CN110527200A - The low temperature resistant high elastic rubber windshield material of one kind, preparation method and windscreen - Google Patents
The low temperature resistant high elastic rubber windshield material of one kind, preparation method and windscreen Download PDFInfo
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- CN110527200A CN110527200A CN201910846760.7A CN201910846760A CN110527200A CN 110527200 A CN110527200 A CN 110527200A CN 201910846760 A CN201910846760 A CN 201910846760A CN 110527200 A CN110527200 A CN 110527200A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of low temperature resistant high elastic rubber windshield material, preparation method and windscreen, the windshield materials to be made of following components by weight: 40-75 parts of ethylene propylene diene rubber；25-60 parts of trielement ethyl butyric rubber；8-12 parts of Liquid Ethylene Propylene Methylene；Maleic anhydride modified polybutadiene 5-8 parts；The ethylene propylene diene rubber and totally 100 parts of the trielement ethyl butyric rubber.The present invention is directed to improve the cryogenic property of EPDM and flexible resistance, resilience performance and resistance to flexion crack growth performance especially under low temperature, physical mechanical property, cryogenic property, resistance to flexion, flame retardant property, in terms of excellent combination property, can satisfy windscreen product technology requirement.
Description
Technical field
The invention belongs to field of rubber materials, more particularly to a kind of low temperature resistant high elastic rubber windshield material, its preparation side
Method and windscreen.
Background technique
Windscreen is the critical component connected between locomotive double heading and vehicle and vehicle, is that crew member and passenger safety are logical
Capable channel.It should also have good longitudinal extension, transverse direction, vertical flexibility in addition to guaranteeing the current safety of passenger, to bear
And adapt to misplace and impact in operation between vehicle, guarantee rolling stock safety curve and track switch.In addition, should also have
Certain sound insulation, heat-insulated, dust-proof and air-tightness.Especially bullet train windscreen generallys use the side that inside and outside windscreen combines
Formula is further promoted and is controlled aerodynamic noise and air drag.Common bullet train is mainly closed jointing and folding with interior windscreen
Two kinds of structures of canopy formula, outer hood then mainly include half-packaging skirtboard type rubber outer hood, the U-shaped rubber outer hood of half-packaging and Quan Bao
Formula bullet train outer hood.This application involves one of rubber material application be as the U-shaped rubber outer hood of light half-packaging
The rubber capsule of (especially standard EMU rubber outer hood).Such product removes in the process of running need to meet environment temperature
Outside the test of factors such as (- 50 DEG C~+70 DEG C), illumination, ozone, sand and dust, sleet, while also needing to meet under frequent torsional deformation
The Functional Requirement of Quick-return, sound insulation and noise reducing.
Ethylene propylene diene rubber (EPDM) is made of ethylene, propylene and unsaturated Third monomer (non-conjugated diene hydrocarbon)
Terpolymer belongs to saturated carbon chains rubber, has brilliant ageing-resistant, resistant to chemical media, excellent electrical insulation characteristics, extensively
Applied to auto industry, wire and cable, sealing material and heat resistant article etc..Although EPDM used by us at present
Rubber is all amorphous, but it still has certain crystallization when ethylene contents are high so that product at low temperature poor flexibility,
Flexural property is poor under height deforms, and can cause because crossing bend windscreen capsule be squeezed significantly torsional deformation in operational process
Windscreen capsule cannot restore in time, issue " whistle ", and more serious generation flexion crackle even cracks, and product is caused to lose
Effect.In addition, ethylene propylene diene rubber be it is non-from reinforcing rubber, self-strength is lower, only 2MPa or so, and belong to inflammable rubber
Glue, thus need to use reinforcement and filler material and a large amount of fire retardants just be able to satisfy windscreen product physical mechanical property require with it is fire-retardant
It is required that.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The low temperature resistant high elastic rubber windshield material of kind, preparation method and windscreen, to improve cryogenic property and flexible resistance.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of low temperature resistant high elastic rubber windshield material, is made of following components by weight:
40-75 parts of ethylene propylene diene rubber；
25-60 parts of trielement ethyl butyric rubber；
8-12 parts of Liquid Ethylene Propylene Methylene；
Maleic anhydride modified polybutadiene 5-8 parts；
The ethylene propylene diene rubber and totally 100 parts of the trielement ethyl butyric rubber.
