CN113861572A - Low-temperature-resistant water stop rubber material and preparation method thereof - Google Patents
Low-temperature-resistant water stop rubber material and preparation method thereof Download PDFInfo
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- CN113861572A CN113861572A CN202111207848.8A CN202111207848A CN113861572A CN 113861572 A CN113861572 A CN 113861572A CN 202111207848 A CN202111207848 A CN 202111207848A CN 113861572 A CN113861572 A CN 113861572A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 150
- 239000005060 rubber Substances 0.000 title claims abstract description 149
- 239000000463 material Substances 0.000 title claims abstract description 132
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 68
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 67
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 65
- 239000004945 silicone rubber Substances 0.000 claims abstract description 57
- 239000006229 carbon black Substances 0.000 claims abstract description 43
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 41
- 150000002978 peroxides Chemical class 0.000 claims abstract description 40
- 239000004014 plasticizer Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 239000012936 vulcanization activator Substances 0.000 claims abstract description 33
- BMFMTNROJASFBW-UHFFFAOYSA-N 2-(furan-2-ylmethylsulfinyl)acetic acid Chemical compound OC(=O)CS(=O)CC1=CC=CO1 BMFMTNROJASFBW-UHFFFAOYSA-N 0.000 claims abstract description 25
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 21
- 230000003078 antioxidant effect Effects 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 16
- 238000004073 vulcanization Methods 0.000 claims description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 claims description 11
- MIMDHDXOBDPUQW-UHFFFAOYSA-N dioctyl decanedioate Chemical group CCCCCCCCOC(=O)CCCCCCCCC(=O)OCCCCCCCC MIMDHDXOBDPUQW-UHFFFAOYSA-N 0.000 claims description 10
- 239000012190 activator Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims 1
- 125000002081 peroxide group Chemical group 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 6
- YARNEMCKJLFQHG-UHFFFAOYSA-N prop-1-ene;styrene Chemical group CC=C.C=CC1=CC=CC=C1 YARNEMCKJLFQHG-UHFFFAOYSA-N 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 6
- -1 ethylene, propylene Chemical group 0.000 description 6
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 150000001993 dienes Chemical class 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229930195734 saturated hydrocarbon Natural products 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- NYMPGSQKHIOWIO-UHFFFAOYSA-N hydroxy(diphenyl)silicon Chemical group C=1C=CC=CC=1[Si](O)C1=CC=CC=C1 NYMPGSQKHIOWIO-UHFFFAOYSA-N 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000005489 elastic deformation Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a low-temperature-resistant water stop rubber material and a preparation method thereof, wherein the low-temperature-resistant water stop rubber material comprises the following components in parts by weight: 70-80 parts of ethylene propylene diene monomer, 30-40 parts of low phenyl silicone rubber, 3-5 parts of zinc methacrylate, 1-3 parts of a vulcanization activator, 1-3 parts of an anti-aging agent, 60-80 parts of carbon black, 5-7 parts of a peroxide crosslinking agent and 1-3 parts of a plasticizer. The preparation method comprises the steps of plasticating ethylene propylene diene monomer after weighing each component, adding low phenyl silicone rubber for mixing, then adding other components in sequence for mixing, then mixing, rolling, discharging and vulcanizing to obtain the low phenyl ethylene propylene diene monomer. The low-temperature-resistant water stop rubber material is compounded by low-phenyl silicone rubber and ethylene propylene diene monomer rubber with good low-temperature resistance, and the water stop made of the obtained rubber material has good mechanical properties such as tear resistance, wear resistance and the like, and also has good aging resistance, high temperature resistance and particularly good low-temperature resistance.
Description
Technical Field
The invention belongs to the technical field of new rubber material preparation, and particularly relates to a low-temperature-resistant waterstop rubber material and a preparation method thereof.
Background
With the rapid development of economy in China, the water stop belt is widely applied to deformation joint water stop in projects such as water conservancy projects, hydropower projects, dam culverts, tunnel subways, civil air defence works, basements of high-rise buildings, parking lots and the like. The rubber water stop is embedded in the deformation joint when concrete is poured, is connected with the concrete into a whole, utilizes the elastic deformation of rubber, thereby exerting the fastening and sealing performance, being used on the permanent joint and the peripheral joint of an underground foundation, a tunnel project, a bridge and the like, playing the roles of fastening and sealing, preventing the water leakage and water seepage of a building component, absorbing shock and buffering and ensuring the service life of the engineering building component.
