CN114395196A - Low-temperature-resistant ethylene propylene diene monomer sealing element and preparation method thereof - Google Patents

Low-temperature-resistant ethylene propylene diene monomer sealing element and preparation method thereof Download PDF

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Publication number
CN114395196A
CN114395196A CN202111645723.3A CN202111645723A CN114395196A CN 114395196 A CN114395196 A CN 114395196A CN 202111645723 A CN202111645723 A CN 202111645723A CN 114395196 A CN114395196 A CN 114395196A
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China
Prior art keywords
parts
propylene diene
ethylene propylene
diene monomer
rubber
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CN202111645723.3A
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Chinese (zh)
Inventor
肖伟
曾轶
周江帆
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Jihua 3517 Rubber Products Co Ltd
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Jihua 3517 Rubber Products Co Ltd
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Priority to CN202111645723.3A priority Critical patent/CN114395196A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Abstract

The invention discloses a low-temperature-resistant ethylene propylene diene monomer sealing element, which belongs to the field of rubber materials and comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 3-8 parts of activator, 3.6-6 parts of vulcanizing agent, 4-8 parts of accelerator, 55-70 parts of filling reinforcing agent and 15-30 parts of plasticizer, and also discloses a preparation method of the low temperature resistant ethylene propylene diene monomer sealing element, which comprises four steps of pre-refining, mixing, vulcanizing and remixing.

