CN110760132A - High-temperature-resistant low-voltage-variable ethylene propylene diene monomer rubber and preparation method thereof - Google Patents
High-temperature-resistant low-voltage-variable ethylene propylene diene monomer rubber and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention discloses high-temperature-resistant low-voltage-change ethylene propylene diene monomer rubber which comprises the following components in parts by weight: 100 parts of raw ethylene propylene diene monomer, 20-30 parts of chloroprene rubber, 30-50 parts of graphene, 5-10 parts of zinc oxide, 0.6-3 parts of zinc stearate, 0.2-0.8 part of BaSO4, 50-80 parts of reinforcing filler, 10-15 parts of benzoyl peroxide, 1-3 parts of vulcanizing assistant and 0.5-1 part of composite additive.
Description
Technical Field
The invention relates to the technical field of rubber preparation, in particular to ethylene propylene diene monomer rubber with high temperature resistance and low pressure change and a preparation method thereof.
Background
The ethylene propylene diene monomer rubber has the main characteristics of excellent oxidation resistance, ozone resistance and erosion resistance, and has excellent vulcanization characteristic because the ethylene propylene diene monomer rubber belongs to a polyolefin family, but the ethylene propylene diene monomer rubber is a combustible substance, and the sulfur-vulcanized ethylene propylene diene monomer rubber in the prior art has poor high temperature resistance and compression permanent deformation resistance and is difficult to meet the use requirement.
Ethylene propylene diene monomer is a terpolymer of ethylene, propylene and non-conjugated diene, the worldwide consumption is 80 ten thousand tons every year, the requirements on the quality of automobiles and parts are continuously improved along with the increase of the demand and the production and sales volume of the automobiles at home and abroad, the requirements on the service environment and the rebound resilience of a hose are higher and higher, and higher requirements are provided for the heat resistance and the low compression permanent deformation performance of the ethylene propylene diene monomer.
Disclosure of Invention
In order to solve the problems, the invention provides the ethylene propylene diene monomer with high temperature resistance and low pressure change resistance and the preparation method thereof, and the ethylene propylene diene monomer has good mechanical property, high temperature resistance, low pressure change resistance and easy edge tearing.
The invention provides ethylene propylene diene monomer rubber with high temperature resistance and low pressure change, which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer raw rubber, 20-30 parts of chloroprene rubber, 30-50 parts of graphene, 5-10 parts of zinc oxide, 0.6-3 parts of zinc stearate, 0.2-0.8 part of BaSO4, 50-80 parts of reinforcing filler, 10-15 parts of benzoyl peroxide, 1-3 parts of vulcanization aid and 0.5-1 part of composite additive.
Preferably, the reinforcing filler comprises carbon black N990, glass beads.
Preferably, the complex additive comprises 2-mercapto benzimidazole, dioctyl adipate and carnauba wax.
Preferably, the vulcanization aid comprises one or more of triallyl cyanurate and triallyl isocyanurate.
Preferably, the method comprises the following steps: s1, mixing, namely mixing ethylene propylene diene monomer raw rubber, chloroprene rubber and zinc stearate, performing heat treatment on the mixture for 3-4 times at a temperature of 60-90 ℃ for 10-30min, carrying out reinforcing filler, graphene, zinc oxide, 2-mercaptopropionyl imidazole, dioctyl adipate and carnauba wax, vacuumizing, discharging rubber after 20-40 min, introducing the rubber material into an open type rubber mixing mill for 2-4 times, and filtering in a rubber filtering mill to obtain a clean and impurity-free rubber material; s2, remilling, heating to restore the plasticity of the rubber material obtained in the S1, adding benzoyl peroxide and an auxiliary crosslinking agent, thinly passing for 10-15 times, and rolling and discharging; s3, vulcanizing, namely vulcanizing the rubber material obtained in the step S2 by using microwave steam to obtain the low-temperature-resistant rubber.
Preferably, the vulcanization temperature of the microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20 min. The carbon black N900 has better elasticity, is easy to disperse in the ethylene propylene diene raw rubber, and is added with a certain amount of BaSO4The high-temperature compression permanent deformation performance and the high-temperature aging resistance of the ethylene propylene diene monomer are improved.