However, with the development of society, people put forward higher requirements on the performance of the water stop, and in addition, the use environment of the water stop is complex and changeable, the use environment temperature of the water stop is lower in some cold regions, such as regions close to polar regions, high-altitude regions and winter in northern regions with large day-night temperature difference, and the low temperature resistance of the existing water stop cannot meet the requirements, so that the application of the existing water stop is limited.
Therefore, the above problems need to be solved.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide the low-temperature-resistant water stop rubber material and the preparation method thereof, and the water stop made of the obtained rubber material has good mechanical properties such as tear resistance, wear resistance and the like, and also has good aging resistance, high temperature resistance and particularly good low-temperature resistance.
The technical scheme is as follows: in order to achieve the purpose, the invention provides a low-temperature-resistant water stop rubber material which comprises the following components in percentage by weight: 70-80 parts of ethylene propylene diene monomer, 30-40 parts of low phenyl silicone rubber, 3-5 parts of zinc methacrylate, 1-3 parts of a vulcanization activator, 1-3 parts of an anti-aging agent, 60-80 parts of carbon black, 5-7 parts of a peroxide crosslinking agent and 1-3 parts of a plasticizer. The low-temperature-resistant water stop rubber material is compounded by adopting the low-phenyl silicone rubber and the ethylene propylene diene monomer rubber with good low-temperature resistance, and the water stop made of the obtained rubber material has good mechanical properties such as tear resistance, wear resistance and the like, and also has good aging resistance, high temperature resistance and particularly good low-temperature resistance.
Further, in the low-temperature-resistant water stop rubber material, the ethylene propylene diene monomer rubber has an ethylene propylene ratio of 50/50. The low-temperature-resistant water stop rubber material is characterized in that ethylene propylene diene monomer is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, is one of ethylene propylene rubbers, and has excellent ozone resistance, heat resistance, weather resistance and other aging resistance because a main chain of the ethylene propylene rubber material consists of chemically stable saturated hydrocarbon and only contains unsaturated double bonds in side chains, so that the low-temperature-resistant water stop rubber material has a wide application temperature range and the lowest use temperature of-40 to-60 ℃. The ethylene propylene ratio of the common ethylene propylene diene monomer is 80/20-50/50, and when the ethylene ratio in the ethylene propylene diene monomer is gradually increased, the low-temperature property of the ethylene propylene diene monomer is gradually deteriorated.
Further, in the low temperature resistant water stop rubber material, the vulcanization activator is selected from zinc oxide or stearic acid.
Further, in the low-temperature-resistant water stop rubber material, the antioxidant is any one selected from the group consisting of antioxidant D, antioxidant A, antioxidant RD and antioxidant AW.
Further, in the low-temperature-resistant water stop rubber material, the carbon black is selected from any one of carbon black N330 and carbon black N220.
Further, in the low-temperature-resistant water stop rubber material, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, in the low-temperature-resistant water stop rubber material, the plasticizer is dioctyl sebacate. In the low-temperature-resistant water stop rubber material, dioctyl sebacate belongs to aliphatic dibasic acid ester cold-resistant plasticizers, and the plasticizer belongs to a plasticizer taking linear methylene as a main body, and can keep the movement among polymer molecular chains at a low temperature, so that the low-temperature-resistant water stop rubber material has good cold resistance, excellent low-temperature performance, strong impact resistance, high plasticizing efficiency and good viscosity. And the rubber water stop is not easy to freeze at a low temperature state, so that the rubber water stop has excellent compatibility with rubber, molecules of a rubber material have a lubricating effect, the rubber material keeps better elasticity in an extremely cold area due to good flexibility, and the rubber water stop has good elasticity and makes up for the defects of the traditional water stop.
Further, in the low-temperature-resistant water stop rubber material, the phenyl content of the low-phenyl silicone rubber is C6H5and/Si is 6-11%. The low-temperature-resistant water stop rubber material disclosed by the invention has the advantages that the phenyl is introduced on the basis of the silicon rubber, the high-temperature resistance and the low-temperature resistance of the silicon rubber can be improved, the low-temperature resistance of the silicon rubber is good, the silicon rubber can still work at the temperature of-55 ℃, and the temperature can reach-73 ℃ after the phenyl is introduced; methyl phenyl vinyl silicone rubber is abbreviated as phenyl silicone rubber. The rubber is obtained by introducing diphenyl siloxane chain segments or methyl phenyl siloxane chain segments into the molecular chain of vinyl silicone rubber. The phenyl content of the low-phenyl silicone rubber is C6H5When the content of the phenyl group is increased, the rigidity of the molecular chain is increased, and the cold resistance and elasticity are reduced.
