CN108546364B - Cold-resistant low-compression permanent deformation rubber composition and preparation method thereof - Google Patents
Cold-resistant low-compression permanent deformation rubber composition and preparation method thereof Download PDFInfo
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- CN108546364B CN108546364B CN201810165735.8A CN201810165735A CN108546364B CN 108546364 B CN108546364 B CN 108546364B CN 201810165735 A CN201810165735 A CN 201810165735A CN 108546364 B CN108546364 B CN 108546364B
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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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Abstract
The invention provides a cold-resistant low-compression permanent deformation rubber composition, which comprises the following raw materials, by weight, 100 parts of ethylene propylene diene monomer, 3-10 parts of zinc oxide, 90-130 parts of carbon black, 30-40 parts of hydrogenated paraffin oil, 10-20 parts of dibutyl sebacate, 0.5-1.5 parts of dicumyl peroxide, 0.5-1.5 parts of N, N' -difurfurylideneacetone, 1-3 parts of an anti-aging agent MB, and 1-3 parts of graphite; the invention takes ethylene propylene diene monomer as a base material, carbon black as a reinforcing agent, hydrogenated paraffin oil and dibutyl sebacate as plasticizers, and dicumyl peroxide and N, N' -bi-furfurylideneacetone as vulcanizing agents to prepare the rubber composition for the rubber damping pad or the sealing pad. The rubber composition has excellent cold resistance, aging resistance and low compression set.
Description
Technical Field
The invention belongs to the field of rubber, and particularly relates to a rubber composition with excellent cold resistance, aging resistance and low compression set and a preparation method thereof.
Background
The Qinghai-Tibet plateau is low in temperature all year round, the ultraviolet irradiation is strong, and due to the abundant geothermal resources and the high sulfur dioxide content in the air, the ethylene propylene diene monomer becomes the best rubber species for various rubber damping pads on the Qinghai-Tibet plateau railway line. The ethylene propylene diene monomer is prepared by copolymerizing ethylene, propylene and non-conjugated diene. The ethylene propylene diene monomer rubber has excellent resilience, ozone resistance, high and low temperature resistance, weather resistance, ageing resistance and chemical resistance.
Chinese patent CN107189236A discloses a sulfur-vulcanized ethylene propylene diene rubber composition with heat aging resistance and low pressure change, a preparation method, application and an application product thereof. The composition is vulcanized by adopting sulfur, a sulfur vulcanization system has the defect of compression permanent deformation, and the product only focuses on heat resistance and does not focus on low-temperature performance.
Chinese patent CN201710172665.4 discloses a heat-resistant low-pressure-change rubber and a preparation method thereof, wherein fillers adopted by the composition are argil, magnesium-reinforced powder and carbon black, and the proportion of the carbon black is less than 50%. Whereas the inorganic non-metallic fillers have poorer compression set properties than the pure carbon black compositions. The raw rubber used in the invention is EPDM 3092E, the ethylene content of the raw rubber of the grade is more than 60%, and the low-temperature performance is poor; the product only focuses on heat resistance and does not focus on low-temperature performance.
Chinese patent CN201010570618.3 discloses an ethylene propylene diene monomer composition, the filler of the composition is carbon black and silica, compared with a pure carbon black composition, the compression permanent property of an inorganic non-metallic filler is poorer, and the raw material used in the composition of the invention does not contain zinc oxide but uses magnesium oxide. The product only focuses on heat resistance and does not focus on low-temperature performance.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a rubber composition for a railway line damping pad or a locomotive car sealing pad, wherein the rubber composition for a rubber damping pad is prepared by using ethylene propylene diene monomer as a base material, carbon black as a reinforcing agent, hydrogenated paraffin oil and dibutyl sebacate as plasticizers, and dicumyl peroxide and N, N' -bi-furfurylideneacetone as vulcanizing agents. The rubber composition has excellent cold resistance, aging resistance and low compression set.
The purpose of the invention is realized by the following technical scheme:
the invention provides a rubber composition, and raw materials of the rubber composition comprise ethylene propylene diene monomer, zinc oxide, carbon black, hydrogenated paraffin oil, dibutyl sebacate, dicumyl peroxide, N' -bi-furfurylideneacetone, an anti-aging agent MB and ultrafine graphite.