Further, the ethylene propylene diene rubber selects the raw rubber of ethylene contents 40-50%, ENB content >=8%.
It further, further include low temperature resistant plasticizer 5-15 parts in component, the low temperature resistant plasticizer is trioctyl phosphate
With the mixture of adipic acid dibutyl ester.
It further, further include 21-56 parts of amine salt modified compound fire retardant in component.
Further, the amine salt modified compound fire retardant includes Polyhedral oligomeric silsesquioxane, diethyl hypo-aluminum orthophosphate
And melamine polyphosphate.
It further, further include modified 20-35 parts of white carbon black of gamma-mercaptopropyltriethoxysilane in component.
It further, further include 4-6 parts of compounded curing system in component, the compounded curing system includes that peroxidating two is different
Propyl benzene, Sulfur and N, penylene polymaleimide between N'-.
Further, the compounded curing system further includes Triallyl isocyanurate, N, and N, N- vulcanize four isobutyl groups
One of thiuram or curing dicaprolactam or any combination.
The preparation method of the low temperature resistant high elastic rubber windshield material provided by the invention, comprising: by ethylene-propylene-diene monomer
Glue, trielement ethyl butyric rubber, Liquid Ethylene Propylene Methylene and maleic anhydride modified polybutadiene are uniformly mixed at 50-80 DEG C；Then exist
Amine salt modified compound fire retardant is added at 125-140 DEG C to be kneaded；Modified white carbon black is added to continue to mix at 140-150 DEG C
Refining；It is subsequently added into low temperature resistant plasticizer, is cooled to 80 DEG C or less addition compounded curing systems after mixing；Finally vulcanized
It is made.
Windscreen provided by the invention, using the low temperature resistant high elastic rubber windshield material.
Compared with prior art, the invention has the benefit that
The present invention is directed to improve resilience performance under the cryogenic property of EPDM and flexible resistance, especially low temperature and resistance to bend
Scratch crack growth resistance energy.Contain the ternary second of flexible group (butadiene) using the EPDM collocation of high ENB, low ethylene content
Buna and the Liquid Ethylene Propylene Methylene with high reaction activity, maleic anhydride modified polybutadiene (glass transition temperature -92
DEG C), by introducing flexible group in strand, the regularity of strand is destroyed, the flexibility of strand is enhanced, so that
Intramolecule activity space increases, and main chain mobility is promoted, and reduces glass transition temperature, cryogenic property is substantially improved, especially
It is the resilience and resistance to flexion crack growth performance under low temperature.The polymer composite is lived with stronger chemical reaction simultaneously
Property, it can be chemically reacted with fillers further occurrences such as modified white carbon black and fire retardants, so that entire sizing material forms one completely
Cross-linked network improves the interaction force of sizing material and modified white carbon black and fire retardant, so as to improve mechanical property.
Furthermore Liquid Ethylene Propylene Methylene has the characteristics such as resistant to extraction, high-low temperature resistant, also can be used as reactivity within this material
Plasticizer is used in combination with a small amount of trioctyl phosphate (< -90 DEG C of freezing point), low temperature ester plasticizer, further promotes low-temperature flexibility
And low temperature elasticity, low temperature buckling is reduced, " ejection " is reduced while EPDM glass transition temperature is greatly lowered, is more advantageous to
Rubber windshield surface is bonded elastic coating, to solve due to using single plasticizer easily to spray and cause the wind of coating shedding
Danger, while the resistance to ozone cracking energy of the material is also advantageously improved, it solves product and is also easy to produce asking for crackle in use
Topic, extends the service life of product.
Fire retardant is modified through amine salt, its surface-active can be improved, and improves the interaction force of fire retardant and sizing material, solve by
Caused by fire retardant surface inertness with the problem of sizing material strand interaction force difference, thus reduce because of fire retardant table itself
To the adverse effect of compound physical performance caused by face is inert.
