi-di-penta compound cross-linking agent and triallyl isocyanate, mixing to 120 ℃, and discharging rubber to obtain final rubber compound;
(3) Vulcanizing: and (3) after the final rubber mixture is molded, the final rubber mixture is sent to a vulcanizing machine and vulcanized for 10 minutes at 170 ℃ to obtain a finished product, namely the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound.
Example 3
The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is prepared from the following raw materials in parts by weight: 50 parts of ethylene propylene diene monomer (5-ethylidene-2-norbornene, 5.0 wt%) 50 parts of ethylene propylene diene monomer, 3 parts of zinc oxide, 3 parts of magnesium oxide, 0.5 part of zinc stearate, 1.5 parts of 2-mercaptomethylbenzimidazole zinc salt, 3 parts of 4,4' -bis (phenylisopropyl) diphenylamine, 3 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 421 parts of dispersant WB, 33030 parts of carbon black N, 5 parts of paraffin oil, 5 parts of dicumyl peroxide DCP and a bis-penta composite cross-linking agent, and 2 parts of triallyl isocyanate (TAIC);
The dicumyl peroxide DCP and the biwurtzite composite cross-linking agent are prepared by the following method: adding the carbon nano tube into concentrated nitric acid according to the weight-to-volume ratio of 1:10 (g/mL), heating and refluxing for reaction overnight after uniform ultrasonic dispersion, filtering, washing with water, and drying to obtain carboxylated carbon nano tube; adding the carboxylated carbon nanotube and hydroxyethyl acrylate into acetone according to the mass ratio of 12:1, adding DMAP accounting for 0.5wt% of the mass of the carboxylated carbon nanotube and DCC accounting for 1wt% of the mass of the carboxylated carbon nanotube, and stirring and reacting for 3 hours to obtain the carbon nanotube with the surface grafted with acrylic ester; and (3) dissolving dicumyl peroxide DCP and bibiwu in absolute ethyl alcohol according to a mass ratio of 3:1, adding 1 times of dicumyl peroxide DCP and biwu mass of the carbon nano tube with the surface grafted with acrylic ester under stirring, stirring and mixing for 3 hours at 30 ℃, distilling under reduced pressure to remove the solvent, and drying in an oven completely to obtain the dicumyl peroxide DCP and biwu composite cross-linking agent.
The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is prepared by the following method:
(1) And (3) mixing: mixing ethylene propylene diene monomer and ethylene propylene diene monomer in an internal mixer for 30s according to the weight parts, adding zinc oxide, magnesium oxide, zinc stearate, 2-mercaptomethylbenzimidazole zinc salt, 4' -di (phenylisopropyl) diphenylamine, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, a dispersing agent WB42, carbon black N330 and paraffin oil, mixing for 30s, lifting a bolt, turning over rubber, pressing a bolt, mixing to 150 ℃ and discharging rubber, wherein the bolt is lifted once at 120 ℃ and 135 ℃ respectively, and the time is 10s, thus obtaining a section of mixed rubber;
(2) Two-stage mixing: standing the first-stage rubber compound for 16 hours, adding dicumyl peroxide DCP, a bi-di-penta compound cross-linking agent and triallyl isocyanate, mixing to 110 ℃, and discharging rubber to obtain final rubber compound;
(3) Vulcanizing: and (3) after the final rubber mixture is molded, the final rubber mixture is sent to a vulcanizing machine and vulcanized for 10 minutes at 170 ℃ to obtain a finished product, namely the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound.
Comparative example 1
The ethylene propylene rubber compound rubber is prepared from the following raw materials in parts by weight: 100 parts of ethylene propylene diene monomer (5-ethylidene-2-norbornene, 5.0 wt%) and 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of zinc stearate, 1.5 parts of 2-mercaptomethylbenzimidazole zinc salt, 1.5 parts of 4,4' -bis (phenylisopropyl) diphenylamine, 2 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 421.5 parts of dispersant WB, 33050 parts of carbon black N, 6 parts of paraffin oil, 2 parts of dicumyl peroxide DCP, 2 parts of bis (penta) and 3 parts of triallyl isocyanate (TAIC).