Preferably, the raw materials of the composition comprise, by weight, 100 parts of ethylene propylene diene monomer, 3-10 parts of zinc oxide, 90-130 parts of carbon black, 30-40 parts of hydrogenated paraffin oil, 10-20 parts of dibutyl sebacate, 0.5-1.5 parts of dicumyl peroxide, 1-3 parts of ultrafine graphite, 0.5-1.5 parts of N, N' -difurfurylideneacetone and 1-3 parts of an anti-aging agent MB;
preferably, the raw materials of the composition comprise 100 parts by weight of ethylene propylene diene monomer, 5 parts by weight of zinc oxide, 110 parts by weight of carbon black, 35 parts by weight of hydrogenated paraffin oil, 15 parts by weight of dibutyl sebacate, 1 part by weight of dicumyl peroxide, 2 parts by weight of ultrafine graphite, 1 part by weight of N, N' -bi-furfurylideneacetone and 2 parts by weight of anti-aging agent MB;
preferably, in the ethylene propylene diene monomer, the ethylene content is 45-51%, the Mooney viscosity ML (1+4) is more than or equal to 70 at 125 ℃, and the ENB content is more than 6%;
preferably, the carbon black is carbon black N550 and/or carbon black N660; carbon black N550 is preferred.
Preferably, the raw materials of the composition consist of ethylene propylene diene monomer, zinc oxide, carbon black, hydrogenated paraffin oil, dibutyl sebacate, dicumyl peroxide, N' -difurfurylideneacetone, an anti-aging agent MB and ultrafine graphite;
preferably, the raw materials of the composition comprise, by weight, 100 parts of ethylene propylene diene monomer, 3-10 parts of zinc oxide, 90-130 parts of carbon black, 30-40 parts of hydrogenated paraffin oil, 10-20 parts of dibutyl sebacate, 0.5-1.5 parts of dicumyl peroxide, 1-3 parts of ultrafine graphite, 0.5-1.5 parts of N, N' -difurfurylideneacetone and 1-3 parts of an anti-aging agent MB;
preferably, the raw materials of the composition comprise, by weight, 100 parts of ethylene propylene diene monomer, 5 parts of zinc oxide, 110 parts of carbon black, 35 parts of hydrogenated paraffin oil, 15 parts of dibutyl sebacate, 1 part of dicumyl peroxide, 2 parts of ultrafine graphite, 1 part of N, N' -bi-furfurylideneacetone and 2 parts of anti-aging agent MB.
The invention also provides a preparation method of the rubber composition, which comprises the following steps: mixing the raw materials of the rubber composition in proportion;
preferably, the raw materials of the rubber composition are mixed in an internal mixer according to the proportion;
preferably, the mixing speed is 40 r/min; preferably, the mixing time is 4-6 min.
The invention also provides the use of the rubber composition of the invention in the preparation of rubber vibration damping mats or rolling stock gaskets.
The main performance indexes of the rubber composition are as follows: the hardness is 55 plus or minus 5, the tensile strength is more than 16.0MPa, the elongation is more than 350 percent, and the compression permanent deformation (150 ℃, 24 hours and 25 percent compression) is less than 30 percent. After the hot air aging at 150 ℃ for 72h, the tensile strength retention rate is more than 90 percent, the elongation at break retention rate is more than 80 percent, the brittleness temperature is lower than-60 ℃, and the compression cold-resistant coefficient at-40 ℃ is more than 0.2; the ozone aging resistance is no crack, and the ozone concentration is (100 +/-20) multiplied by 10-8The volume fraction, the stretching ratio is 30 +/-2%, the temperature is 40 +/-2 ℃, and the exposure time is 96 h.
Compared with the prior art, the invention has at least the following beneficial effects:
1. the rubber composition has good low-temperature performance, and the brittleness temperature is constant at minus 60 ℃, and the cold resistance coefficient is more than 0.2 at minus 40 ℃.
The present invention ensures superior low-temperature performance in the following respects.
Firstly, the ethylene content in the ethylene-propylene-diene monomer is controlled to be 48 +/-3% in the selection of the raw material ethylene-propylene-diene monomer. As can be seen in the comparative examples in the table below, this will result in compositions having excellent low temperature properties. In addition, the content of ENB in the raw material of the ethylene propylene diene monomer is more than 6 percent, and the higher the content of ENB in the ethylene propylene diene monomer is, the more favorable the crosslinking is, and the more favorable the improvement of low-temperature elasticity is.
Secondly, the low-temperature performance is also ensured by adopting dicumyl peroxide and N, N' -bi-furfurylideneacetone for vulcanization in the rubber composition.