Further, the preparation method of the low-temperature-resistant water stop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 70-80 parts of ethylene propylene diene monomer, 30-40 parts of low phenyl silicone rubber, 3-5 parts of zinc methacrylate, 1-3 parts of a vulcanization activator, 1-3 parts of an anti-aging agent, 60-80 parts of carbon black, 5-7 parts of a peroxide crosslinking agent and 1-3 parts of a plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 0.5-1.5 MPa, and the plastication lasts for 5-9 minutes;
thirdly, adding low-phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 3-7 minutes at the temperature of 85 +/-5 ℃ and the pressure of 0.5-1.5 MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer rubber and the low phenyl silicone rubber, and continuously mixing for 2-4 minutes; adding a vulcanization activator, and continuously mixing for 1-3 minutes;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the low-temperature-resistant water stop rubber material.
Further, the vulcanization condition of the low-temperature-resistant water stop rubber material is 10MPa and 170 ℃ for 10 min.
The technical scheme shows that the invention has the following beneficial effects:
1. the ethylene propylene diene monomer rubber adopted by the low-temperature-resistant water stop rubber material is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, is one of ethylene propylene rubbers, and has excellent aging resistance such as ozone resistance, heat resistance, weather resistance and the like because the main chain of the ethylene propylene rubber is composed of chemically stable saturated hydrocarbon and only contains unsaturated double bonds in the side chain, the application temperature range is wide, and the lowest use temperature is-40 to-60 ℃.
2. The silicone rubber is a linear polymer with main molecular chain mainly comprising Si-O bond and side group as organic group (mainly methyl), and is a high molecular elastomer with both inorganic and organic properties. Because the Si-O bond energy of the main chain is much higher than the C-C bond energy of the main chain of a common rubber molecule, the silicon rubber has excellent heat resistance, elasticity, cold resistance, excellent mold release property, electrical property, air permeability, heat conductivity, waterproofness and good temperature stability. The introduction of the phenyl can improve the high and low temperature resistance of the silicon rubber, the low temperature resistance of the silicon rubber is good, the silicon rubber can still work at the temperature of minus 55 ℃, and the temperature can reach minus 73 ℃ after the phenyl is introduced. The low-phenyl silicone rubber adopted by the low-temperature-resistant waterstop rubber material is obtained by introducing diphenyl siloxane chain links or methyl phenyl siloxane chain links into the molecular chain of vinyl silicone rubber. The phenyl content of the low-phenyl silicone rubber is C6H5the/Si is 6-11%, and the water stop made of the rubber material has good mechanical properties such as tear resistance, wear resistance and the like, and also has good aging resistance, high temperature resistance and particularly good low temperature resistance by compounding the low phenyl silicone rubber and the ethylene propylene diene monomer rubber with good low temperature resistance.
3. The dioctyl sebacate adopted by the low-temperature-resistant water stop rubber material belongs to aliphatic dibasic acid ester cold-resistant plasticizers, belongs to plasticizers taking linear methylene as a main body, and can keep the movement among polymer molecular chains at a low temperature, so that the low-temperature-resistant water stop rubber material has good cold resistance, excellent low-temperature performance, strong impact resistance, high plasticizing efficiency and good viscosity. And the rubber water stop is not easy to freeze at a low temperature state, so that the rubber water stop has excellent compatibility with rubber, molecules of a rubber material have a lubricating effect, the rubber material keeps better elasticity in an extremely cold area due to good flexibility, and the rubber water stop has good elasticity and makes up for the defects of the traditional water stop.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments and specific experimental data, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The low-temperature-resistant water stop rubber material comprises the following components in parts by weight: 70 parts of ethylene propylene diene monomer, 30 parts of low phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 1 part of anti-aging agent, 60 parts of carbon black, 5 parts of peroxide crosslinking agent and 1 part of plasticizer.
Wherein the ethylene propylene diene monomer has an ethylene propylene ratio of 50/50.
And the vulcanization activator is zinc oxide.
The antioxidant is antioxidant D.
And the carbon black is carbon black N220.
Further, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, the plasticizer is dioctyl sebacate.