The interaction of dispersibility and white carbon black and sizing material of the white carbon black in sizing material can be improved using modified white carbon black
Power inhibits crystallization while improving mechanical property, improves cold snap-back and resistance to flexion crack growth performance.
Select compounded curing system, peroxide and Sulfur, N, penylene polymaleimide is used in compounding between N'-, is increased
The flexibility for having added the movable free space of segment, having promoted strand ,-C-C- cross-bond, sulfide linkage and the non-sulphur of long-chain of formation
Hetero atom cross-bond further decreases heat and glass transition temperature, promotes cryogenic property and fatigue behaviour.
Using new mixing technique, first fire retardant is added in rubber system under the high temperature conditions, fire retardant can be improved
The compatibility of dispersibility and fire retardant and sizing material in sizing material is further reduced the addition of fire retardant to compound physical performance
Adverse effect.
The present invention comprehensively considers from physical mechanical property, cryogenic property, resistance to flexion, flame retardant property, environmental-protecting performance etc.,
The optimum formula system of the light-colour rubber windshield material of the flame-proof environmental protection of low temperature resistant high rebound long-life, Ke Yiman has finally been determined
Sufficient windscreen product technology requirement, environmental-protecting performance meet iron mark TB/T3139, Q-CRRC J 26-2018 " railway transportation equipment product
Disabling and regulated substance " require and EU REACH Legislation requirement, it is fire-retardant meet DIN5510-2 requirement.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is done below in conjunction with preferred embodiment and more comprehensively, is meticulously described,
But protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
The light-colour rubber windshield material of the environmental protection of the low temperature resistant high rebound long-life of one specific embodiment of the present invention,
Main Components and quality proportioning are as follows: EPDM (ethylene propylene diene rubber) and totally 100 parts of trielement ethyl butyric rubber compound rubber；Liquid second third
8-12 parts of rubber；Maleic anhydride modified polybutadiene 5-8 parts；Low temperature resistant plasticizer 5-15 parts；Amine salt modified compound fire retardant 21-
56 parts；20-35 parts of modified white carbon black；8-15 parts of titanium dioxide；4-6 parts of compounded curing system.
In a specific embodiment, the suitable quality ratio of EPDM and trielement ethyl butyric rubber mixture is 75:25-40:60.
In following Examples 1 to 5, EPDM selects ethylene contents 40-50%, ENB (ethylidene norbornene) content >=8%
Raw rubber, third monomer ENB content is high, and the curingprocess rate and state of cure (vulcanization) of sizing material can be improved, determining to stretch and answer so as to improve sizing material
The physical properties such as power, resilience and buckling；Low ethylene content can inhibit sizing material to crystallize, so that sizing material has lower glass
Change transition temperature, to have excellent cold snap-back and flexural property.Trielement ethyl butyric rubber selects ethylene contents 45-
55%, the raw rubber of ENB content >=6.5%.
In following Examples 1 to 5, the Third monomer of Liquid Ethylene Propylene Methylene is ENB, and content >=7% of ENB.Liquid second
Third rubber has high chemical reactivity, and the compatibility and sizing material and filler of EPDM and trielement ethyl butyric rubber can be improved
Interaction force；Meanwhile Liquid Ethylene Propylene Methylene can play the role of similar plasticizer, improve the cryogenic property of sizing material；In addition, also
The Mooney viscosity of sizing material can be reduced, so as to improve the building-up property of product.
In a specific embodiment, low temperature resistant plasticizer is the mixture of trioctyl phosphate and adipic acid dibutyl ester, is mixed
Conjunction mass ratio is 5:4-8:5.
