CN108546364A - A kind of cold-resistant low compression set rubber composition and preparation method thereof - Google Patents
A kind of cold-resistant low compression set rubber composition and preparation method thereof Download PDFInfo
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The present invention provides a kind of cold-resistant low compression set rubber composition, it counts in parts by weight, the raw material of the composition includes 100 parts of ethylene propylene diene rubber, 3 10 parts of zinc oxide, 90 130 parts of carbon black, 30 40 parts of hydrowax oil, 10 20 parts of dibutyl sebacate, 0.5 1.5 parts of cumyl peroxide, N, 13 parts of 0.5 1.5 parts of the double furfurylidene-acetones of N ' and antioxidant MB, 13 parts of graphite；The present invention is using ethylene propylene diene rubber as basis material, using carbon black as reinforcing agent, using hydrowax oil and dibutyl sebacate as plasticizer, with cumyl peroxide and N, the double furfurylidene-acetones of N ' are vulcanizing agent, prepare the rubber composition for rubber damper or gasket.The rubber composition has excellent cold tolerance, ageing-resistant performance and low compression set.
Description
Technical field
The invention belongs to rubber materials, and in particular to one kind having excellent cold tolerance, ageing-resistant performance and low pressure contracting forever
Rubber composition deformed long and preparation method thereof.
Background technology
The long-term low temperature in Qinghai-Tibet Platean, ultraviolet light irradiation is strong, since geothermal energy resources are abundant, sulfur dioxide content in air compared with
It is high so that ethylene propylene diene rubber becomes the best glue kind that various rubber dampers are used on Qinghai-Tibet Plateau Railway line.EPDM
Rubber is copolymerized by three kinds of ethylene, propylene and non-conjugated diene monomers.Ethylene propylene diene rubber has excellent resilience performance, resistance to
Ozone performance, high and low temperature resistance, weatherability, ageing-resistant performance and chemical resistance.
The sulfur cross-linking ethylene propylene diene rubber group that Chinese patent CN107189236A discloses a kind of heat-proof aging, low pressure becomes
Close object, preparation method, purposes and its application product.The composition is vulcanized using sulphur, and sulfur cross-linking system has pressure
The defect of compression permanent deformation, product only focus on heat resistance, are not concerned with cryogenic property.
Chinese patent CN201710172665.4 discloses a kind of resistance to heat low and becomes rubber and preparation method thereof, the composition
Used filler is clay, the strong powder of magnesium and carbon black, and carbon black ratio is less than 50%.And pure carbon composition is compared, it is inorganic non-
The permanent performance of compression of metal packing is poor.It is EPDM 3092E, the raw rubber ethylene of the trade mark that the raw rubber used is done in the invention
Content is more than 60%, and cryogenic property is not good enough；Its product only focuses on heat resistance, is not concerned with cryogenic property.
Chinese patent CN201010570618.3 discloses a kind of EPT rubber composition, and the composition filler is charcoal
Black and tripoli compares pure carbon composition, and the permanent performance of compression of inorganic non-metallic filler is poor, is made in the inventive composition
There is no zinc oxide in raw material and has used magnesia.Its product only focuses on heat resistance, is not concerned with cryogenic property.
Invention content
In view of the above problems, the object of the present invention is to provide a kind of for railway line cushion blocking or rolling stock gasket
Rubber composition, the present invention is using ethylene propylene diene rubber as basis material, using carbon black as reinforcing agent, with hydrowax oil and decanedioic acid
Dibutyl ester is plasticizer, and with cumyl peroxide and N, the bis- furfurylidene-acetones of N '-are vulcanizing agent, prepare and are used for rubber damper
Rubber composition.The rubber composition has excellent cold tolerance, ageing-resistant performance and low compression set.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention provides a kind of rubber composition, the raw material of the rubber composition include ethylene propylene diene rubber, zinc oxide,
Carbon black, hydrowax oil, dibutyl sebacate, cumyl peroxide, N, the bis- furfurylidene-acetones of N '-, antioxidant MB and ultra-fine
Graphite.