And the phenyl content of the low phenyl silicone rubber is C6H5/Si＝6～11％。
The preparation method of the low-temperature-resistant water stop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 70 parts of ethylene propylene diene monomer, 30 parts of low phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 1 part of anti-aging agent, 60 parts of carbon black, 5 parts of peroxide crosslinking agent and 1 part of plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal rubber mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 0.5MPa, and the plastication lasts for 5 minutes;
thirdly, adding low phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 3 minutes at the temperature of 85 +/-5 ℃ and under the pressure of 0.5MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer rubber and the low phenyl silicone rubber, and continuously mixing for 2 minutes; adding a vulcanization activator, and continuously mixing for 1 minute;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the low-temperature-resistant water stop rubber material.
Wherein the vulcanization condition is vulcanization for 10min under the conditions of 10MPa and 170 ℃.
Example 2
The low-temperature-resistant water stop rubber material comprises the following components in parts by weight: 80 parts of ethylene propylene diene monomer, 40 parts of low phenyl silicone rubber, 5 parts of zinc methacrylate, 3 parts of a vulcanization activator, 3 parts of an anti-aging agent, 80 parts of carbon black, 7 parts of a peroxide crosslinking agent and 3 parts of a plasticizer.
Wherein the ethylene propylene diene monomer has an ethylene propylene ratio of 50/50.
And the vulcanization activator is stearic acid.
The antioxidant is AW.
And the carbon black is carbon black N220.
Further, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, the plasticizer is dioctyl sebacate.
And the phenyl content of the low phenyl silicone rubber is C6H5/Si＝11％。
The preparation method of the low-temperature-resistant water stop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 80 parts of ethylene propylene diene monomer, 40 parts of low phenyl silicone rubber, 5 parts of zinc methacrylate, 3 parts of a vulcanization activator, 3 parts of an anti-aging agent, 80 parts of carbon black, 7 parts of a peroxide crosslinking agent and 3 parts of a plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal rubber mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 1.5MPa, and the plastication lasts for 9 minutes;
thirdly, adding low phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 7 minutes at the temperature of 85 +/-5 ℃ and under the pressure of 1.5MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer rubber and the low phenyl silicone rubber, and continuously mixing for 4 minutes; adding a vulcanization activator, and continuously mixing for 3 minutes;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the low-temperature-resistant water stop rubber material.
Wherein the vulcanization condition is vulcanization for 10min under the conditions of 10MPa and 170 ℃.
Example 3
The low-temperature-resistant water stop rubber material comprises the following components in parts by weight: 75 parts of ethylene propylene diene monomer, 35 parts of low phenyl silicone rubber, 4 parts of zinc methacrylate, 2 parts of a vulcanization activator, 2 parts of an anti-aging agent, 70 parts of carbon black, 6 parts of a peroxide crosslinking agent and 2 parts of a plasticizer.
Wherein the ethylene propylene diene monomer has an ethylene propylene ratio of 50/50.
And the vulcanization activator is zinc oxide.
The antioxidant is antioxidant RD.
And the carbon black is carbon black N330.
Further, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, the plasticizer is dioctyl sebacate.
And the phenyl content of the low phenyl silicone rubber is C6H5/Si＝8％。
The preparation method of the low-temperature-resistant water stop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 75 parts of ethylene propylene diene monomer, 35 parts of low phenyl silicone rubber, 4 parts of zinc methacrylate, 2 parts of a vulcanization activator, 2 parts of an anti-aging agent, 70 parts of carbon black, 6 parts of a peroxide crosslinking agent and 2 parts of a plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal rubber mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 1MPa, and the plastication lasts for 7 minutes;
thirdly, adding low phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 5 minutes at the temperature of 85 +/-5 ℃ and under the pressure of 1MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer rubber and the low phenyl silicone rubber, and continuously mixing for 3 minutes; adding a vulcanization activator, and continuously mixing for 2 minutes;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the low-temperature-resistant water stop rubber material.
Wherein the vulcanization condition is vulcanization for 10min under the conditions of 10MPa and 170 ℃.
Example 4
The low-temperature-resistant water stop rubber material comprises the following components in parts by weight: 70 parts of ethylene propylene diene monomer, 40 parts of low phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 3 parts of anti-aging agent, 70 parts of carbon black, 6 parts of peroxide crosslinking agent and 2 parts of plasticizer.
Wherein the ethylene propylene diene monomer has an ethylene propylene ratio of 50/50.
And the vulcanization activator is stearic acid.
The antioxidant is antioxidant A.
And the carbon black is carbon black N220.
Further, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, the plasticizer is dioctyl sebacate.