In a specific embodiment, amine salt modified compound fire retardant mainly includes Polyhedral oligomeric silsesquioxane, diethyl
Base hypo-aluminum orthophosphate and melamine polyphosphate, the mass ratio of three kinds of fire retardants are 1:(3-5): (1-3), gross mass number are
21-56 parts.Amine salt modified compound fire retardant in following Examples 1 to 5, Polyhedral oligomeric silsesquioxane, diethyl hypophosphorous acid
The proportion of aluminium and melamine polyphosphate is 1:4:2.Method of modifying: according to composite flame-retardant agent: Antiradon: -3 uncle of 1- amino
Butyl thiourea molar ratio is 1:(2-8): the proportion of (5-10) adds potassium carbonate, sodium carbonate and sodium bicarbonate in DMF solvent
One or more of, using potassium iodide as catalyst, in 60-110 DEG C of condition under the inert gas shieldings such as nitrogen or argon gas
Then lower reaction 20-30 hours is filtered, is washed at least 5 times, then is dried in vacuo 24 hours or more under the conditions of 80-100 DEG C, most
It is ground into the powder that partial size is 10-100nm afterwards.
In a specific embodiment, modifying agent used in modified white carbon black is gamma-mercaptopropyltriethoxysilane, according to heavy
Shallow lake method, white carbon black: gamma-mercaptopropyltriethoxysilane mass ratio is the proportion of 5:1-12:1, in DMF solvent, in 80-120
DEG C condition is reacted 22-24 hour, is then filtered, is washed at least 5 times, then vacuum drying 48 hours under normal temperature conditions, is finally ground
Wear into the powder that partial size is 10-110nm.
In a specific embodiment, compounded curing system mainly includes that cumyl peroxide, Sulfur, triallyl are different
Cyanurate, N, penylene polymaleimide, N between N'-, N, N- vulcanize four isobutyl group thiurams, curing dicaprolactam.Its
Middle sulphur 0.2-0.5 parts, it can get good fatigue life；0.5-0.9 parts of penylene polymaleimide, molecule between N, N'-
Polyfunctional group on chain participates in Alder-ENE reaction, and the non-sulfur heteroatom cross-bond of the long-chain of formation increases tensile property, reduces
Glass transition temperature improves cryogenic property.In following Examples 1 to 5, addition cumyl peroxide, Sulfur and
Penylene polymaleimide between N, N'-, three's mass ratio are (1.2~2.5): (0.2~0.5): (0.5~0.9).
Titanium dioxide used in following Examples 1 to 5 is rutile-type.If it is necessary, can be in rubber windshield material of the invention
Various auxiliary agents are added in material, such as processing aid, anti-aging agent.
The preparation method of the rubber windshield material of one specific embodiment includes first adding in proportion in open mill
Enter raw rubber (EPDM, trielement ethyl butyric rubber, Liquid Ethylene Propylene Methylene and maleic anhydride modified polybutadiene), is mixed at 50-80 DEG C
It is 1-2 minutes, then thin to pass to 3 times less, after mixing, it is compound that the amine salt modification being pre-mixed is added at 125-140 DEG C
Fire retardant is kneaded 3-5 minutes；Modified white carbon black is added to continue to be kneaded 2-5 minutes at 140-150 DEG C；Then it sequentially adds
Low temperature resistant plasticizer and the auxiliary agent needed for other, are cooled to 80 DEG C or less addition compounded curing systems after mixing, bottom sheet,
And natural cooling.After parking 16 hours, by 150-170 DEG C of curing temperature, sulfide stress is controlled in 15-25MPa, vulcanization time control
System was at 40-80 minutes, rubber windshield product needed for being made.
Embodiment 1
The each component and quality of the light-colour rubber windshield material of the flame-proof environmental protection of the present embodiment low temperature resistant high rebound long-life
Number are as follows: ethylene propylene diene rubber, 75 parts；Trielement ethyl butyric rubber, 25 parts；Liquid Ethylene Propylene Methylene, 8 parts；Maleic anhydride modified poly- fourth
Diene (commercially available), 8 parts；Zinc oxide, 5 parts；Stearic acid, 1 part；Modified white carbon black, 20 parts；Amine salt modified compound fire retardant, 35 parts；
Cumyl peroxide, 1.5 parts；Sulfur, 0.3 part；Penylene polymaleimide between N, N'-, 0.7 part；Triallyl isocyanide urea
Acid esters, 0.9 part；N, N, N- four isobutyl group thiurams of vulcanization, 0.9 part；Titanium dioxide, 10 parts, trioctyl phosphate, 4 parts；Adipic acid two
Monooctyl ester, 3 parts.