Preferably, it counts in parts by weight, the raw material of the composition includes 100 parts of ethylene propylene diene rubber, zinc oxide 3-10
Part, 90-130 parts of carbon black, 30-40 parts of hydrowax oil, 10-20 parts of dibutyl sebacate, cumyl peroxide 0.5-1.5
1-3 parts of part, 1-3 parts of superfine graphite, N, bis- furfurylidene-acetone 0.5-1.5 parts of N '-and antioxidant MB；
Preferably, count in parts by weight, the raw material of the composition include 100 parts of ethylene propylene diene rubber, 5 parts of zinc oxide,
110 parts of carbon black, 35 parts of hydrowax oil, 15 parts of dibutyl sebacate, 1 part of cumyl peroxide, 2 parts of superfine graphite, N, N '-
2 parts of 1 part of double furfurylidene-acetones and antioxidant MB；
Preferably, in the ethylene propylene diene rubber, ethylene contents 45-51%, Mooney viscosity ML (1+4) 125 DEG C >=70,
ENB contents ＞ 6%；
Preferably, the carbon black is carbon black N550 and/or carbon black N660；It is preferred that carbon black N550.
Preferably, the raw material of the composition is by ethylene propylene diene rubber, zinc oxide, carbon black, hydrowax oil, decanedioic acid two
Butyl ester, cumyl peroxide, N, the bis- furfurylidene-acetones of N '-, antioxidant MB and superfine graphite composition；
Preferably, count in parts by weight, the raw material of the composition by 100 parts of ethylene propylene diene rubber, 3-10 parts of zinc oxide,
90-130 parts of carbon black, 10-20 parts of dibutyl sebacate, 0.5-1.5 parts of cumyl peroxide, surpasses 30-40 parts of hydrowax oil
1-3 parts of fine graphite, N, 1-3 parts of compositions of bis- furfurylidene-acetone 0.5-1.5 parts of N '-and antioxidant MB；
Preferably, it counts in parts by weight, the raw material of the composition is by 100 parts of ethylene propylene diene rubber, 5 parts of zinc oxide, charcoal
Black 110 parts, 35 parts of hydrowax oil, 15 parts of dibutyl sebacate, 1 part of cumyl peroxide, 2 parts of superfine graphite, N, N '-is bis-
2 parts of compositions of 1 part of furfurylidene-acetone and antioxidant MB.
The present invention also provides a kind of preparation methods of rubber composition of the present invention, and the preparation method includes following
Step：Each raw material of the rubber composition is mixed in proportion；
Preferably, each raw material of the rubber composition is kneaded in mixer in proportion；
Preferably, the mixing speed is 40r/min；Preferably, the mixing time is 4-6min.
The present invention also provides rubber compositions of the present invention in preparing rubber damper or rolling stock gasket
Purposes.
Rubber composition main performance index of the present invention is as follows：Hardness 55 ± 5, tensile strength ＞ 16.0MPa, elongation
Rate ＞ 350%, (150 DEG C, for 24 hours, compress 25%) ＜ 30% for compression set.After 150 DEG C of * 72h hot air agings, stretch strong
Spend conservation rate ＞ 90%, elongation at break conservation rate ＞ 80%, the compression at ＜ -60 DEG C, -40 DEG C of brittleness temperature is resisted cold coefficient ＞
0.2；No cracking after resistance to ozone aging, ozone concentration are (100 ± 20) × 10-8Volume fraction, extensibility are 30 ± 2%, temperature
Degree is 40 DEG C ± 2 DEG C, exposure duration 96h.
Compared with prior art, the present invention has at least following advantageous effect：
1, rubber composition low temperature performance well of the present invention, constantly, resist cold -60 DEG C of brittleness temperature coefficient ＞ at -40 DEG C
0.2。
The present invention ensure that superior cryogenic property from the following aspect.
First, on to raw material ethylene propylene diene rubber selection, the ethylene contents control in the ethylene propylene diene rubber exists
48 ± 3%.Comparative example in following article table is as it can be seen that will make composition have excellent cryogenic property.Also, raw material three of the present invention
ENB contents in first EP rubbers are more than 6%, and the ENB contents of ethylene propylene diene rubber are higher, then are more conducive to be crosslinked, to low
The improvement of warm elasticity is more advantageous.
Second, use in rubber composition of the present invention cumyl peroxide and N, the bis- furfurylidene-acetones of N '-to carry out
Vulcanization also ensures cryogenic property.
Third, in the plasticizer selection in composition of the present invention, simultaneously using hydrowax oil and dibutyl sebacate
With composition can be made to obtain excellent cryogenic property, the especially higher cold-resistant coefficient of compression.If only using hydrowax
Oil, then the cold-resistant coefficient of the low temperature of the rubber composition cannot be satisfied the requirement of ＞ 0.2, and use hydrowax oil and the last of the ten Heavenly stems simultaneously
Adipate can improve the cold-resistant coefficient of compression of the rubber composition；Wherein, the dibutyl sebacate is as polarity
Plasticizer, the dosage in preparing the rubber composition are restricted, excessively few not have the due effect for improving low temperature then
Fruit crosses and is at most easy to be precipitated.