In order to improve the crosslinking efficiency of peroxide, accelerate the vulcanization speed, reduce the decomposition temperature of the peroxide and maintain the excellent performance of the vulcanized rubber, the proposal uses the vulcanization aids triallyl cyanurate and triallyl isocyanurate to vulcanize the rubber, the vulcanization aid contains 2 or more unsaturated groups in molecules, the unsaturated groups can be polymerized to form a reinforcing substance similar to resin under the condition of the existence of free radicals, the increase degree of the elastic modulus of a sizing material is larger than that of the single peroxide, the coagent is polymerized to form a multi-branched resin reinforcing filler or the coagent reacts with polymer free radicals to form a polymer branched chain under the existence of the free radicals, the vulcanization aid and the vulcanizing agent benzoyl peroxide form a composite combination simultaneously containing the nuclear crosslinking assisting function of the peroxide, the defect of generating odorous byproducts when being used alone is solved, and the solubility and the dynamic performance of the peroxide are improved, the crosslinking density of vulcanized rubber is improved, and the flame resistance is improved; meanwhile, in the scheme, inflammable ethylene propylene diene monomer raw rubber is mixed with flame-retardant chloroprene rubber, and a flame-retardant polymer is used together with inflammable rubber to improve flame retardance.
The vulcanizate is in the use, and polysulfide bond can fracture, and the hydrogen sulfide of formation can accelerate the ageing of rubber, and in this scheme, graphite alkene has the adsorption to alkali metal, with the even absorption of zinc oxide on graphite alkene surface, and zinc oxide can react with the hydrogen sulfide that generates, consumes hydrogen sulfide to slow down the ageing of rubber, promote the ageing-resistant performance of rubber, the addition of graphite alkene has reduced the gluey content of raw rubber, makes the finished product easily tear the limit.
The scheme adopts microwave steam vulcanization, overcomes the defect of slow heat transfer of hot air, and has short vulcanization time, difficult aging, thorough vulcanization and no byproduct production; and the micromolecule low-boiling-point substances are removed by vacuum in the mixing process.
Compared with the prior art, the beneficial effect of this scheme is as follows:
1. the carbon black N900 has better elasticity, but is easy to disperse in the ethylene propylene diene raw rubber, and the addition of a certain amount of BaSO4 is beneficial to improving the high-temperature compression permanent deformation performance and the high-temperature aging resistance of the ethylene propylene diene raw rubber;
2. the vulcanization auxiliary agent and the vulcanizing agent benzoyl peroxide form a composite combination simultaneously containing a peroxide core-assisted crosslinking function, so that the vulcanization speed is accelerated, the decomposition temperature of the peroxide is reduced, the excellent performance of vulcanized rubber is kept, the crosslinking density of the vulcanized rubber is improved, the flame resistance is improved, and the flammable ethylene propylene diene monomer raw rubber and the flame-retardant chloroprene rubber are mixed, so that the flame resistance can be improved and the heat resistance can be improved by using the flame-retardant polymer and the flammable rubber together;
3. the zinc oxide is uniformly adsorbed on the surface of the graphene, and the zinc oxide reacts with generated hydrogen sulfide to consume the hydrogen sulfide, so that the aging of the rubber is slowed down, the aging resistance of the rubber is improved, the low-pressure change is realized, the rubber content of raw rubber is reduced due to the addition of the graphene, and the finished product is easy to tear;
5. microwave steam vulcanization is adopted, the defect of slow heat transfer of hot air is overcome, the vulcanization time is short, the aging is not easy, the vulcanization is thorough, and byproducts are not produced; and in the mixing process, small molecular low-boiling-point substances and mechanical bubbles are removed by using vacuum;
drawings
FIG. 1 shows the results of the mechanical property measurements of the high temperature and low pressure resistant EPDM prepared in examples 1-4.
