CN116003917A - Environment-friendly oil-resistant ethylene propylene rubber composition for light-colored rubber tubes and preparation method thereof - Google Patents
Environment-friendly oil-resistant ethylene propylene rubber composition for light-colored rubber tubes and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title description 14
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 60
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 36
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- 239000011593 sulfur Substances 0.000 claims description 5
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
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- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical compound [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 description 1
- 238000010059 sulfur vulcanization Methods 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- WMYJOZQKDZZHAC-UHFFFAOYSA-H trizinc;dioxido-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S WMYJOZQKDZZHAC-UHFFFAOYSA-H 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Abstract
The invention discloses an environment-friendly oil-resistant ethylene propylene rubber composition for a light-colored rubber tube, which is prepared from the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 2-5 parts of zinc oxide, 1-3 parts of stearic acid, 150-230 parts of inorganic filler, 0-5 parts of silane coupling agent, 40-120 parts of paraffin oil, 2-4 parts of anti-aging agent, 0-2 parts of vulcanizing agent and 3-8 parts of accelerator. The environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube has the advantages of meeting the oil resistance, along with environment protection, good processing performance and physical and mechanical properties, suitability for extrusion process and high economic value.
Description
Technical Field
The invention belongs to the field of rubber, relates to environment-friendly oil-resistant rubber for preparing rubber products, and in particular relates to an environment-friendly oil-resistant ethylene propylene rubber composition for light-colored rubber tubes and a preparation method thereof.
Background
Ethylene Propylene Diene Monomer (EPDM) is widely used in the fields of automobile parts, heat-resistant rubber pipes and the like because of its excellent heat resistance and weather resistance. However, ethylene propylene diene monomer itself belongs to nonpolar rubber, has poor oil resistance, and is easily damaged by the swelling of nonpolar mineral oil and fuel oil. In order to solve the problem of poor oil resistance of ethylene propylene diene monomer rubber, polar rubber such as Nitrile Butadiene Rubber (NBR) and ethylene acrylic ester rubber (AEM) can be used together, but the compatibility of the two polar rubbers is problematic after the polar rubber is used together, and the rubber mixing process is relatively complex.
The oil resistance of the ethylene propylene diene monomer can be improved by adding raw rubber Mooney and ethylene content, adding parts of filler, adding the dosage of vulcanizing agent and the like. Patent application CN111057317A discloses an oil-resistant radiator water pipe material vulcanized by a peroxide system, which is an oil-resistant EPDM rubber material of the peroxide vulcanization system, and the rubber material has good oil resistance but poor hot tearing and fatigue performance due to the formation of carbon-carbon crosslinking bonds by the peroxide vulcanization system, and an oxygen removal process is also needed when the rubber material is used for naked vulcanization of the outer layer of a rubber pipe, so that the energy consumption is increased. Patent application CN107759909a relates to an oil-resistant EPDM rubber material of sulfur vulcanization system, which is not easy to bloom, but has poor compression property due to the selection of oil-filled raw rubber with high ethylene content, and has large limitation, and is only suitable for injection products, when being used for extrusion products, the rubber is easy to roll during braiding, so that the size is unstable, and simultaneously, the selected vulcanizing agent generates nitrosamine in the vulcanization process to generate aminolysis reaction on a polyester reinforcing layer, so that the performance of the products is reduced.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides an ethylene propylene rubber composition which is suitable for an extrusion process and has excellent physical properties, light color, environmental protection and oil resistance.
The invention aims at realizing the following technical scheme:
the environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube is prepared from the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 2-5 parts of zinc oxide, 1-3 parts of stearic acid, 150-230 parts of inorganic filler, 0-5 parts of silane coupling agent, 40-120 parts of paraffin oil, 2-4 parts of anti-aging agent, 0-2 parts of vulcanizing agent and 3-8 parts of accelerator.
In consideration of vulcanization speed, processability and physical properties, the environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube is prepared from the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 2-5 parts of zinc oxide, 1-3 parts of stearic acid, 150-230 parts of inorganic filler, 2-5 parts of silane coupling agent, 60-80 parts of paraffin oil, 2-4 parts of anti-aging agent, 1-2 parts of sulfur and 3-8 parts of accelerator.