2, the compression set of rubber composition of the present invention is small, 150 DEG C of ＜ 30% under the conditions of * 24 hours.
First, to the raw material ethylene propylene diene rubber selection on, the ethylene contents in ethylene propylene diene rubber it is excessively high or
Too low, then the crystallization tendency of ethylene propylene diene rubber is just apparent, and plasticity increases, poor performance at low temperatures.
Secondly, the reinforcing agent in the raw material of rubber composition of the present invention selects carbon black to do filler, without using hard charcoal
The inorganic fillers such as black, clay, talcum powder, mica, tripoli, fine particle calcium carbonate.It is well known that due to the reason of surface nature, the pressure of carbon black
Compression permanent deformation is significantly less than inorganic filler.
Peroxide and N, the bis- furfurylidene-acetones of N '-is used to vulcanize in rubber composition of the present invention, cross-bond is heat-resisting
Property is good, then the compression set of product is significantly excellent.
Plasticizer in rubber composition of the present invention is oily using hydrowax, rather than common high-flash paraffin
Oil interferes vulcanization to avoid the unsaturated ingredient in paraffin oil, influences compression set performance.
In rubber composition of the present invention do not use stearic acid or zinc stearate, antioxidant 4010,4010NA or
4020 etc..
3, the intensity of rubber composition of the present invention and elongation are big, and intensity is more than 16MPa, and elongation is more than 350%；
On to raw material ethylene propylene diene rubber selection, the ethylene propylene diene rubber of high Mooney, Mooney viscosity ML have been selected
125 DEG C of (1+4) is more than or equal to 70.And Mooney is higher, then strand is longer, and molecular weight is bigger, and ethylene propylene diene rubber was stretching
Cheng Zhong, molecule intermediate node is more, therefore intensity and elongation are bigger.
4, the thermal aging property of rubber composition of the present invention is good, after 150 DEG C of * 72h hot air agings, stretches strong
Spend conservation rate ＞ 90%, elongation at break conservation rate ＞ 80%.Other than selecting ethylene propylene diene rubber itself, how to select
It is also most important to select vulcanizing agent.The present invention uses cumyl peroxide and N, the bis- furfurylidene-acetones of N '-to make vulcanizing agent, formation
Cross-bond thermal stability is high.
5, the ozone resistance of rubber composition of the present invention is good, in ozone concentration (100 ± 20) × 10-8 volumes point
Number, extensibility：30% ± 2%, temperature：40 DEG C ± 2 DEG C, exposure duration：96h, no cracking.
Specific implementation mode
The present invention is described below with reference to specific embodiments.It will be appreciated by those skilled in the art that these embodiments are only
For illustrating the present invention, do not limit the scope of the invention in any way.
The experimental method of following embodiments is unless otherwise specified conventional method.Original as used in the following examples
Material, reagent material etc. are commercially available products unless otherwise specified.
In following example 1-3 and comparative example 4-7, country's mark based on each measured performance parameter method
It is accurate specific as follows：Tensile strength, elongation at break are measured by GB/T 528；Hardness is measured by GB/T 531；Compression set
It is measured by GB/T7759.1, condition：150 DEG C, for 24 hours, compression 25%；Thermal aging property is measured by GB/T 3512, condition：
150 DEG C, 72h,；Brittleness temperature is measured by GB/T 1682；Ozone resistance is measured by GB/T 7762, ozone concentration：(100±
20) × 10-8 volume fractions, extensibility：30% ± 2%, temperature：40 DEG C ± 2 DEG C, exposure duration 96h；The cold-resistant coefficient of compression is pressed
HG/T 3866 is measured, -40 DEG C of test temperature.
Raw material：
Ethylene propylene diene rubber, 9550, Lang Sheng speciality chemical Co., Ltd products；
Carbon black, N550, Cabot Co., Ltd's product；
Hydrowax oil, dibutyl sebacate, Ningbo co evolution work Co., Ltd product；
Cumyl peroxide, Shanghai Gaoqiao petrochemical corporation (complex) product；
Science and Technology Ltd.'s product is contained in N, N '-bis- furfurylidene-acetones, Guangzhou Jinchang；
Other are commercially available industrial goods.
Rubber composition preparation method of the present invention：
Each raw material of the rubber composition is kneaded in mixer in proportion, the mixing speed is 40r/min, institute
It is 4-6min to state mixing time.