The ethylene propylene rubber compound is prepared by the following method:
(1) And (3) mixing: mixing ethylene propylene diene monomer rubber in an internal mixer for 45s according to the weight parts, adding zinc oxide, magnesium oxide, zinc stearate, zinc salt of 2-mercaptomethyl benzimidazole, 4' -di (phenylisopropyl) diphenylamine, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, a dispersing agent WB42, carbon black N330 and paraffin oil, mixing for 45s, lifting a bolt, turning over rubber, pressing the bolt, mixing to 150 ℃ and discharging rubber, wherein the lifting of the bolt is carried out once at 120 ℃ and 135 ℃ for 20s, and obtaining a section of mixed rubber;
(2) Two-stage mixing: standing the first-stage rubber compound for 20 hours, adding dicumyl peroxide DCP, bis-di-penta-and triallyl isocyanate, mixing to 115 ℃, and discharging rubber to obtain final rubber compound;
(3) Vulcanizing: and (3) after the final rubber compound is molded, feeding the final rubber compound into a vulcanizing machine, and vulcanizing for 10min at 170 ℃ to obtain a finished product, namely the ethylene propylene rubber compound.
Comparative example 2
The ethylene propylene rubber compound rubber is prepared from the following raw materials in parts by weight: 60 parts of ethylene propylene diene monomer (5-ethylidene-2-norbornene, 5.0 wt%) ethylene propylene diene monomer, 40 parts of ethylene propylene diene monomer, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of zinc stearate, 1.5 parts of zinc salt of 2-mercaptomethylbenzimidazole, 1.5 parts of 4,4' -bis (phenylisopropyl) diphenylamine, 2 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 421.5 parts of dispersant WB, 33050 parts of carbon black N, 6 parts of paraffin oil, 3 parts of dicumyl peroxide DCP, 1 part of bis-penta and 3 parts of triallyl isocyanate (TAIC).
The ethylene propylene rubber compound is prepared by the following method:
(1) And (3) mixing: mixing ethylene propylene diene monomer and ethylene propylene diene monomer in an internal mixer according to the weight parts for 45s, then adding zinc oxide, magnesium oxide, zinc stearate, 2-mercaptomethylbenzimidazole zinc salt, 4' -di (phenylisopropyl) diphenylamine, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, a dispersing agent WB42, carbon black N330 and paraffin oil, mixing for 45s, lifting a bolt, turning over rubber, pressing a bolt, mixing to 150 ℃ and discharging rubber, wherein the bolt is lifted once at 120 ℃ and 135 ℃ respectively, and the time is 20s, thus obtaining a section of mixed rubber;
(2) Two-stage mixing: standing the first-stage rubber compound for 20 hours, adding dicumyl peroxide DCP, bis-di-penta-and triallyl isocyanate, mixing to 115 ℃, and discharging rubber to obtain final rubber compound;
(3) Vulcanizing: and (3) after the final rubber compound is molded, feeding the final rubber compound into a vulcanizing machine, and vulcanizing for 10min at 170 ℃ to obtain a finished product, namely the ethylene propylene rubber compound.
The compounds obtained in example 1 and comparative examples 1 to 2 were subjected to the relevant property test, and the test items are shown in Table 1 below.