Detailed Description
The following is a detailed description of the embodiments of the present invention with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
S1, mixing: kneading 100g of raw ethylene propylene diene monomer, 20g of chloroprene rubber and 0.6g of zinc stearate in a vacuum kneader for 3-5 minutes, firstly adding 30g of graphene into organic solvent tetrahydrofuran, performing ultrasonic treatment for 5 minutes to form uniform and stable dispersion liquid, then adding the dispersion liquid into the kneaded silica gel, continuing performing ultrasonic stirring, gathering a raw rubber mixture into a graphene oxide lamellar structure in an intercalation form, continuously ensuring the entropy balance of a system in a desorption form by solvent molecules, finally forming a stable intercalation structure, removing the solvent by rotary evaporation to obtain a graphene/rubber composite material, and adding 0.2g of BaSO 3-4 times450g of carbon black N990, 5g of zinc oxide, 0.1g of 2-mercaptobenzimidazole, 0.2g of dioctyl adipate and 0.1g of carnauba wax are stirred and mixed uniformly at 10-50 r/min, then heat treatment is carried out for 10-30min at the temperature of 60-90 ℃, then the degree of vacuum pumping is-0.07-0.05 Mpa, the rubber is discharged after vacuum pumping is carried out for 30-60 min, then the rubber material is thinly passed through an open rubber mixing mill for 3-5 times, and then filtration is carried out on a rubber filter to obtain the clean and impurity-free rubber material;
s2, remilling: heating to restore plasticity of the silicone rubber, when the rubber material becomes soft and smooth, adding 10g of benzoyl peroxide and 1g of triallyl cyanurate, performing thin passing for 8-10 times, and rolling and discharging;
s3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 2
S1, mixing: kneading 100g of raw ethylene propylene diene monomer, 30g of chloroprene rubber and 3g of zinc stearate in a vacuum kneader for 3-5 minutes, firstly adding 50g of graphene into organic solvent tetrahydrofuran, performing ultrasonic treatment for 5 minutes to form uniform and stable dispersion liquid, then adding the dispersion liquid into the kneaded silica gel, continuing to perform ultrasonic stirring, gathering a raw rubber mixture into a graphene oxide lamellar structure in an intercalation form, continuously ensuring the entropy balance of a system in a desorption form by solvent molecules, finally forming a stable intercalation structure, performing rotary evaporation to remove the solvent to obtain a graphene/rubber composite material, adding 0.8g of BaSO4, 40g of carbon black N990, 40g of glass beads, 10g of zinc oxide, 0.2g of 2-mercaptophenylimidazole, 0.4g of dioctyl adipate and 0.4g of carnauba wax 3-4 times, stirring and mixing uniformly at a speed of 10-50 r/min, performing heat treatment at 60-90 deg.C for 10-30min, vacuumizing to-0.07-0.05 Mpa for 30-60 min, discharging, passing the rubber material on an open rubber mixing mill for 3-5 times, and filtering on a rubber filter to obtain clean and impurity-free rubber material;
s2, remilling: heating to restore the plasticity of the silicon rubber, when the rubber material becomes soft and smooth, adding 15g of benzoyl peroxide and 3g of triallyl isocyanurate, performing thin passing for 8-10 times, and rolling and discharging;
s3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 3
S1, mixing: kneading 100g of raw ethylene propylene diene monomer, 25g of chloroprene rubber and 1g of zinc stearate in a vacuum kneader for 3-5 minutes, firstly adding 40g of graphene into organic solvent tetrahydrofuran, performing ultrasonic treatment for 5 minutes to form uniform and stable dispersion liquid, then adding the dispersion liquid into the kneaded silica gel, continuing to perform ultrasonic stirring, gathering a raw rubber mixture into a graphene oxide lamellar structure in an intercalation form, continuously ensuring the entropy balance of a system in a desorption form by solvent molecules, finally forming a stable intercalation structure, performing rotary evaporation to remove the solvent to obtain a graphene/rubber composite material, adding 0.6g of BaSO4, 60g of carbon black N990, 8g of zinc oxide, 0.2g of 2-mercaptobenzimidazole, 0.2g of dioctyl adipate and 0.2g of carnauba wax for 3-4 times, stirring and mixing uniformly at the speed of 10-50 r/min, performing heat treatment at 60-90 deg.C for 10-30min, vacuumizing to-0.07-0.05 Mpa for 30-60 min, discharging, passing the rubber material on an open rubber mixing mill for 3-5 times, and filtering on a rubber filter to obtain clean and impurity-free rubber material;
s2, remilling: heating to restore the plasticity of the silicon rubber, when the rubber material becomes soft and smooth, adding 13g of benzoyl peroxide and 2g of triallyl isocyanurate, performing thin passing for 8-10 times, and rolling and discharging;
s3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 4
S1, mixing: kneading 100g of ethylene propylene diene monomer raw rubber and 1g of zinc stearate in a vacuum kneader for 3-5 minutes, adding 60g of carbon black N990, 8g of zinc oxide and 0.2g of carnauba wax 3-4 times, stirring and mixing uniformly at 10-50 r/min, carrying out heat treatment for 10-30min at the temperature of 60-90 ℃, vacuumizing to-0.07-0.05 Mpa, discharging the rubber after vacuumizing for 30-60 minutes, thinly passing the rubber material on an open rubber mixing mill for 3-5 times, and filtering on a rubber filter to obtain the clean and impurity-free rubber material;
s2, remilling: heating to restore plasticity of the silicone rubber, when the rubber material becomes soft and smooth, adding 13g of benzoyl peroxide, performing thin passing for 8-10 times, and rolling to obtain a sheet;
s3, vulcanization: adjusting the conditions that the vulcanization temperature of microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20min, and vulcanizing the colloid to obtain the low-temperature resistant rubber.