Each raw material composition of 1-3 of the embodiment of the present invention and comparative example 4-12 is shown in Table 1；
Table 1：Each raw material of 1-3 of the embodiment of the present invention and comparative example 4-12 forms
As seen from Table 1, the carbon black in comparative example 4,5, hydrowax oil, dibutyl sebacate, cumyl peroxide, N,
The selection of the component contents such as the bis- furfurylidene-acetones of N '-, graphite, obtained product compression set, intensity, resist cold coefficient
Deng the performances such as aging conservation rate are all poor；
Selection in comparative example 6,7 to Mooney, ethylene contents, obtained product resists cold coefficient can be poor.Such as second
Alkene too high levels, EP rubbers crystallization tendency is just apparent, then its plasticity increases, and cryogenic property is bad；Wherein, ethylene contents are excessively high
Ethylene propylene diene rubber, although high tensile strength can be obtained, the poor flexibility under low temperature；And the Gao Yi of peroxide cure
Although the ethylene propylene diene rubber brittleness temperature of alkene content can be more than -60 DEG C, it is without resilience at -40 DEG C, and resist cold coefficient
Value is very low；
Clay, intensity, compression set rate, ageing properties and the cold-resistant system of obtained product are used in comparative example 8
Number is all poor；
Common paraffin oil, the cold-resistant coefficient of compression and compression set ratio of obtained product are used in comparative example 9
It is poor；
Sulfur cross-linking system, compression set rate, the hot air aging of obtained product are used in comparative example 10
The coefficient that resists cold can, be compressed significantly to be deteriorated；And the EP rubbers of sulfur cross-linking, black brittleness do not cross -55 DEG C；
N, the bis- furfurylidene-acetones of N '-is not used to work as assistant crosslinking agent in comparative example 11, the compression of obtained product permanently becomes
Coefficient is resisted cold in form quotient, intensity, thermal aging property and compression can be poor；
4010NA is used in comparative example 12, interferes peroxide cure, the intensity of obtained product, compression set
Coefficient is resisted cold in rate, ageing properties and compression all can be poor.
In short, specific description of embodiments of the present invention above is not intended to limit the present invention, those skilled in the art can be with
It is variously modified or is deformed according to the present invention, without departing from the spirit of the present invention, right appended by the present invention should all belonged to and wanted
The range asked.
Claims (5)
1. a kind of cold-resistant low compression set rubber composition, the raw material of the rubber composition include ethylene propylene diene rubber,
Zinc oxide, superfine carbon black, hydrowax oil, dibutyl sebacate, cumyl peroxide, N, the bis- furfurylidene-acetones of N '-are prevented always
Agent MB and graphite.
2. rubber composition according to claim 1, which is characterized in that count in parts by weight, the raw material of the composition
Including 100 parts of ethylene propylene diene rubber, 3-10 parts of zinc oxide, 90-130 parts of superfine carbon black, 30-40 parts of hydrowax oil, decanedioic acid
10-20 parts of dibutyl ester, 0.5-1.5 parts of cumyl peroxide, 1-3 parts of superfine graphite, N, the bis- furfurylidene-acetone 0.5-1.5 of N '-
1-3 parts of part and antioxidant MB；
Preferably, it counts in parts by weight, the raw material of the composition includes 100 parts of ethylene propylene diene rubber, 5 parts of zinc oxide, ultra-fine
110 parts of carbon black, 35 parts of hydrowax oil, 15 parts of dibutyl sebacate, 1 part of cumyl peroxide, 2 parts of superfine graphite, N, N '-
2 parts of 1 part of double furfurylidene-acetones and antioxidant MB；
Preferably, in the ethylene propylene diene rubber, ethylene contents 45-51%, Mooney viscosity ML (1+4) 125 DEG C >=70, ENB
Content ＞ 6%；
Preferably, the carbon black is carbon black N550 and/or carbon black N660；It is preferred that carbon black N550.
3. rubber composition according to claim 1 or 2, which is characterized in that the raw material of the composition is by EPDM
Rubber, zinc oxide, superfine carbon black, hydrowax oil, dibutyl sebacate, cumyl peroxide, N, the bis- furfurylidenes of N '-third
Ketone, antioxidant MB and graphite composition；
Preferably, it counts in parts by weight, the raw material of the composition is by 100 parts of ethylene propylene diene rubber, 3-10 parts of zinc oxide, carbon black
90-130 parts, 30-40 parts of hydrowax oil, 10-20 parts of dibutyl sebacate, 0.5-1.5 parts of cumyl peroxide, ultra-fine stone
Bis- furfurylidene-acetone 0.5-1.5 parts of 1-3 parts black, N, N '-and 1-3 parts of compositions of antioxidant MB；
Preferably, it counts in parts by weight, the raw material of the composition is by 100 parts of ethylene propylene diene rubber, 5 parts of zinc oxide, ultrafine carbon
Black 110 parts, 35 parts of hydrowax oil, 15 parts of dibutyl sebacate, 1 part of cumyl peroxide, 2 parts of graphite, N, the bis- sub- chaffs of N '-
2 parts of compositions of 1 part of benzylacetone and antioxidant MB.
