CN111234388A - High-temperature-resistant low-pressure-change radiator water pipe material vulcanized by sulfur system and preparation method thereof - Google Patents
High-temperature-resistant low-pressure-change radiator water pipe material vulcanized by sulfur system and preparation method thereof Download PDFInfo
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- CN111234388A CN111234388A CN201811438078.6A CN201811438078A CN111234388A CN 111234388 A CN111234388 A CN 111234388A CN 201811438078 A CN201811438078 A CN 201811438078A CN 111234388 A CN111234388 A CN 111234388A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 67
- 239000011593 sulfur Substances 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 35
- 239000005662 Paraffin oil Substances 0.000 claims abstract description 24
- 239000011787 zinc oxide Substances 0.000 claims abstract description 23
- 239000006229 carbon black Substances 0.000 claims abstract description 21
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 14
- 239000011256 inorganic filler Substances 0.000 claims abstract description 14
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 14
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 14
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008117 stearic acid Substances 0.000 claims abstract description 14
- 229960002447 thiram Drugs 0.000 claims abstract description 14
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 6
- 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 claims abstract description 5
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 4
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 4
- 229920001971 elastomer Polymers 0.000 claims description 50
- 238000007599 discharging Methods 0.000 claims description 21
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000012752 auxiliary agent Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000002131 composite material Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 230000003712 anti-aging effect Effects 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 229940053200 antiepileptics fatty acid derivative Drugs 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- DUEPRVBVGDRKAG-UHFFFAOYSA-N carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2 DUEPRVBVGDRKAG-UHFFFAOYSA-N 0.000 claims description 2
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 2
- 239000011863 silicon-based powder Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 14
- 238000004073 vulcanization Methods 0.000 description 27
- 230000032683 aging Effects 0.000 description 14
- 238000001125 extrusion Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000010059 sulfur vulcanization Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- IUJLOAKJZQBENM-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)-2-methylpropan-2-amine Chemical compound C1=CC=C2SC(SNC(C)(C)C)=NC2=C1 IUJLOAKJZQBENM-UHFFFAOYSA-N 0.000 description 3
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 2
- ZNRLMGFXSPUZNR-UHFFFAOYSA-N 2,2,4-trimethyl-1h-quinoline Chemical compound C1=CC=C2C(C)=CC(C)(C)NC2=C1 ZNRLMGFXSPUZNR-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 description 2
- 238000010060 peroxide vulcanization Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- DFWCPLGXFMSUCW-UHFFFAOYSA-N 3-(dimethylamino)propyl carbamimidothioate;hydron;dichloride Chemical compound Cl.Cl.CN(C)CCCSC(N)=N DFWCPLGXFMSUCW-UHFFFAOYSA-N 0.000 description 1
- CPGFMWPQXUXQRX-UHFFFAOYSA-N 3-amino-3-(4-fluorophenyl)propanoic acid Chemical compound OC(=O)CC(N)C1=CC=C(F)C=C1 CPGFMWPQXUXQRX-UHFFFAOYSA-N 0.000 description 1
- QRYFCNPYGUORTK-UHFFFAOYSA-N 4-(1,3-benzothiazol-2-yldisulfanyl)morpholine Chemical compound C1COCCN1SSC1=NC2=CC=CC=C2S1 QRYFCNPYGUORTK-UHFFFAOYSA-N 0.000 description 1
- HLBZWYXLQJQBKU-UHFFFAOYSA-N 4-(morpholin-4-yldisulfanyl)morpholine Chemical compound C1COCCN1SSN1CCOCC1 HLBZWYXLQJQBKU-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 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
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
- RKQOSDAEEGPRER-UHFFFAOYSA-L zinc diethyldithiocarbamate Chemical compound [Zn+2].CCN(CC)C([S-])=S.CCN(CC)C([S-])=S RKQOSDAEEGPRER-UHFFFAOYSA-L 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
A high temperature resistant and low pressure change resistant radiator water pipe material vulcanized by a sulfur system and a preparation method thereof are disclosed, wherein the preparation raw materials of the material comprise: ethylene propylene diene monomer A: 40-100 parts by weight of ethylene propylene diene monomer B: 0-105 parts by weight of carbon black: 100-160 parts by weight of an inorganic filler: 0-50 parts by weight, paraffin oil: 30-100 parts by weight of zinc oxide: 2-15 parts by weight of stearic acid: 1-2 parts by weight of an antioxidant: 2-5.0 parts by weight, sulfur: 0 to 1.0 part by weight, a sulfur donor: 0-2.5 parts by weight, a thiuram accelerator: 1-2.5 parts by weight, carbamate and derivative accelerator: 2.0-5.0 parts by weight of a sulfenamide accelerator: 0 to 2.5 parts by weight of other additives and 1 to 5 parts by weight of other additives. The preparation method of the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system is also provided, and the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system is obtained by adjusting the proportion of the raw materials according to proper raw materials.