Thirdly, the composition of the present invention has excellent low temperature performance, especially high cold resistance coefficient of compression, due to the selection of the plasticizer in combination with the hydrogenated paraffin oil and dibutyl sebacate. If only the hydrogenated paraffin oil is used, the low-temperature cold resistance coefficient of the rubber composition cannot meet the requirement of more than 0.2, and the compressed cold resistance coefficient of the rubber composition can be improved by simultaneously using the hydrogenated paraffin oil and dibutyl sebacate; among them, dibutyl sebacate is a polar plasticizer, and the amount thereof used in the preparation of the rubber composition is limited, and when it is too small, it does not exert the effect of improving the low temperature, and when it is too large, it is liable to precipitate.
2. The rubber composition of the invention has a small compression set, less than 30% at 150 ℃ for 24 hours.
Firstly, in the selection of the raw material ethylene propylene diene monomer, if the ethylene content in the ethylene propylene diene monomer is too high or too low, the crystallization tendency of the ethylene propylene diene monomer is obvious, the plasticity is increased, and the low-temperature performance is poor.
Secondly, the reinforcing agent in the raw materials of the rubber composition is carbon black as a filler, and inorganic fillers such as white carbon black, argil, talcum powder, mica, silica, light calcium carbonate and the like are not adopted. It is well known that carbon black has a significantly smaller compression set than inorganic fillers due to surface properties.
The rubber composition is vulcanized by adopting peroxide and N, N' -difurfurylidene acetone, the heat resistance of a cross-linking bond is good, and the compression set of the product is remarkably excellent.
The plasticizer in the rubber composition adopts hydrogenated paraffin oil instead of common high-flash-point paraffin oil so as to avoid the interference of unsaturated components in the paraffin oil with vulcanization and influence on the compression permanent deformation performance.
Stearic acid or zinc stearate, anti-aging agents 4010, 4010NA or 4020 and the like are not used in the rubber composition.
3. The rubber composition has high strength and elongation, the strength is more than 16MPa, and the elongation is more than 350 percent;
in the selection of the raw material ethylene propylene diene monomer, the ethylene propylene diene monomer with high Mooney is selected, and the Mooney viscosity ML (1+4) is more than or equal to 70 ℃ at 125 ℃. And the higher the Mooney, the longer the molecular chain and the larger the molecular weight, and the more intermolecular nodes are in the ethylene propylene diene monomer during the stretching process, so the strength and the elongation are higher.
4. The rubber composition has good hot air aging performance, and after hot air aging at 150 ℃ for 72 hours, the tensile strength retention rate is more than 90%, and the elongation at break retention rate is more than 80%. In addition to the choice of the ethylene propylene diene monomer itself, it is also important how the vulcanizing agent is selected. The invention adopts dicumyl peroxide and N, N' -difurfurylidene acetone as vulcanizing agents, and the formed cross-linked bond has high thermal stability.
5. The rubber composition has good ozone resistance, and the ozone concentration (100 +/-20) multiplied by 10-8 volume fraction, the tensile ratio: 30% ± 2%, temperature: 40 ℃. + -. 2 ℃, exposure time: 96h, no cracking.
Detailed Description
The invention is illustrated below with reference to specific examples. It will be understood by those skilled in the art that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention in any way.
The experimental procedures of the following examples are conventional unless otherwise specified. The raw materials and reagent materials used in the following examples are all commercially available products unless otherwise specified.
In the following examples 1 to 3 and comparative examples 4 to 7, the national standards according to which the respective performance parameters were determined were as follows: the tensile strength and the elongation at break are measured according to GB/T528; the hardness is measured according to GB/T531; compression set was determined according to GB/T7759.1, conditions: compressing at 150 deg.C for 24 hr for 25%; the hot air aging performance is determined according to GB/T3512, conditions: 150 ℃ for 72 h; the brittleness temperature is measured according to GB/T1682; ozone resistance was measured according to GB/T7762, and the concentration of ozone: (100. + -. 20). times.10-8 volume fraction, elongation: 30% ± 2%, temperature: the exposure time is 96 hours at the temperature of 40 +/-2 ℃; the cold resistance to compression is determined as HG/T3866 at-40 ℃.
Raw materials:
ethylene propylene diene monomer, 9550, product of langshi specialty chemicals limited;
carbon black, N550, product of cabot corporation;
hydrogenated paraffin oil, dibutyl sebacate, Ningbo Co., Ltd;
dicumyl peroxide, a product of Shanghai Gaoqiao petrochemical company;
n, N' -Bifurfurylideneacetone, a product of Kyokuoshan technologies, Inc., Guangzhou;
the others are commercial products.
The preparation method of the rubber composition comprises the following steps:
and mixing the raw materials of the rubber composition in an internal mixer in proportion, wherein the mixing speed is 40r/min, and the mixing time is 4-6 min.