The ethylene propylene diene monomer is long-chain branched ethylene propylene diene monomer, the Mooney viscosity ML (1+8) is 60-70 at 150 ℃, the ethylene content is 50-70%, and the ENB content is 5-10%.
In particular, 10950C may be used for ethylene propylene diene monomer.
The inorganic filler is light-colored inorganic filler and is selected from one or a combination of more of Sililitin V85, sililitin VM56 and titanium dioxide; preferably, the weight ratio of the Sililitin V85, the VM56 and the titanium pigment is (2-3): 1, more preferably, the weight ratio of the Sililitin V85, the VM56 and the titanium pigment is 2:2:1.
The silane coupling agent is silane coupling agent A151, silane coupling agent SI69 and silane coupling agent A172.
The paraffin oil is YP5002.
The anti-aging agent is one or a combination of more of anti-aging agent TNP, anti-aging agent ZMTI and anti-aging agent 445; preferably a combination of anti-aging agent TNP, anti-aging agent ZMTI and anti-aging agent 445 in a weight ratio of 1:1:1.
The vulcanizing agent is sulfur S-80.
The accelerator is a comprehensive accelerator LHG-80.
The invention further aims to provide a preparation method of the environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube, which comprises the following steps of:
setting the initial temperature of an internal mixer to 55 ℃ and the rotating speed of a rotor to 30r/min, firstly adding ethylene propylene diene monomer into the internal mixer, banburying for 30s, then adding zinc oxide, stearic acid and an anti-aging agent, banburying for 60s, then adding a silane coupling agent, an inorganic filler which is half of the total weight and paraffin oil which is half of the total weight, banburying for 4-6 min, then adding the rest inorganic filler and paraffin oil, continuously mixing, discharging rubber when the temperature of the internal mixer is increased to 130 ℃, transferring to an open rubber mixer for thin-pass sheet discharging, and cooling to room temperature to obtain master batch;
step (2), putting the masterbatch prepared in the step (1) into an internal mixer, adding a vulcanizing agent and an accelerator at the temperature of 85 ℃, discharging the masterbatch when the temperature of the internal mixer is increased to 105 ℃, and thinning out the masterbatch to obtain ethylene propylene diene monomer rubber compound;
and (3) placing the ethylene propylene diene monomer rubber compound into a plate vulcanizing machine, and vulcanizing for 30min at 160+/-3 ℃ to obtain the ethylene propylene diene monomer rubber composition.
The invention relates to a light-color rubber tube, which takes the environment-friendly oil-resistant ethylene propylene rubber composition for the light-color rubber tube as an inner rubber layer and an outer rubber layer, extrudes the ethylene propylene rubber composition on a steel core through an extruder to obtain a tube blank, places the tube blank with a core rod into a braiding machine, adopts 1500D polyester wires to carry out braiding to form a polyester reinforcing layer, and coats the ethylene propylene rubber composition on the braided tube through the extruder, and then carries out vulcanization and core pulling to obtain a rubber tube product.
The invention has the beneficial effects that:
the environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube, which is prepared by proportioning various raw materials, has the advantages of environment friendliness, good processability and physical and mechanical properties while meeting the oil resistance, is suitable for extrusion process, and has high economic value, and the environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube is particularly characterized in that:
the invention selects the long-chain branched ethylene propylene diene monomer with ultrahigh Mooney and medium ethylene content, provides excellent physical and mechanical properties and processing properties for rubber materials, can effectively prevent the phenomenon of rolling rubber in the process of braiding rubber tubes, and ensures the dimensional stability of products.
The Sillitin V85 is an inorganic mineral consisting of natural quasi-spherical granular quartz and platy kaolin, and the minerals with different shapes are naturally combined to form a loose lamination mosaic structure of granules, and the natural loose lamination mosaic structure cannot be separated by a common physical and mechanical mode, so that the natural loose lamination mosaic structure has more excellent dispersibility and fluidity when being added into other objects, has excellent dispersibility and no agglomeration tendency, and ensures that the product has low compression permanent deformation; VM56 has a structure similar to that of Sillitin V85, and both have good reinforcing performance and oil resistance; the excellent high hiding power of the titanium pigment can improve the smoothness of the sizing material and simultaneously endow the sizing material with good weather resistance. The invention further improves the dispersibility and the fluidity of the inorganic filler in the sizing material through the silane coupling agent, and avoids agglomeration.