Description
Technical Field
The invention relates to the technical field of automobile radiator water pipe materials, in particular to a high temperature (125 ℃) and low pressure change (compression permanent deformation: 125 ℃ 72h is less than or equal to 50%) radiator water pipe material vulcanized by a sulfur system and a preparation method thereof. The ethylene propylene rubber material mainly replaces part of peroxide vulcanized ethylene propylene rubber materials, and can effectively reduce production energy consumption, accelerate vulcanization time, improve processing performance and promote cost to be reasonable on the basis of meeting the performance.
Background
The cooling system of the automobile engine mainly comprises a radiator, a matched water pipe and the like. With the diversification of automobile functions and the compactification of the structure, the contact temperature of the inner layer and the outer layer of a radiator water pipe is higher and higher, and the requirements cannot be met by the conventional 100 ℃ long-time use and 125 ℃ short-time use. In order to meet the long-time use requirement of 125 ℃, more and more radiator water pipes use ethylene propylene rubber materials of peroxide vulcanization systems, so that the requirements of heat resistance and pressure change can be met more easily. Correspondingly, the production energy consumption is improved because steam deoxygenation vulcanization is required, the production efficiency is reduced because microwave vulcanization cannot be carried out or the vulcanization time is reduced, and the dynamic performance and the like of the ethylene propylene rubber are not the same as those of the ethylene propylene rubber of a sulfur vulcanization system.
At present, various standards of radiator water pipe materials are established in various automobile main engine factories, and the technical standards similar to the long-time aging at 125 ℃ are as follows: a2 and B2 specifications of FISHITE 9.02136/01 standard (requiring 125 ℃ X336 h aging and 125 ℃ X72 h voltage change), Volkswagen TL680 standard (requiring 120 ℃ X504 h aging and 120 ℃ X22 h PV voltage change), Dawler DBL6254 standard 11/15/20 specification (requiring 125 ℃ X1008 h aging and 125 ℃ X72 h voltage change), general GME13001 standard P specification (requiring 150 ℃ X168 h aging and 125 ℃ X70 h voltage change), and GMW15024 standard A/C/D specification (requiring 150 ℃ X168 h aging and 125 ℃ X70 h voltage change). Other devices such as walvo, toyota, honda, modern and some domestic automobile host plants have similar technical standards. Compared with ethylene propylene rubber of a sulfur vulcanization system, the technical indexes are strict, but the production cost is increased by adopting the ethylene propylene rubber of a peroxide vulcanization system.
The existing radiator water pipe material vulcanized by a conventional sulfur system is mainly matched with general ethylene propylene rubber, carbon black, inorganic filler, moderate-quantity sulfur, thiazole accelerant and other assistants, and cannot meet the long-time aging and pressure change requirements at 125 ℃. The ethylene-propylene rubber composite material partially meeting the performance requirements is mainly matched by measures of reducing the content of paraffin oil, adding a quick accelerator, replacing ethylene-propylene rubber with high ENB content and the like, and has the advantages of high rubber content, short scorching time, high Mooney viscosity, difficult actual production and use due to factors including outlet control chemical substances and the like or certain use risk. The radiator water pipe material in actual production needs to be manufactured into a product through the working procedures of extrusion, vulcanization (steam tank vulcanization, electric heating air vulcanization and the like), drying tunnel assembly, mould pressing assembly and the like, so that good processability is needed. It is mainly reflected on technical indexes such as T10, T90, Mooney viscosity and the like of a vulcanization curve.