Description

Low-temperature-resistant ethylene propylene diene monomer sealing element and preparation method thereof
Technical Field
The invention belongs to the field of rubber materials, relates to a low-temperature-resistant ethylene propylene diene monomer sealing element and a preparation method thereof, and particularly relates to an ethylene propylene diene monomer sealing element used for a long time under the condition of low temperature (-60 ℃) and a preparation method thereof.
Background
At present, the ethylene propylene diene monomer sealing element can be generally used below 150 ℃ for a long time, but under the condition of sufficient low temperature, the ethylene propylene diene monomer can be converted into a glass state and lose elasticity, so that the ethylene propylene diene monomer sealing element cannot be used, and the ethylene propylene diene monomer can be converted into the glass state under the condition of generally-45 ℃ to-55 ℃ according to the difference of ethylene content, so that the use value is lost. Therefore, if the ethylene propylene diene monomer product has a service function at a lower temperature, the ethylene propylene diene monomer sealing element needs to be improved.
The ethylene propylene diene monomer sealing element is used in some conventional equipment in the past, the requirement on the low temperature is not high, generally, the low temperature is about-50 ℃, but with the continuous development of the society, people are exploring more and more in the world, the requirement on the conventional equipment is higher and higher, the condition for using the equipment is more and more rigorous, and therefore, the requirements on various parts of the equipment are higher and higher, for example, the original-50 ℃ condition now requires the temperature to reach-60 ℃ or even lower, if only one small sealing element causes paralysis of large-scale equipment, even causes potential safety hazard.
The ethylene propylene diene monomer rubber sealing element prepared by the invention can enable the glass transition temperature of ethylene propylene diene monomer rubber to reach-65 ℃, can enable the ethylene propylene diene monomer rubber sealing element to be used for a long time under the temperature condition of-60 ℃ or even lower without failure, and meets increasingly severe environmental condition requirements.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a low-temperature-resistant ethylene propylene diene monomer rubber sealing element which can be used for a long time under the condition of low temperature (below minus 60 ℃).
The invention also provides a preparation method of the low-temperature-resistant ethylene propylene diene monomer rubber sealing element.
In order to realize the purpose, the invention adopts the technical scheme that:
the low-temperature-resistant ethylene propylene diene monomer rubber sealing member comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 3-8 parts of activator, 3.6-6 parts of vulcanizing agent, 4-8 parts of accelerator, 55-70 parts of filling reinforcing agent and 15-30 parts of plasticizer; the Mooney viscosity of the ethylene propylene diene monomer is 60-90 N.m, wherein the ethylene content is 42-48%, and the ethylidene norbornene content of the third monomer is 9-11%.
Preferably, 100 parts of ethylene propylene diene monomer, 5.5 parts of activator, 4 parts of vulcanizing agent, 8 parts of accelerator, 60 parts of filling reinforcing agent and 20 parts of plasticizer; the Mooney viscosity of the ethylene propylene diene monomer is 65 N.m, wherein the ethylene content is 44%, and the ethylidene norbornene content of the third monomer is 9.0%.
Further, the ethylene propylene diene monomer rubber sealing element further comprises 1-2 parts of microcrystalline wax.
Furthermore, the active agent is 2-5 parts of metal oxide and 1-3 parts of stearic acid.
Further, the vulcanizing agent comprises 0.6-1 part of sulfur, 2-3 parts of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane (bis 2-5) and 1-2 parts of triallyl isocyanurate.
Further, the accelerator comprises 1-3 parts of zinc dibenzyl dithiocarbamate (ZBEC), 2-3 parts of 2, 2 '-Dithiodibenzothiazole (DM), 2-3 parts of 4, 4' -dithiodimorpholine (DTDM) and 1-2 parts of dipentaerythritol Tetrasulfide (TRA), and the accelerator at least comprises three of the ZBEC, the DM, the DTDM and the TRA.
Furthermore, the filling reinforcing agent is non-pollution high-ductility semi-reinforcing furnace black.
Further, the plasticizer is a mixture of 15-20 parts of ester plasticizer and 0-5 parts of alkyl phenolic resin.
A preparation method of a low-temperature-resistant ethylene propylene diene monomer sealing element comprises the following steps:
A. pre-smelting: mixing 100 parts of ethylene propylene diene monomer rubber in an open mill for 6-8 times, and obtaining a rubber material with a roller spacing of 1 mm;
B. mixing: adding a filling reinforcing agent and a plasticizer into the rubber material obtained in the step A, adding a vulcanizing agent, an accelerator, an activator and microcrystalline wax, mixing for 10-20min at a roll spacing of 3-4mm, controlling the temperature of an open mill at 50-70 ℃, and discharging and standing for 24h to obtain rubber compound;
C. smelting again: b, remilling the rubber compound obtained in the step B, thinly passing for 4-6 times, keeping the roller spacing at 1mm, keeping the temperature of an open mill at 40-60 ℃, and then discharging;
D. and (3) vulcanization: and D, carrying out mould pressing vulcanization on the fragment rubber material obtained in the step C by using a flat vulcanizing machine.
Further, the temperature of the sulfurization in the step D is 160-180 ℃, and the time is 20-50 min.
The invention has the beneficial effects that: 1. the vulcanized rubber product with low temperature resistance is manufactured by the selection of components and the optimization of content, the improvement of the process and the synergistic cooperation effect, and can be used for a long time at the temperature of below 60 ℃ below zero without failure;
2. the ethylene propylene diene monomer selected by the invention has medium Mooney, good processing property, low ethylene content and high ethylidene norbornene content as a third monomer, and can ensure full crosslinking;
3. the activator adopted by the invention is the combination of metal oxide and stearic acid, so that the heat resistance of the ethylene propylene diene monomer sealing element can be better improved, and the metal oxide with higher components is adopted to have quick heat transfer and quick heat dissipation, and has better performance compared with the prior art;