Table 1 results of Performance test of the compounds of examples and comparative examples
As can be seen from the above table, the performance of the compounds described in the examples is better than that of the compounds described in comparative examples 1-2; the rubber compound disclosed by the invention has the advantages of good hardness, breaking strength, breaking elongation, pressure change, good processability and the like, and particularly has excellent high temperature resistance and liquid resistance.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (15)

1. The high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is characterized by comprising the following raw materials in parts by weight:
20-100 parts of ethylene propylene diene monomer, 0-80 parts of ethylene propylene diene monomer, 6-14 parts of activating agent, 0.5-2 parts of release agent, 2-8 parts of anti-aging agent, 1-3 parts of dispersing agent, 30-70 parts of reinforcing filler, 0-10 parts of plasticizer, 5-10 parts of dicumyl peroxide DCP and a double-five composite cross-linking agent, and 0-5 parts of auxiliary cross-linking agent;
The dicumyl peroxide DCP and the bibiwu composite cross-linking agent are supported composite cross-linking agents, which are obtained by using carbon nanotubes as carriers and adsorbing the dicumyl peroxide DCP and the biwu on the carriers;
Acrylic ester is grafted on the surface of the carbon nano tube;
The dicumyl peroxide DCP and the biwurtzite composite cross-linking agent are prepared by the following method: acidifying the carbon nanotube to obtain a carboxylated carbon nanotube, and reacting hydroxyethyl acrylate or hydroxypropyl acrylate with the carboxylated carbon nanotube to obtain a carbon nanotube with acrylate grafted on the surface; and dispersing the carbon nano tube with the acrylic ester grafted on the surface, dicumyl peroxide DCP and biwurtzite in an organic solvent, and stirring and mixing completely to obtain the dicumyl peroxide DCP and biwurtzite composite cross-linking agent.
2. The high temperature and liquid resistant ethylene propylene rubber compound according to claim 1, wherein the ethylene propylene diene monomer comprises at least one of 5-ethylidene-2-norbornene, 5-vinyl-2-norbornene, dicyclopentadiene or 1, 4-hexadiene in addition to ethylene and propylene.
3. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the weight ratio of the ethylene propylene diene monomer to the ethylene propylene diene monomer is 1-3:1.
4. The high temperature and liquid resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the activator is at least one of zinc oxide, magnesium oxide or calcium oxide.
5. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the activator comprises zinc oxide and magnesium oxide in a mass ratio of 1-1.5:1.
6. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the release agent is at least one of stearic acid, zinc stearate or calcium stearate.
7. The high temperature and liquid resistant ethylene propylene rubber compound according to claim 1 or 2, characterized in that the release agent is zinc stearate.
8. The high temperature and liquid resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the anti-aging agent is at least one of zinc salt of 2-mercaptomethyl benzimidazole, 4' -di (phenylisopropyl) diphenylamine or 2, 4-trimethyl-1, 2-dihydroquinoline polymer.
9. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the anti-aging agent comprises zinc salt of 2-thiol-based methyl benzimidazole, 4' -di (phenylisopropyl) diphenylamine and 2, 4-trimethyl-1, 2-dihydroquinoline polymer, and the mass ratio of the anti-aging agent to the zinc salt of 2-thiol-based methyl benzimidazole is 1:1-2:1-2.
10. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the reinforcing filler is at least one of carbon black, white carbon black, calcium carbonate or talcum powder.
11. The high temperature and liquid resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the reinforcing filler is at least one of carbon black N330, carbon black N375, carbon black N339 or carbon black N550.
12. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, characterized in that the dispersant is a fatty acid derivative;
The plasticizer is at least one of paraffin oil, pine tar, naphthenic oil or paraffin oil.
13. The high temperature-resistant and liquid-resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the dispersant is at least one of dispersant WB42, dispersant WB212 or dispersant RDP-100;
The plasticizer is paraffin oil.
14. The high temperature and liquid resistant ethylene propylene rubber compound according to claim 1 or 2, wherein the co-crosslinking agent is at least one of triallyl isocyanate, trimethylolpropane trimethacrylate or ethylene glycol dimethacrylate.
15. The preparation method of the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound is characterized by comprising the following steps of: uniformly mixing ethylene propylene diene monomer and ethylene propylene diene monomer, adding an activating agent, a release agent, an anti-aging agent, a dispersing agent, a reinforcing filler and a plasticizer, uniformly mixing, and discharging rubber to obtain a section of rubber compound; after the primary rubber compound is stood, adding dicumyl peroxide DCP, a bi-di-penta compound cross-linking agent and a co-cross-linking agent, uniformly mixing, and discharging rubber to obtain final rubber compound; and vulcanizing the final rubber compound to obtain a finished product, namely the high-temperature-resistant and liquid-resistant ethylene propylene rubber compound.
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