Preparation process are as follows: it is first proportionally added into raw rubber in open mill, is mixed at 60 DEG C 1.5 minutes, it is then thin by logical 4
It is secondary, after mixing, amine salt modified compound fire retardant is added under the conditions of 130 DEG C, is kneaded 3.5 minutes；Then it is white that modification is added
Carbon black continues to be kneaded 3 minutes at 145 DEG C；Low temperature plasticizer and other auxiliary agents are subsequently added into, are cooled to 80 DEG C after mixing
Compounded curing system, bottom sheet, and natural cooling are added below.After parking 16 hours, by 160 DEG C of curing temperature, sulfide stress control
In 20MPa, vulcanization time was controlled at 55 minutes system, rubber windshield product needed for being made.
Comparative example 1
Raw rubber in embodiment 1 is changed to 100 parts of ethylene propylene diene rubber, zinc oxide, 5 parts；Stearic acid, 2 parts；Modified hard charcoal
It is black, 20 parts；Amine salt modified compound fire retardant, 35 parts；Cumyl peroxide, 1.4 parts；Sulfur, 0.2 part；Penylene is more between N, N'-
Maleimide, 0.7 part；Triallyl isocyanurate, 1.0 parts；Tetramethylthiuram disulfide, 1.0 parts, titanium dioxide, 10
Part, trioctyl phosphate, 4 parts；Dioctyl adipate, 3 parts.Preparation process is same as Example 1.
Embodiment 2
The each component and quality of the light-colour rubber windshield material of the flame-proof environmental protection of the present embodiment low temperature resistant high rebound long-life
Number are as follows: ethylene propylene diene rubber 60；Trielement ethyl butyric rubber, 40 parts；Liquid Ethylene Propylene Methylene, 10 parts；Maleic anhydride modified polybutadiene
Alkene, 6 parts；Zinc oxide, 5 parts；Stearic acid, 1 part；Modified white carbon black, 30 parts；Amine salt modified compound fire retardant, 42 parts；Tricresyl phosphate is pungent
Ester, 5 parts；Adipic acid dibutyl ester, 4 parts；Cumyl peroxide, 1.2 parts；Sulfur, 0.3 part；Penylene More Malay acyl is sub- between N, N'-
Amine, 0.6 part；Triallyl isocyanurate, 0.9 part；N, N, N- four isobutyl group thiurams of vulcanization, 0.75 part；Curing two oneself
Lactams, 0.5 part, titanium dioxide, 10 parts.
Preparation process are as follows: it is first proportionally added into raw rubber in open mill, is mixed at 60 DEG C 1.5 minutes, it is then thin by logical 5
It is secondary, after mixing, amine salt modified compound fire retardant is added under the conditions of 135 DEG C, is kneaded 2.5 minutes；Then it is white that modification is added
Carbon black continues to be kneaded 4 minutes at 140 DEG C；Low temperature plasticizer and other auxiliary agents are subsequently added into, are cooled to 80 DEG C after mixing
Compounded curing system, bottom sheet, and natural cooling are added below.After parking 16 hours, by 170 DEG C of curing temperature, sulfide stress control
In 22MPa, vulcanization time was controlled at 45 minutes system, rubber windshield product needed for being made.
Comparative example 2
By in embodiment 2 Liquid Ethylene Propylene Methylene and maleic anhydride modified polybutadiene removal, 5 parts of trioctyl phosphate and oneself
4 parts of diacid dibutyl ester replace with 9 parts of dioctyl phthalate, other compositions and dosage are consistent with embodiment 2.Prepare work
Skill is same as Example 2.