4. the selection of the vulcanization system is very important, generally speaking, the peroxide vulcanization system is stronger than the effective vulcanization system, and the invention adopts two types of vulcanizing agents with specific contents and accelerators to play a good synergistic effect, thereby not only improving the crosslinking performance of rubber, but also improving the vulcanization efficiency of the rubber;
5. the polar ester plasticizer is used in the non-polar rubber, so that the precipitation pollution of the plasticizer is not caused, the ester plasticizer is used to bear lower temperature compared with straight-chain hydrocarbon and naphthenic hydrocarbon plasticizers, and other performances of the rubber product are not reduced, but the product can be used at lower temperature;
6. the microcrystalline wax is added, so that the ethylene propylene diene monomer rubber is smoother, higher in smoothness and better in softening performance, and can play a role in optimizing the process;
7. the mixing process has great influence on the performance of the rubber compound, and mainly improves the dispersion uniformity of various compounding agents in rubber, controls the feeding sequence, mixing time, mixing temperature, mixing capacity, standing time and the like, ensures the uniform dispersion of the compounding agents, eliminates internal stress and ensures the quality of the rubber compound.
Detailed Description
For a better understanding of the present invention, embodiments of the present invention are described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
the low-temperature-resistant ethylene propylene diene monomer rubber sealing member comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 5.5 parts of activator, 4 parts of vulcanizing agent, 8 parts of accelerator, 60 parts of filling reinforcing agent, 20 parts of plasticizer and 1 part of microcrystalline wax; the Mooney viscosity of the ethylene propylene diene monomer is 65 N.m, wherein the ethylene content is 44%, and the ethylidene norbornene content of the third monomer is 9.0%.
A preparation method of a low-temperature-resistant ethylene propylene diene monomer sealing element comprises the following steps:
A. pre-smelting: mixing 100 parts of ethylene propylene diene monomer rubber in an open mill, performing thin passing for 6 times, and obtaining a rubber material with a roller spacing of 1 mm;
B. mixing: adding a filling reinforcing agent and a plasticizer into the rubber material obtained in the step A, adding a vulcanizing agent, an accelerator, an activator and microcrystalline wax, mixing for 10min, controlling the roll spacing to be 4mm, controlling the temperature of an open mill to be 50 ℃, and discharging and standing for 24h to obtain rubber compound;
C. smelting again: b, remilling the rubber compound obtained in the step B, thinly passing for 4 times, wherein the roller distance is 1mm, the temperature of an open mill is 60 ℃, and then discharging;
D. and (3) vulcanization: and D, carrying out mould pressing vulcanization on the fragment rubber material obtained in the step C by using a flat vulcanizing machine, wherein the vulcanization temperature is 160 ℃, and the vulcanization time is 50 min.
Example 2:
the low-temperature-resistant ethylene propylene diene monomer rubber sealing member comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 3 parts of activator, 6 parts of vulcanizing agent, 4 parts of accelerator, 55 parts of filling reinforcing agent, 30 parts of plasticizer and 2 parts of microcrystalline wax; the Mooney viscosity of the ethylene propylene diene monomer is 60 N.m, wherein the ethylene content is 48%, and the ethylidene norbornene content of the third monomer is 11%.
A preparation method of a low-temperature-resistant ethylene propylene diene monomer sealing element comprises the following steps:
A. pre-smelting: mixing 100 parts of ethylene propylene diene monomer rubber in an open mill, thinly passing for 8 times, and obtaining a rubber material with the roller spacing of 1 mm;
B. mixing: adding a filling reinforcing agent and a plasticizer into the rubber material obtained in the step A, adding a vulcanizing agent, an accelerator, an activator and microcrystalline wax, mixing for 20min, controlling the roll gap to be 3mm, controlling the temperature of an open mill to be 70 ℃, and discharging and standing for 24h to obtain rubber compound;
C. smelting again: b, remilling the rubber compound obtained in the step B, thinly passing for 6 times, keeping the roller spacing at 1mm, keeping the temperature of an open mill at 40 ℃, and then discharging;
D. and (3) vulcanization: and D, carrying out mould pressing vulcanization on the fragment rubber material obtained in the step C by using a flat vulcanizing machine, wherein the vulcanization temperature is 180 ℃, and the time is 20 min.
Example 3:
the low-temperature-resistant ethylene propylene diene monomer rubber sealing member comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 8 parts of activator, 3.6 parts of vulcanizing agent, 6 parts of accelerator, 70 parts of filling reinforcing agent, 15 parts of plasticizer and 1 part of microcrystalline wax; the Mooney viscosity of the ethylene propylene diene monomer is 90 N.m, wherein the ethylene content is 42%, and the ethylidene norbornene content of the third monomer is 10%.
A preparation method of a low-temperature-resistant ethylene propylene diene monomer sealing element comprises the following steps:
A. pre-smelting: mixing 100 parts of ethylene propylene diene monomer rubber in an open mill, thinly passing for 7 times, and obtaining a rubber material with the roller spacing of 1 mm;
B. mixing: adding a filling reinforcing agent and a plasticizer into the rubber material obtained in the step A, adding a vulcanizing agent, an accelerator, an activator and microcrystalline wax, mixing for 12min, controlling the roll spacing to be 4mm, controlling the temperature of an open mill to be 70 ℃, and discharging and standing for 24h to obtain rubber compound;
C. smelting again: b, remilling the rubber compound obtained in the step B, thinly passing for 5 times, keeping the roller spacing at 1mm, keeping the temperature of an open mill at 48 ℃, and then discharging;
D. and (3) vulcanization: and D, carrying out mould pressing vulcanization on the fragment rubber material obtained in the step C by using a flat vulcanizing machine, wherein the vulcanization temperature is 167 ℃, and the vulcanization time is 39 min.
The ethylene propylene diene monomer rubber sealing members prepared in the above examples 1 to 3 were used in low temperature equipment at a temperature of-60 ℃ or lower, and the performance parameters thereof are shown in table 1.
TABLE 1
Example 1 Example 2 Example 3
Glass transition temperature (Tg) -61.2℃ -59.6℃ -60.7℃
Brittleness temperature (Tb) -67.3℃ -64.5℃ -65.6℃
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.