The paraffin oil YP5002 is high-saturation hydrogenated paraffin oil, has extremely low content of heterocyclic compounds such as nitrogen, sulfur and oxygen, effectively avoids the conditions of fading, aging and polymer cracking caused by the heterocyclic compounds, has small content of dimethyl sulfoxide extract in the paraffin oil YP5002, does not need to mark carcinogenesis tendency, and is harmless to human health and environment.
The invention selects the anti-aging agents TNP and ZMTI, which belong to non-pollution heat-resistant antioxidant anti-aging agents, have high thermo-oxidative stability and do not change color in the process of processing and use, and are especially suitable for serving as non-color-changing stabilizers; the color of the rubber plastic product is not affected, the heat resistance and the oxidation resistance of the rubber plastic product can be improved, and the thermo-oxidative aging and the yellowing of the rubber plastic product are prevented; the antioxidant 445 is an efficient and non-discoloring arylamine main antioxidant, and has good heat stability and long-term heat aging performance; the antioxidant 445 is used in combination with the antioxidants TNP and ZMTI to provide excellent synergistic effects.
The invention selects the comprehensive accelerator LHG-80, which is an environment-friendly comprehensive accelerator special for EPDM by synergistic combination of zinc dithiophosphate, benzothiazole and sulfenamide accelerators, has good dispersibility in sizing materials, can improve the vulcanization rate of EPDM and does not spray frost, is especially suitable for extrusion products, does not generate nitrosamine in the vulcanization process to generate aminolysis on polyester materials, and ensures the performance of the products.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
TABLE 1 Components and parts by weight of rubber compositions of examples 1-3 and comparative examples 1-4
Note that: paraffin oil YP5002 was purchased from angyi composites limited.
Example 1
The environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube is prepared according to the following preparation method, wherein the components and the parts by weight of the composition are shown in table 1:
setting the initial temperature of an internal mixer to 55 ℃ and the rotating speed of a rotor to 30r/min, firstly adding ethylene propylene diene monomer into the internal mixer, after banburying for 30s, adding zinc oxide, stearic acid, an anti-aging agent TNP, an anti-aging agent ZMTI and an anti-aging agent 445, after banburying for 60s, adding a silane coupling agent A151 and an inorganic filler accounting for half of the total weight (namely, respectively adding half of the Sillitin V85, VM56 and titanium pigment) and a paraffin oil YP5002 accounting for half of the total weight, after banburying for 300s, adding the rest inorganic filler and the paraffin oil YP5002, continuing to mix, discharging rubber, moving to an open rubber mixer for thin-pass discharging sheet when the temperature of the internal mixer is raised to 130 ℃, and cooling to room temperature to obtain master batch;
step (2), putting the masterbatch prepared in the step (1) into an internal mixer, adding S-80 and an integrated accelerator LHG-80 at the temperature of 85 ℃, discharging the masterbatch when the temperature of the internal mixer is increased to 105 ℃, and thinning out the masterbatch to obtain ethylene propylene diene monomer rubber compound;
and (3) placing the ethylene propylene diene monomer rubber compound into a plate vulcanizing machine for vulcanization, wherein the vulcanization temperature is 160+/-3 ℃ and the vulcanization time is 30 minutes, and obtaining the ethylene propylene diene monomer rubber composition.
The ethylene propylene diene monomer composition prepared in the embodiment is extruded on a steel core with the outer diameter of 10.0mm as inner rubber through an extruder to obtain a tube blank with the outer diameter of 13.9mm, the tube blank with a core rod is put into a braiding machine to be braided, a 24-spindle 2-strand 1500D polyester wire with a braiding structure forms a polyester reinforcing layer, the lead is 33.0mm, the outer diameter is 14.7mm, the ethylene propylene diene monomer composition prepared in the embodiment is coated on the braided tube through the extruder by the braided tube, a rubber hose with the outer diameter of 17.0mm is produced, and the core is pulled out after vulcanization for 30min at 160 ℃ to obtain a rubber hose product. In the embodiment, the rubber rolling phenomenon is not seen in the weaving process of the rubber hose.