Embodiment 3
The each component and quality of the light-colour rubber windshield material of the flame-proof environmental protection of the present embodiment low temperature resistant high rebound long-life
Number are as follows: ethylene propylene diene rubber 50；Trielement ethyl butyric rubber, 50 parts；Liquid Ethylene Propylene Methylene, 12 parts；Maleic anhydride modified polybutadiene
Alkene, 6 parts；Zinc oxide, 5 parts；Stearic acid, 1 part；Modified white carbon black, 25 parts；Amine salt modified compound fire retardant, 49 parts；Tricresyl phosphate is pungent
Ester, 5 parts；Adipic acid dibutyl ester, 4 parts；Cumyl peroxide, 2.5 parts；Sulfur, 0.4 part；Penylene More Malay acyl is sub- between N, N'-
Amine, 0.6 part；Triallyl isocyanurate, 0.6 part；N, N, N- four isobutyl group thiurams of vulcanization, 0.8 part；Curing two is in oneself
Amide, 0.4 part, titanium dioxide, 10 parts.
Preparation process are as follows: it is first proportionally added into raw rubber in open mill, is mixed at 60 DEG C 1.5 minutes, it is then thin by logical 4
It is secondary, after mixing, amine salt modified compound fire retardant is added under the conditions of 125 DEG C, is kneaded 3.5 minutes；Then it is white that modification is added
Carbon black continues to be kneaded 3 minutes at 150 DEG C；Low temperature plasticizer and other auxiliary agents are subsequently added into, are cooled to 80 DEG C after mixing
Compounded curing system, bottom sheet, and natural cooling are added below.After parking 16 hours, by 150 DEG C of curing temperature, sulfide stress control
In 20MPa, vulcanization time was controlled at 80 minutes system, rubber windshield product needed for being made.
Comparative example 3
Compounded curing system in embodiment 3 is replaced with into cumyl peroxide, 2.2 parts；Triallyl isocyanuric acid
Ester, 1.0 parts；Tetramethylthiuram disulfide, 0.8 part, other compositions and dosage are consistent with embodiment 3.Preparation process with
Embodiment 3 is identical.
Embodiment 4
The each component and mass fraction of the light-colour rubber windshield material of the flame-proof environmental protection of the low temperature resistant high rebound of the present embodiment are as follows:
Ethylene propylene diene rubber 40；Trielement ethyl butyric rubber, 60 parts；Liquid Ethylene Propylene Methylene, 12 parts；Maleic anhydride modified polybutadiene, 8 parts；
Zinc oxide, 5 parts；Stearic acid, 1 part；Modified white carbon black, 30 parts；Amine salt modified compound fire retardant, 56 parts；Trioctyl phosphate, 6 parts；
Adipic acid dibutyl ester, 4 parts；Cumyl peroxide, 1.5 parts；Sulfur, 0.4 part；Penylene polymaleimide between N, N'-, 0.6
Part；Triallyl isocyanurate, 0.6 part；N, N, N- four isobutyl group thiurams of vulcanization, 0.8 part；Curing dicaprolactam,
0.4 part, titanium dioxide, 10 parts.
Preparation process are as follows: it is first proportionally added into raw rubber in open mill, is mixed at 60 DEG C 1.5 minutes, it is then thin by logical 4
It is secondary, after mixing, amine salt modified compound fire retardant is added under the conditions of 140 DEG C, is kneaded 2 minutes；Then modified hard charcoal is added
It is black to continue to be kneaded 4 minutes at 140 DEG C；Be subsequently added into low temperature plasticizer and other auxiliary agents, be cooled to after mixing 80 DEG C with
Lower addition compounded curing system, bottom sheet, and natural cooling.After parking 16 hours, by 155 DEG C of curing temperature, sulfide stress is controlled
In 25MPa, vulcanization time was controlled at 75 minutes, rubber windshield product needed for being made.
Comparative example 4
Modified white carbon black equivalent in embodiment 4 is replaced with into ordinary precipitation process white carbon black, other compositions and dosage and reality
Example 4 is applied to be consistent.Preparation process is same as Example 4.