Claims (10)

1. The low-temperature-resistant ethylene propylene diene monomer rubber sealing element is characterized by comprising the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 3-8 parts of activator, 3.6-6 parts of vulcanizing agent, 4-8 parts of accelerator, 55-70 parts of filling reinforcing agent and 15-30 parts of plasticizer; the Mooney viscosity of the ethylene propylene diene monomer is 60-90 N.m, wherein the ethylene content is 42-48%, and the ethylidene norbornene content of the third monomer is 9-11%.
2. The low temperature resistant EPDM rubber sealing member according to claim 1, wherein the EPDM rubber comprises 100 parts of EPDM rubber, 5.5 parts of activator, 4 parts of vulcanizing agent, 8 parts of accelerator, 60 parts of filling reinforcing agent and 20 parts of plasticizer; the Mooney viscosity of the ethylene propylene diene monomer is 65 N.m, wherein the ethylene content is 44%, and the ethylidene norbornene content of the third monomer is 9.0%.
3. The low temperature resistant epdm seal of claim 1, wherein the epdm seal composition further comprises 1-2 parts microcrystalline wax.
4. The low temperature resistant EPDM rubber seal of claim 1, wherein said activator is selected from the group consisting of metal oxide 2-5 parts and stearic acid 1-3 parts.
5. The low temperature resistant EPDM rubber seal according to claim 1, wherein said vulcanizing agent comprises sulfur 0.6-1 part, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5)2-3 parts, and triallyl isocyanurate 1-2 parts.
6. The low temperature resistant epdm rubber seal of claim 1, wherein the accelerators include zinc dibenzyl dithiocarbamate (ZBEC)1-3 parts, 2, 2 '-Dithiodibenzothiazyl (DM)2-3 parts, 4, 4' -dithiodimorpholine (DTDM)2-3 parts, and dipentamethylene Tetrasulfide (TRA)1-2 parts, and the accelerators include at least three of ZBEC, DM, DTDM, TRA.
7. The low temperature resistant EPDM rubber seal according to claim 1, wherein said filler is non-polluting high-ductility semi-reinforcing furnace black.
8. The low temperature resistant epdm rubber seal of claim 1, wherein the plasticizer is a mixture of 15-20 parts ester plasticizer and 0-5 parts alkylphenol formaldehyde resin.
9. The preparation method of the low-temperature-resistant ethylene propylene diene monomer sealing element is characterized by comprising the following steps of:
A. pre-smelting: mixing 100 parts of ethylene propylene diene monomer rubber in an open mill for 6-8 times, and obtaining a rubber material with a roller spacing of 1 mm;
B. mixing: adding a filling reinforcing agent and a plasticizer into the rubber material obtained in the step A, adding a vulcanizing agent, an accelerator, an activator and microcrystalline wax, mixing for 10-20min at a roll spacing of 3-4mm, controlling the temperature of an open mill at 50-70 ℃, and discharging and standing for 24h to obtain rubber compound;
C. smelting again: b, remilling the rubber compound obtained in the step B, thinly passing for 4-6 times, keeping the roller spacing at 1mm, keeping the temperature of an open mill at 40-60 ℃, and then discharging;
D. and (3) vulcanization: and D, carrying out mould pressing vulcanization on the fragment rubber material obtained in the step C by using a flat vulcanizing machine.
10. The method as claimed in claim 9, wherein the temperature of the vulcanization in step D is 160-180 ℃ for 20-50 min.
CN202111645723.3A 2021-12-30 2021-12-30 Low-temperature-resistant ethylene propylene diene monomer sealing element and preparation method thereof Pending CN114395196A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030149147A1 (en) * 2001-08-30 2003-08-07 Cooper Standard Automotive Inc. EPDM compounds for dynamic applications
CN107033406A (en) * 2016-11-29 2017-08-11 株洲时代新材料科技股份有限公司 Resilient sleeper-bearing under a kind of arctic rubber composite and preparation method thereof and the iron chair made by the arctic rubber composite
CN108841091A (en) * 2018-07-24 2018-11-20 湖南昶力轨道交通设备有限公司 One kind heat-resistant high-strength rubber material and its manufacturing process made of blend
CN110527200A (en) * 2019-09-09 2019-12-03 株洲时代新材料科技股份有限公司 The low temperature resistant high elastic rubber windshield material of one kind, preparation method and windscreen

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030149147A1 (en) * 2001-08-30 2003-08-07 Cooper Standard Automotive Inc. EPDM compounds for dynamic applications
CN107033406A (en) * 2016-11-29 2017-08-11 株洲时代新材料科技股份有限公司 Resilient sleeper-bearing under a kind of arctic rubber composite and preparation method thereof and the iron chair made by the arctic rubber composite
CN108841091A (en) * 2018-07-24 2018-11-20 湖南昶力轨道交通设备有限公司 One kind heat-resistant high-strength rubber material and its manufacturing process made of blend
CN110527200A (en) * 2019-09-09 2019-12-03 株洲时代新材料科技股份有限公司 The low temperature resistant high elastic rubber windshield material of one kind, preparation method and windscreen

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Application publication date: 20220426