Example 2
The ethylene propylene diene monomer rubber composition is prepared by a preparation method of the ethylene propylene diene monomer rubber composition in example 1, wherein the components and the parts by weight of the ethylene propylene diene monomer rubber composition are shown in table 1.
Referring to the preparation method of the rubber hose of example 1, the ethylene propylene diene monomer rubber composition prepared in this example was used as the inner rubber and the outer rubber, and the rest was the same as in example 1, so as to prepare the rubber hose.
Example 3
The ethylene propylene diene monomer rubber composition is prepared by a preparation method of the ethylene propylene diene monomer rubber composition in example 1, wherein the components and the parts by weight of the ethylene propylene diene monomer rubber composition are shown in table 1.
Referring to the preparation method of the rubber hose of example 1, the ethylene propylene diene monomer rubber composition prepared in this example was used as the inner rubber and the outer rubber, and the rest was the same as in example 1, so as to prepare the rubber hose.
Comparative example 1
The ethylene propylene diene monomer rubber composition is prepared by a preparation method of the ethylene propylene diene monomer rubber composition in example 1, wherein the components and the parts by weight of the ethylene propylene diene monomer rubber composition are shown in table 1.
Referring to the preparation method of the rubber hose of example 1, the rubber hose was prepared by using the ethylene propylene diene monomer composition prepared in comparative example 1 as an inner layer rubber and an outer layer rubber, and the rest was the same as in example 1.
Comparative example 2
The ethylene propylene diene monomer rubber composition is prepared by a preparation method of the ethylene propylene diene monomer rubber composition in example 1, wherein the components and the parts by weight of the ethylene propylene diene monomer rubber composition are shown in table 1.
Comparative example 3
The ethylene propylene diene monomer rubber composition is prepared by a preparation method of the ethylene propylene diene monomer rubber composition in example 1, wherein the components and the parts by weight of the ethylene propylene diene monomer rubber composition are shown in table 1.
Comparative example 4
The ethylene propylene diene monomer rubber composition is prepared by a preparation method of the ethylene propylene diene monomer rubber composition in example 1, wherein the components and the parts by weight of the ethylene propylene diene monomer rubber composition are shown in table 1.
The ethylene propylene diene monomer compositions prepared in examples 1 to 3 and comparative examples 1 to 4 were subjected to detection tests according to the detection standards of GB/T531.1-2008, GBT 528-2009, GBT 7759.1-2015, GBT 1682-2014 and GBT 1690-2010, and the results are shown in Table 2.
TABLE 2 Properties of the rubber materials of examples 1-3 and comparative examples 1-4
The rubber hoses prepared in examples 1 to 3 and comparative example 1 were tested according to the test standard of GBT 16897-2010, and the results are shown in Table 3.
TABLE 3 Properties of the rubber hose products of examples 1-3 and comparative example 1
| Project | Unit (B) | Index (I) | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Burst strength | MPa | ≥10 | 12.2 | 12.1 | 12.4 | 8.9 |
From the data in tables 2 and 3, it can be derived that: the accelerator used in comparative example 1 was subject to an aminolysis reaction with the polyester reinforcing layer, resulting in a decrease in burst strength of the rubber hose, compared with examples 1 to 3; in comparative example 2, paraffin oil 2280 is selected, the pour point of which is higher than that of paraffin oil YP5002, the brittleness temperature is higher, and the low-temperature performance is poor; comparative example 3 uses ethylene propylene diene monomer 8570C, which has low molecular weight and high ethylene content, resulting in ethylene propylene diene monomer compositions having significantly lower low temperature performance, compression set and oil resistance than those of the ethylene propylene diene monomer compositions of examples 1-3; comparative example 4 uses clay instead of willitin V85, resulting in compression set and reduced oil resistance of the compound. The technical index of the ethylene propylene diene monomer rubber composition completely meets the technical index requirement, has excellent low temperature and oil resistance, has excellent physical and mechanical properties, does not generate aminolysis reaction, and ensures the bursting property of the rubber hose.