Embodiment 5
The each component and mass fraction of the light-colour rubber windshield material of the flame-proof environmental protection of the low temperature resistant high rebound of the present embodiment are as follows:
Ethylene propylene diene rubber 50；Trielement ethyl butyric rubber, 50 parts；Liquid Ethylene Propylene Methylene, 12 parts；Maleic anhydride modified polybutadiene, 8 parts；
Zinc oxide, 5 parts；Stearic acid, 1 part；Modified white carbon black, 35 parts；Amine salt modified compound fire retardant, 28 parts；Trioctyl phosphate, 8 parts；
Adipic acid dibutyl ester, 5 parts；Cumyl peroxide, 1.6 parts；Sulfur, 0.3 part；Penylene polymaleimide between N, N'-, 0.8
Part；Triallyl isocyanurate, 0.5 part；N, N, N- four isobutyl group thiurams of vulcanization, 0.5 part；Curing dicaprolactam,
0.6 part, titanium dioxide, 10 parts.
Preparation process are as follows: it is first proportionally added into raw rubber in open mill, is mixed at 60 DEG C 1.5 minutes, it is then thin by logical 4
It is secondary, after mixing, amine salt modified compound fire retardant is added under the conditions of 140 DEG C, is kneaded 2 minutes；Then modified hard charcoal is added
It is black to continue to be kneaded 4 minutes at 140 DEG C；Be subsequently added into low temperature plasticizer and other auxiliary agents, be cooled to after mixing 80 DEG C with
Lower addition compounded curing system, bottom sheet, and natural cooling.After parking 16 hours, by 155 DEG C of curing temperature, sulfide stress is controlled
In 25MPa, vulcanization time was controlled at 75 minutes, rubber windshield product needed for being made.
Comparative example 5
Amine salt modified compound fire retardant in embodiment 5 replaces with to the aluminium hydroxide of equivalent, other compositions and dosage with
Embodiment 5 is consistent, and calendering process is different from embodiment 5.
Preparation process are as follows: it is first proportionally added into raw rubber in open mill, is mixed at 60 DEG C 1.5 minutes, it is then thin by logical 4
It is secondary, after mixing, modified white carbon black is added under the conditions of 140 DEG C, fire retardant is kneaded 4 minutes；It is subsequently added into low temperature plasticizer
And other auxiliary agents, it is cooled to 80 DEG C or less addition compounded curing systems, bottom sheet, and natural cooling after mixing.It is small to park 16
Shi Hou, by 150 DEG C of curing temperature, sulfide stress control is in 15MPa, and vulcanization time was controlled at 80 minutes, rubber wind needed for being made
Keep off product.
The detection performance parameter that above embodiments and comparative example correspond to outer hood rubber material is as follows:
Note: 1. cold snap-backs test (product technology requirement): the upper left or upper right outer hood for 1. intercepting 200mm length produce
Product exemplar is tested elemental height H1, is then placed 2 hours or more under -40 DEG C of environment；2. tooling is used, by the glue of outer hood
Bag pressure contracting 140mm (calculates decrement according to curve displacement), keeps subzero 40 DEG C of environment, maintains 30 minutes；3. exemplar is taken out,
Restore normal temperature environment, the height H2 after test product is restored after five minutes；Cold snap-back=H2/H1 × %.
At 23 DEG C as Lmm extend to kilocycle number needed for L+2mm, at 23 DEG C as L+2mm extend to kilocycle number needed for L+6mm ,-
It is extended at kilocycle number needed for L+2mm and -25 DEG C at 25 DEG C as Lmm and kilocycle number needed for L+6mm this four is extended to as L+2mm
The crack growth of the resistance to flexion performance of corner characterization sizing material.
The low temperature resistant high rebound long-life environmental protection light-colour rubber material that the present invention uses, cryogenic property, mechanical property, environmental protection
Performance can reach the technical requirements of rubber windshield, especially compared with comparative example, glass transition temperature, it is low temperature resistant rebound,
The crack growth of resistance to flexion performance under tensile strength, room temperature and cryogenic conditions etc. has a clear superiority, and environmental-protecting performance meets TB/T
3139, Q-CRRC J 26-2018 " railway transportation equipment product disabling and regulated substance " and EU REACH Legislation requirement, it is fire-retardant
Meet DIN5510-2 requirement.