4. a kind of preparation method of rubber composition as claimed any one in claims 1 to 3, the preparation method include with
Lower step：Each raw material of the rubber composition is mixed in proportion；
Preferably, each raw material of the rubber composition is kneaded in mixer in proportion；
Preferably, the mixing speed is 40r/min；Preferably, the mixing time is 4-6min.
5. cold-resistant low compression set rubber composition is preparing rubber damping as claimed any one in claims 1 to 3
Purposes in pad or rolling stock gasket.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204838A (en) * | 2019-06-20 | 2019-09-06 | 宁国市正道橡塑零部件有限公司 | A kind of high rigidity low compression set ethylene propylene diene rubber and preparation method thereof |
| CN111607165A (en) * | 2020-06-24 | 2020-09-01 | 长缆电工科技股份有限公司 | High-expansion insulating ethylene-propylene rubber cold-contraction material, and preparation method and application thereof |
| CN111732791A (en) * | 2020-07-07 | 2020-10-02 | 博戈橡胶塑料（株洲）有限公司 | Ethylene propylene diene monomer material and preparation method and application thereof |
| CN112592542A (en) * | 2020-12-28 | 2021-04-02 | 苏州国泰科技发展有限公司 | Novel rubber environment-friendly material |
| CN113861572A (en) * | 2021-10-18 | 2021-12-31 | 上安实业江苏有限公司 | Low-temperature-resistant water stop rubber material and preparation method thereof |
| CN114044986A (en) * | 2021-12-25 | 2022-02-15 | 常州坚正橡塑制品有限公司 | Low-temperature-resistant rubber, preparation method thereof and air spring end cover applying low-temperature-resistant rubber |
| CN114292454A (en) * | 2021-12-30 | 2022-04-08 | 铁科纵横（天津）科技发展有限公司 | Rubber floor material raw material composition, rubber floor material and preparation method thereof |
| CN115505216A (en) * | 2022-11-01 | 2022-12-23 | 国网新疆电力有限公司电力科学研究院 | Preparation method of cold-resistant ethylene propylene diene monomer sealing material for GIS equipment |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110204838A (en) * | 2019-06-20 | 2019-09-06 | 宁国市正道橡塑零部件有限公司 | A kind of high rigidity low compression set ethylene propylene diene rubber and preparation method thereof |
| CN111607165A (en) * | 2020-06-24 | 2020-09-01 | 长缆电工科技股份有限公司 | High-expansion insulating ethylene-propylene rubber cold-contraction material, and preparation method and application thereof |
| CN111732791A (en) * | 2020-07-07 | 2020-10-02 | 博戈橡胶塑料（株洲）有限公司 | Ethylene propylene diene monomer material and preparation method and application thereof |
| CN112592542A (en) * | 2020-12-28 | 2021-04-02 | 苏州国泰科技发展有限公司 | Novel rubber environment-friendly material |
| CN113861572A (en) * | 2021-10-18 | 2021-12-31 | 上安实业江苏有限公司 | Low-temperature-resistant water stop rubber material and preparation method thereof |
| CN114044986A (en) * | 2021-12-25 | 2022-02-15 | 常州坚正橡塑制品有限公司 | Low-temperature-resistant rubber, preparation method thereof and air spring end cover applying low-temperature-resistant rubber |
| CN114292454A (en) * | 2021-12-30 | 2022-04-08 | 铁科纵横（天津）科技发展有限公司 | Rubber floor material raw material composition, rubber floor material and preparation method thereof |
| CN114292454B (en) * | 2021-12-30 | 2023-10-03 | 铁科纵横（天津）科技发展有限公司 | Rubber flooring material raw material composition, rubber flooring material and preparation method thereof |
| CN115505216A (en) * | 2022-11-01 | 2022-12-23 | 国网新疆电力有限公司电力科学研究院 | Preparation method of cold-resistant ethylene propylene diene monomer sealing material for GIS equipment |
| CN115505216B (en) * | 2022-11-01 | 2023-08-29 | 国网新疆电力有限公司电力科学研究院 | Preparation method of cold-resistant ethylene propylene diene monomer rubber sealing material for GIS (gas insulated switchgear) equipment |
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