And the phenyl content of the low phenyl silicone rubber is C6H5/Si＝9％。
The preparation method of the low-temperature-resistant water stop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 70 parts of ethylene propylene diene monomer, 40 parts of low phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 3 parts of anti-aging agent, 70 parts of carbon black, 6 parts of peroxide crosslinking agent and 2 parts of plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal rubber mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 1.5MPa, and the plastication lasts for 5 minutes;
thirdly, adding low phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 5 minutes at the temperature of 85 +/-5 ℃ and under the pressure of 1.2MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer rubber and the low phenyl silicone rubber, and continuously mixing for 4 minutes; adding a vulcanization activator, and continuously mixing for 2 minutes;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the low-temperature-resistant water stop rubber material.
Wherein the vulcanization condition is vulcanization for 10min under the conditions of 10MPa and 170 ℃.
Comparative example 1
The water stop rubber material comprises the following components in parts by weight: 70 parts of ethylene propylene diene monomer, 30 parts of phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 1 part of anti-aging agent, 60 parts of carbon black, 5 parts of peroxide crosslinking agent and 1 part of plasticizer.
Wherein the ethylene propylene diene monomer has an ethylene propylene ratio of 50/50.
And the vulcanization activator is zinc oxide.
The antioxidant is antioxidant D.
And the carbon black is carbon black N220.
Further, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, the plasticizer is dioctyl sebacate.
And the phenyl silicone rubber has a phenyl content of C6H5/Si＝20％。
The preparation method of the waterstop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 70 parts of ethylene propylene diene monomer, 30 parts of phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 1 part of anti-aging agent, 60 parts of carbon black, 5 parts of peroxide crosslinking agent and 1 part of plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal rubber mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 0.5MPa, and the plastication lasts for 5 minutes;
thirdly, adding phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 3 minutes at the temperature of 85 +/-5 ℃ and under the pressure of 0.5MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer and the phenyl silicone rubber, and continuously mixing for 2 minutes; adding a vulcanization activator, and continuously mixing for 1 minute;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the water stop rubber material.
Wherein the vulcanization condition is vulcanization for 10min under the conditions of 10MPa and 170 ℃.
Comparative example 2
The water stop rubber material comprises the following components in parts by weight: 70 parts of ethylene propylene diene monomer, 30 parts of phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 1 part of anti-aging agent, 60 parts of carbon black, 5 parts of peroxide crosslinking agent and 1 part of plasticizer.
Wherein the ethylene propylene diene monomer has an ethylene propylene ratio of 80/20.
And the vulcanization activator is zinc oxide.
The antioxidant is antioxidant D.
And the carbon black is carbon black N220.
Further, the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
Further, the plasticizer is dioctyl sebacate.
And the phenyl silicone rubber has a phenyl content of C6H5/Si＝6％。
The preparation method of the waterstop rubber material comprises the following steps:
weighing the following raw materials in parts by weight: 70 parts of ethylene propylene diene monomer, 30 parts of phenyl silicone rubber, 3 parts of zinc methacrylate, 1 part of vulcanization activator, 1 part of anti-aging agent, 60 parts of carbon black, 5 parts of peroxide crosslinking agent and 1 part of plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal rubber mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 0.5MPa, and the plastication lasts for 5 minutes;
thirdly, adding phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 3 minutes at the temperature of 85 +/-5 ℃ and under the pressure of 0.5MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer and the phenyl silicone rubber, and continuously mixing for 2 minutes; adding a vulcanization activator, and continuously mixing for 1 minute;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the water stop rubber material.
Wherein the vulcanization condition is vulcanization for 10min under the conditions of 10MPa and 170 ℃.
Test example
The physical properties of the products of examples 1-4 and comparative examples 1-2 of the present invention were tested by GB/18173.2-2014, and the test results are shown in Table 1.
TABLE 1 results of testing the properties of the inventive and comparative examples
As can be seen from Table 1, the low temperature resistant rubber material for waterstops obtained in examples 1 to 4 has good physical properties such as hardness, tensile strength, elongation and the like, meets the national standard requirements, has a brittle temperature far lower than the national standard requirements, and has good low temperature resistance.
The phenyl silicone rubber used in comparative example 1 is a medium phenyl silicone rubber with a phenyl content of 20%, and the phenyl silicone rubber is obtained by introducing diphenylsiloxane chain units or methylphenylsiloxane chain units into the molecular chain of vinyl silicone rubber; with the increase of the content of phenyl, the rigidity of a silicon rubber molecular chain is gradually increased, the flame resistance and the radiation resistance of vulcanized rubber are correspondingly improved, but the low-temperature resistance of the silicon rubber is gradually reduced, and the low-temperature resistance of a product is poorer.