The compositions of the respective raw materials of examples 1 to 3 of the present invention and comparative examples 4 to 12 are shown in Table 1;
table 1: the raw material compositions of examples 1 to 3 of the present invention and comparative examples 4 to 12
As can be seen from Table 1, the selection of the content of carbon black, hydrogenated paraffin oil, dibutyl sebacate, dicumyl peroxide, N' -bi-furfurylideneacetone, graphite, etc. in the comparative examples 4 and 5, the compression set, strength, cold resistance coefficient, etc. of the obtained product, aging retention rate, etc. are all poor;
the selection of Mooney and ethylene contents in comparative examples 6 and 7 resulted in products having a relatively poor cold resistance coefficient. For example, if the ethylene content is too high, the crystallization tendency of the ethylene propylene rubber is obvious, the plasticity is increased, and the low-temperature performance is not good; among them, ethylene propylene diene monomer rubber with too high ethylene content has poor low-temperature elasticity although high tensile strength can be obtained; while the brittleness temperature of the ethylene propylene diene monomer rubber with high ethylene content vulcanized by peroxide can exceed minus 60 ℃, the ethylene propylene diene monomer rubber has no resilience at minus 40 ℃ and has very low cold resistance coefficient value;
in comparative example 8, clay was used, and the obtained product was poor in strength, compression set, aging resistance and cold resistance coefficient;
in comparative example 9, the common paraffin oil was used, and the resulting product was inferior in cold resistance coefficient and compression set;
in the comparative example 10, a sulfur vulcanization system was used, and the compression set rate, hot air aging property, and compression cold resistance coefficient of the obtained product were significantly deteriorated; the low-temperature brittleness of the sulfur-vulcanized ethylene propylene rubber is less than minus 55 ℃;
in comparative example 11, N' -difurfurylideneacetone was not used as an auxiliary crosslinking agent, and the resulting product would have poor compression set, strength, hot air aging properties, and compression cold resistance coefficient;
comparative example 12, in which 4010NA was used, interfered with peroxide vulcanization, resulted in a product having poor strength, compression set, aging properties and compression cold resistance coefficient.
In conclusion, the above description of the embodiments of the present invention is not intended to limit the present invention, and those skilled in the art can make various changes or modifications according to the present invention without departing from the spirit of the present invention, which falls within the scope of the appended claims.
Claims (9)
1. The cold-resistant low-compression permanent deformation rubber composition comprises, by weight, 100 parts of ethylene propylene diene monomer, 3-10 parts of zinc oxide, 90-130 parts of carbon black, 30-40 parts of hydrogenated paraffin oil, 10-20 parts of dibutyl sebacate, 0.5-1.5 parts of dicumyl peroxide, 1-3 parts of ultrafine graphite, 0.5-1.5 parts of N, N' -difurfurylideneacetone and 1-3 parts of an anti-aging agent MB;
in the ethylene-propylene-diene monomer, the ethylene content is 45-51%, the Mooney viscosity ML (1+4) is more than or equal to 70 at 125 ℃, and the ENB content is more than 6%.
2. The cold-resistant low-compression permanent-deformation rubber composition as claimed in claim 1, wherein the raw materials of the composition comprise, by weight, 100 parts of ethylene propylene diene monomer, 5 parts of zinc oxide, 110 parts of carbon black, 35 parts of hydrogenated paraffin oil, 15 parts of dibutyl sebacate, 1 part of dicumyl peroxide, 2 parts of ultrafine graphite, 1 part of N, N' -difurfurylideneacetone and 2 parts of anti-aging agent MB.
3. The cold-resistant low compression set rubber composition according to claim 1 or 2, wherein the carbon black is carbon black N550 and/or carbon black N660.
4. The cold resistant low compression set rubber composition of claim 3, wherein the carbon black is carbon black N550.
5. A method for preparing the rubber composition of any of claims 1-4, comprising the steps of: mixing the raw materials of the rubber composition in proportion.
6. The method according to claim 5, wherein the mixing is kneading in an internal mixer.
7. The production method according to claim 6, wherein the kneading speed is 40 r/min.
8. The method according to claim 6, wherein the mixing time is 4 to 6 min.
9. Use of the cold-resistant low compression set rubber composition according to any one of claims 1 to 4 for the preparation of rubber vibration damping mats or gaskets for rolling stock.
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| 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 |
| CN118325268B (en) * | 2024-05-13 | 2024-10-15 | 东莞市信东橡塑五金制品有限公司 | Low-compression permanent deformation battery sealing material and preparation method thereof |
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