Claims (10)
1. An environment-friendly oil-resistant ethylene propylene rubber composition for a light-colored rubber tube is characterized in that: the composite material is prepared from the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 2-5 parts of zinc oxide, 1-3 parts of stearic acid, 150-230 parts of inorganic filler, 0-5 parts of silane coupling agent, 40-120 parts of paraffin oil, 2-4 parts of anti-aging agent, 0-2 parts of vulcanizing agent and 3-8 parts of accelerator.
2. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 1, wherein: the composite material is prepared from the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 2-5 parts of zinc oxide, 1-3 parts of stearic acid, 150-230 parts of inorganic filler, 2-5 parts of silane coupling agent, 60-80 parts of paraffin oil, 2-4 parts of anti-aging agent, 1-2 parts of sulfur and 3-8 parts of accelerator.
3. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 1 or 2, which is characterized in that: the ethylene propylene diene monomer is long-chain branched ethylene propylene diene monomer, the Mooney viscosity ML (1+8) is 60-70 at 150 ℃, the ethylene content is 50-70%, and the ENB content is 5-10%.
4. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 1 or 2, which is characterized in that: the inorganic filler is one or a combination of more of silicon powder Sillitin V85, silicon powder VM56 and titanium dioxide; the anti-aging agent is one or a combination of more of anti-aging agent TNP, anti-aging agent ZMTI and anti-aging agent 445.
5. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 4, wherein: the inorganic filler is a combination of (2-3): 1 by weight of the silicon powder Sillitin V85, the silicon powder VM56 and the titanium pigment; the anti-aging agent is a combination of an anti-aging agent TNP, an anti-aging agent ZMTI and an anti-aging agent 445 in a weight ratio of 1:1:1.
6. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 1 or 2, which is characterized in that: the silane coupling agent is silane coupling agent A151, silane coupling agent SI69 and silane coupling agent A172.
7. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 1 or 2, which is characterized in that: the paraffin oil is YP5002.
8. The environmentally friendly oil resistant ethylene propylene rubber composition for light rubber hose according to claim 1 or 2, which is characterized in that: the vulcanizing agent is sulfur S-80; the accelerator is a comprehensive accelerator LHG-80.
9. A method for preparing the environment-friendly oil-resistant ethylene propylene rubber composition for light-colored rubber tubes, which is characterized in that: the method comprises the following steps:
setting the initial temperature of an internal mixer to 55 ℃ and the rotating speed of a rotor to 30r/min, firstly adding ethylene propylene diene monomer into the internal mixer, banburying for 30s, then adding zinc oxide, stearic acid and an anti-aging agent, banburying for 60s, then adding a silane coupling agent, an inorganic filler which is half of the total weight and paraffin oil which is half of the total weight, banburying for 4-6 min, then adding the rest inorganic filler and paraffin oil, continuously mixing, discharging rubber when the temperature of the internal mixer is increased to 130 ℃, transferring to an open rubber mixer for thin-pass sheet discharging, and cooling to room temperature to obtain master batch;
step (2), putting the masterbatch prepared in the step (1) into an internal mixer, adding a vulcanizing agent and an accelerator at the temperature of 85 ℃, discharging the masterbatch when the temperature of the internal mixer is increased to 105 ℃, and thinning out the masterbatch to obtain ethylene propylene diene monomer rubber compound;
and (3) placing the ethylene propylene diene monomer rubber compound into a plate vulcanizing machine, and vulcanizing for 30min at 160+/-3 ℃ to obtain the ethylene propylene diene monomer rubber composition.
10. The utility model provides a light-colored rubber tube which characterized in that: the environment-friendly oil-resistant ethylene propylene rubber composition for the light-colored rubber tube is used as an inner rubber layer and an outer rubber layer, the ethylene propylene rubber composition is extruded on a steel core through an extruder to obtain a tube blank, the tube blank with a core rod is put into a braiding machine, a 1500D polyester wire is adopted for braiding to form a polyester reinforcing layer, the ethylene propylene rubber composition is coated on the braided tube through the extruder, and the rubber tube product is obtained through vulcanization and core pulling.
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