In order to solve the problems, the ethylene-propylene rubber composite material of a sulfur vulcanization system needs to be developed and can meet the requirements in the aspects of cost performance, high temperature resistance, long-time aging, low pressure change, processability, hazardous substance control and the like. In actual technical indexes and application, the selected ethylene-propylene rubber composite material must have the performances of meeting the technical index performance, good extrusion manufacturability and good vulcanization manufacturability. Therefore, it is necessary to develop a new radiator water pipe material with high temperature resistance and low pressure change resistance for sulfur system vulcanization.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized in a sulfur system, which has excellent performance, proper cost performance, good processing and long service life, and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that: a high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by a sulfur system comprises the following raw materials in parts by weight: ethylene propylene diene monomer A: 40-100 parts by weight of ethylene propylene diene monomer B: 0-105 parts by weight of carbon black: 100-160 parts by weight of an inorganic filler: 0-50 parts by weight, paraffin oil: 30-100 parts by weight of zinc oxide: 2-15 parts by weight of stearic acid: 1-2 parts by weight of an antioxidant: 2-5.0 parts by weight, sulfur: 0 to 1.0 part by weight, a sulfur donor: 0-2.5 parts by weight, a thiuram accelerator: 1-2.5 parts by weight, carbamate and derivative accelerator: 2.0-5.0 parts by weight of a sulfenamide accelerator: 0 to 2.5 parts by weight of other additives and 1 to 5 parts by weight of other additives.
The ethylene propylene diene monomer A is ethylene propylene diene monomer with Mooney viscosity ML (1+4) at 125 ℃ of 75-85, ethylene content of 50-60%, ENB content of 5-6% and oil charge of 0. The method mainly improves the extrusion performance of the ethylene propylene rubber composite material and balances physical and mechanical properties, vulcanization efficiency, cost performance and the like.
The ethylene-propylene-diene monomer rubber B is ethylene-propylene-diene monomer rubber with Mooney viscosity ML (1+4) at 125 ℃ of 45-55, ethylene content of 60-70%, ENB content of 4-5% and oil-extended portion of 75. The material mainly improves the pressure-variable performance and the processing performance, and avoids the defects that the pressure-variable performance is not met due to excessive addition of paraffin oil and the extrusion performance is deteriorated due to insufficient addition of paraffin oil when ethylene propylene diene monomer A is used simply, so that the material can complement the ethylene propylene diene monomer A and improve the performance of the material together through mutual cooperation. In addition, the oil-extended part is limited to 75 parts, and the performance can be improved compared with the performance only by adding paraffin oil into the rubber compound composite material.
The carbon black of the invention is one or a combination of several of N550, N762 and N774. It can effectively balance physical and mechanical properties, definite elongation, pressure change, cost performance, processability and the like.
The inorganic filler of the invention is one or the combination of two of silicon powder and carbofuran powder. The silica powder is a natural combination of granular quartz and platy kaolin, and has good affinity with rubber after surface modification treatment, and the extrusion performance is improved on the basis of ensuring certain physical reinforcing performance. The Qianwei powder is a nano silicate sheet-structured filler, and can improve the extrusion performance of rubber materials on the basis of certain reinforcement.
The paraffin oil is one or a combination of more of high flash point paraffin oil 2280, 2240 and T16. The ethylene propylene diene monomer has good compatibility with ethylene propylene diene monomer, can be highly filled, has good heat resistance, and is not easy to generate volatile substances to cause product failure.
The zinc oxide is indirect zinc oxide. It is used in combination with stearic acid to produce complexing matter, activating promoter and other matter, so as to raise the sulfurizing speed. Meanwhile, the heat resistance of the ethylene propylene diene monomer composite material can be effectively improved by increasing the content of zinc oxide.
The anti-aging agent is one or the combination of two of RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer) and MB (2-mercaptobenzimidazole).
Preferably, the RD: 0-2.0 parts by weight, MB: 0 to 3 parts by weight, and the mass ratio of the two is 1:1 to 2. The limitation of the two kinds and the limitation of the proportion can generate a synergistic effect, further improve the heat aging resistance and have good cost performance.
The sulfur donor is one or a combination of more of DTDM (4,4 '-dithiodimorpholine), DTDC (1, 1' -dithiobiscaprolactam) and MDB (2- (4-morpholinyl dithio) benzothiazole). DTDM is a commonly used sulfur donor, and has low price and high vulcanization efficiency. DTDC, being somewhat expensive, does not produce controlled chemicals. MDB, the price is general, and the smell is small during vulcanization; DTDM is mostly adopted, and if the requirement on odor is severe, MDB is used as a sulfur donor.
The thiuram accelerator of the present invention is one or a combination of two of TMTD (tetramethylthiuram disulfide) and DPTT (dipentamethylenethiuram tetrasulfide). TMTD is a commonly used thiuram type accelerator with low cost, and tends to cause precipitation of substances during vulcanization. DPTT is slightly expensive, the vulcanization speed is higher, and the addition amount of the DPTT can be slightly increased. The combination of the two can effectively prevent the precipitation of microcrystalline substances and improve the vulcanization speed.