The ethylene propylene diene rubber used in comparative example 2 has an ethylene propylene ratio of 80/20, the ethylene propylene diene rubber is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, and is one of ethylene propylene rubbers, the main chain of the ethylene propylene diene rubber is composed of chemically stable saturated hydrocarbons, only unsaturated double bonds are contained in side chains, the ethylene propylene ratio of the commonly used ethylene propylene diene rubber ranges from 80/20 to 50/50, and when the ethylene ratio in the ethylene propylene diene rubber is gradually increased, the low-temperature characteristic of the ethylene propylene diene rubber gradually becomes poor, and the low-temperature resistance of the product is poor.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. The low-temperature-resistant waterstop rubber material is characterized by comprising the following components in parts by weight: 70-80 parts of ethylene propylene diene monomer, 30-40 parts of low phenyl silicone rubber, 3-5 parts of zinc methacrylate, 1-3 parts of a vulcanization activator, 1-3 parts of an anti-aging agent, 60-80 parts of carbon black, 5-7 parts of a peroxide crosslinking agent and 1-3 parts of a plasticizer.
2. The low temperature resistant water stop rubber material according to claim 1, wherein the ethylene propylene diene monomer rubber has an ethylene propylene ratio of 50/50.
3. The low temperature-resistant water stop rubber material according to claim 1, wherein the vulcanization activator is selected from zinc oxide or stearic acid.
4. The low temperature-resistant water stop rubber material according to claim 1, wherein the antioxidant is any one selected from the group consisting of antioxidant D, antioxidant A, antioxidant RD and antioxidant AW.
5. The low temperature-resistant water stop rubber material according to claim 1, wherein the carbon black is selected from any one of carbon black N330 and carbon black N220.
6. The low temperature resistant water stop rubber material according to claim 1, wherein the peroxide crosslinking agent is a peroxide crosslinking agent BIBP.
7. The low temperature-resistant water stop rubber material according to claim 1, wherein the plasticizer is dioctyl sebacate.
8. The low temperature-resistant water stop rubber material according to claim 1, wherein the phenyl content of the low phenyl silicone rubber is C6H5/Si=6~11%。
9. The method for preparing the low temperature-resistant water stop rubber material according to claim 1, comprising the following steps of:
weighing the following raw materials in parts by weight: 70-80 parts of ethylene propylene diene monomer, 30-40 parts of low phenyl silicone rubber, 3-5 parts of zinc methacrylate, 1-3 parts of a vulcanization activator, 1-3 parts of an anti-aging agent, 60-80 parts of carbon black, 5-7 parts of a peroxide crosslinking agent and 1-3 parts of a plasticizer;
secondly, putting the ethylene propylene diene monomer rubber into an internal mixer for plastication, wherein the temperature of the internal mixer is 95 +/-5 ℃, the pressure is 0.5-1.5 MPa, and the plastication lasts for 5-9 minutes;
thirdly, adding low-phenyl silicone rubber into the plasticated ethylene propylene diene monomer, and mixing for 3-7 minutes at the temperature of 85 +/-5 ℃ and the pressure of 0.5-1.5 MPa in an internal mixer;
adding zinc methacrylate, an anti-aging agent, carbon black, a peroxide crosslinking agent and a plasticizer into the mixed rubber material of the ethylene propylene diene monomer rubber and the low phenyl silicone rubber, and continuously mixing for 2-4 minutes; adding a vulcanization activator, and continuously mixing for 1-3 minutes;
cooling the mixed rubber material added with the vulcanizing activator for 2 hours, placing the cooled mixed rubber material on an open mill, making a triangular bag, thinly passing the mixed rubber material, uniformly mixing the mixed rubber material and the rubber material, and discharging the mixed rubber material;
sixthly, vulcanizing the flaky rubber material obtained in the fifth step, taking out and cooling to room temperature to obtain the low-temperature-resistant water stop rubber material.
10. The low temperature-resistant water stop rubber material according to claim 9, wherein the vulcanization condition is 10min at 170 ℃ under 10 MPa.
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| CN116041864A (en) * | 2022-12-29 | 2023-05-02 | 四川铁拓科技有限公司 | Cold-resistant rubber water stop suitable for cold region and preparation method thereof |
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