Above-mentioned only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form.Therefore, it is all not
Be detached from technical solution of the present invention content, according to the present invention technical spirit it is made to the above embodiment it is any it is simple modification, etc.
With variation and modification, all shall fall within the protection scope of the technical scheme of the invention.
Claims (10)
1. a kind of low temperature resistant high elastic rubber windshield material, which is characterized in that be made of following components by weight:
40-75 parts of ethylene propylene diene rubber；
25-60 parts of trielement ethyl butyric rubber；
8-12 parts of Liquid Ethylene Propylene Methylene；
Maleic anhydride modified polybutadiene 5-8 parts；
The ethylene propylene diene rubber and totally 100 parts of the trielement ethyl butyric rubber.
2. low temperature resistant high elastic rubber windshield material according to claim 1, which is characterized in that the ethylene propylene diene rubber
Select the raw rubber of ethylene contents 40-50%, ENB content >=8%.
3. low temperature resistant high elastic rubber windshield material according to claim 1 or 2, which is characterized in that further include in component
Low temperature resistant plasticizer 5-15 parts, the low temperature resistant plasticizer is the mixture of trioctyl phosphate and adipic acid dibutyl ester.
4. low temperature resistant high elastic rubber windshield material according to claim 3, which is characterized in that further include amine salt in component
21-56 parts of modified compound fire retardant.
5. low temperature resistant high elastic rubber windshield material according to claim 4, which is characterized in that the amine salt modification is compound
Fire retardant includes Polyhedral oligomeric silsesquioxane, diethyl hypo-aluminum orthophosphate and melamine polyphosphate.
6. low temperature resistant high elastic rubber windshield material according to claim 4 or 5, which is characterized in that further include in component
20-35 parts of white carbon black of gamma-mercaptopropyltriethoxysilane modification.
7. low temperature resistant high elastic rubber windshield material according to claim 6, which is characterized in that further include compound in component
4-6 parts of vulcanizing system, the compounded curing system includes cumyl peroxide, Sulfur and N, penylene More Malay acyl between N'-
Imines.
8. low temperature resistant high elastic rubber windshield material according to claim 7, which is characterized in that the compounded curing system
Further include Triallyl isocyanurate, N, N, N- vulcanize one of four isobutyl group thiurams or curing dicaprolactam or
Any combination.
9. a kind of preparation method of the low temperature resistant high elastic rubber windshield material of claim 7 or 8 characterized by comprising
Ethylene propylene diene rubber, trielement ethyl butyric rubber, Liquid Ethylene Propylene Methylene and maleic anhydride modified polybutadiene are mixed at 50-80 DEG C
Uniformly；Then amine salt modified compound fire retardant is added at 125-140 DEG C to be kneaded；Modified white carbon black is added in 140-
Continue to be kneaded at 150 DEG C；It is subsequently added into low temperature resistant plasticizer, is cooled to 80 DEG C or less addition composite sulfuration bodies after mixing
System；Vulcanization is finally carried out to be made.
10. a kind of windscreen, which is characterized in that using any low temperature resistant high elastic rubber windscreen material of claim 1~8
Material.
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| CN201910846760.7A CN110527200B (en) | 2019-09-09 | 2019-09-09 | Low-temperature-resistant high-resilience rubber windshield material, preparation method thereof and windshield |
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| CN201910846760.7A CN110527200B (en) | 2019-09-09 | 2019-09-09 | Low-temperature-resistant high-resilience rubber windshield material, preparation method thereof and windshield |
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| CN110527200B CN110527200B (en) | 2022-01-25 |
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| CN114395196A (en) * | 2021-12-30 | 2022-04-26 | 际华三五一七橡胶制品有限公司 | Low-temperature-resistant ethylene propylene diene monomer sealing element and preparation method thereof |
| CN115461397A (en) * | 2020-09-30 | 2022-12-09 | 住友理工株式会社 | Flame-retardant rubber composition and outer windshield for railway vehicle |
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| CN110527200B (en) | 2022-01-25 |
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