Example 5
The ethylene propylene diene monomer rubber with high temperature resistance and low pressure change prepared by the scheme is tested according to the standards GB/T531.1-2008, GB/T528-2009, GB/T3512-2014 and GB/T7759.1-2014, and the result is shown in figure 1, and the ethylene propylene diene monomer rubber has good mechanical property, is resistant to high temperature and low pressure change at 150 ℃ and has small deformation.
The above mentioned matters are not related, and all the matters are applicable to the prior art.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (6)
1. The high-temperature-resistant low-voltage-change ethylene propylene diene monomer is characterized by comprising the following components in parts by weight: 100 parts of ethylene propylene diene monomer raw rubber, 20-30 parts of chloroprene rubber, 30-50 parts of graphene, 5-10 parts of zinc oxide, 0.6-3 parts of zinc stearate and 0.2-0.8 part of BaSO450-80 parts of reinforcing filler, 10-15 parts of benzoyl peroxide, 1-3 parts of vulcanization aid and 0.5-1 part of composite additive.
2. The EPDM rubber with high temperature and low pressure resistance as recited in claim 1, wherein the reinforcing filler comprises carbon black N990 and glass beads.
3. The ethylene propylene diene monomer rubber resistant to high temperature and low pressure changes as claimed in claim 1, wherein the composite additive comprises 2-mercapto benzimidazole, dioctyl adipate and carnauba wax.
4. The EPDM of claim 1, wherein the vulcanization aid comprises one or more of triallyl cyanurate and triallyl isocyanurate.
5. Ternary B with high temperature resistance and low voltage changeThe preparation method of the propylene rubber is characterized by comprising the following steps: s1, mixing, namely mixing ethylene propylene diene monomer raw rubber, chloroprene rubber and zinc stearate, and adding BaSO 3-4 times4Heat-treating reinforcing filler, graphene, zinc oxide, 2-mercapto benzimidazole, dioctyl adipate and carnauba wax at 60-90 ℃ for 10-30min, vacuumizing, discharging glue 20-40 min, thinly passing the glue stock for 2-4 times in an open rubber mixing mill, and filtering in a rubber filter to obtain a clean and impurity-free glue stock; s2, remilling, heating to restore the plasticity of the rubber material obtained in the S1, adding benzoyl peroxide and an auxiliary crosslinking agent, thinly passing for 10-15 times, and rolling and discharging; s3, vulcanizing, namely vulcanizing the rubber material obtained in the step S2 by using microwave steam to obtain the low-temperature-resistant rubber.
6. The method for preparing EPDM rubber with high temperature and low pressure resistance as recited in claim 5, wherein the vulcanization temperature of the microwave steam vulcanization is 120-150 ℃, the microwave frequency is 1000-1500MHz, and the vulcanization time is 10-20 min.
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| CN116063800A (en) * | 2023-02-03 | 2023-05-05 | 六安江淮电机有限公司 | Self-lubricating fluorosilicone rubber sealing ring for motor and preparation method thereof |
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| CN110900914A (en) * | 2019-12-06 | 2020-03-24 | 云南大泽电极科技股份有限公司 | Production and vulcanization process of rubber cathode insulating strip |
| CN114874557B (en) * | 2022-05-27 | 2023-11-21 | 陕西特种橡胶制品有限公司 | High-temperature-resistant low-expansion-rate rubber material for nuclear island equipment and preparation method thereof |
| CN115124788A (en) * | 2022-07-15 | 2022-09-30 | 安徽工程大学 | High-strength high-toughness modified ethylene propylene diene monomer rubber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812204A (en) * | 2009-12-08 | 2010-08-25 | 天津鹏翎胶管股份有限公司 | Formula of rubber hose of peroxide vulcanization radiator |
| CN105400088A (en) * | 2015-12-11 | 2016-03-16 | 重庆可益荧新材料有限公司 | Ethylene-propylene-diene monomer and chloroprene rubber co-vulcanization material and preparation method therefor |
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- 2019-09-24 CN CN201910902968.6A patent/CN110498977A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812204A (en) * | 2009-12-08 | 2010-08-25 | 天津鹏翎胶管股份有限公司 | Formula of rubber hose of peroxide vulcanization radiator |
| CN105400088A (en) * | 2015-12-11 | 2016-03-16 | 重庆可益荧新材料有限公司 | Ethylene-propylene-diene monomer and chloroprene rubber co-vulcanization material and preparation method therefor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116063800A (en) * | 2023-02-03 | 2023-05-05 | 六安江淮电机有限公司 | Self-lubricating fluorosilicone rubber sealing ring for motor and preparation method thereof |
| CN116063800B (en) * | 2023-02-03 | 2024-05-28 | 六安江淮电机有限公司 | Self-lubricating fluorosilicone rubber sealing ring for motor and preparation method thereof |
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Application publication date: 20200207 |