The carbamate and derivative accelerator of the present invention is one or a combination of two of BZ (zinc dibutyldithiocarbamate) and EZ (zinc diethyldithiocarbamate). When the sulfur donor content is large (about 2.5 belongs to a large amount), and the thiuram type accelerator is used as a main accelerator, the vulcanization speed is slow, and the vulcanization speed can be effectively improved by adding the carbamate and the derivative type accelerator in a matching way. The sulfur donor of the present invention is preferably contained in an amount of 1.5 to 2.5 parts by weight. The BZ accelerator has a high vulcanization speed, can effectively accelerate the decomposition reaction of a thiuram accelerator, but has a scorching risk, and the EZ accelerator has a low vulcanization speed and can balance the defects of the BZ accelerator.
The sulfenamide accelerator is one or a combination of two of CZ (N-cyclohexyl-2-benzothiazole sulfenamide) and NS (N-tertiary butyl-2-benzothiazole sulfenamide). The rapid reaction brought by carbamate and derivative accelerators in the initial vulcanization stage can be balanced, so that the safety of the ethylene propylene diene monomer composite material during extrusion is improved.
The other auxiliary agents are one or a combination of more of silane coupling agents SI69, polyethylene glycol PEG400 and fatty acid derivatives WB 42. The silane coupling agent can improve the affinity of the inorganic filler and rubber and prevent the inorganic filler from being dispersed unevenly. The polyethylene glycol balances the acid-base balance degree of the sizing material, reduces the waste of the accelerant and gives certain lubricating property. The fatty acid derivative mainly improves the external lubricating property of the rubber material, prevents the rubber material from self-adhering when the rubber material is mixed and stripped, and improves the extrusion speed.
The invention also provides a preparation method of the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system, which comprises the following preparation steps:
(1) preparing a rubber compound: preparing raw materials according to a formula proportion, and sequentially putting ethylene propylene diene monomer, other auxiliary agents, an anti-aging agent, zinc oxide, stearic acid, an inorganic filler, carbon black and paraffin oil into an internal mixer, wherein the rubber discharging temperature is 130-150 ℃, and the time is 2-4 min;
(2) preparation of a two-stage rubber compound: and filtering the first-stage rubber compound, standing at room temperature for 16 hours after filtering, putting into an internal mixer, adding other raw materials such as sulfur, sulfur donor, thiuram accelerators and the like, discharging rubber at 100-120 ℃ for 0.5-1 min, and discharging rubber and obtaining the ethylene-propylene rubber composite material.
The specific adding sequence of the invention can realize better dispersion of various components, the ethylene propylene diene monomer is added firstly for plastication to improve the wrapping property of the material, otherwise, the ethylene propylene diene monomer cannot be fully contacted with carbon black and the like to increase the mixing effect. Other auxiliary agents, zinc oxide and the like are added later because the rubber has no great chemical reaction and is difficult to disperse in the rubber, the rubber can be better dispersed when the auxiliary agents and the zinc oxide are added first, and compared with other auxiliary agents, the mixing time of the auxiliary agents and the zinc oxide is longer; the other principle is the same, namely adding the mixture before dispersing the mixture, adding the mixture after dispersing the mixture easily, and adding the mixture finally after chemical reaction.
The invention has the advantages and excellent effects that:
1. according to the invention, through proper raw materials and adjustment of the proportion of the raw materials, the performance of the raw materials is synergistically promoted, so that the high-temperature-resistant low-pressure-change radiator water pipe material for sulfur system vulcanization is obtained, and the material has the performances of 125 ℃ long-time aging resistance, low pressure change resistance, high fixed elongation, excellent processability and the like.
2. The invention finally obtains the radiator water pipe material which meets the requirements of long-time aging resistance at 125 ℃, low pressure change, high fixed elongation, excellent processability and the like by using a new vulcanization system, particularly by matching sulfur with a specific kind of sulfur donor and simultaneously limiting the specification performance and the dosage proportion of the ethylene propylene diene monomer crude rubber, the carbon black, the zinc oxide, the anti-aging agent and the like.
3. The peroxide curing system in the prior art needs steam oxygen-discharging curing in boiler curing, and the energy consumption is increased. The technical scheme of the invention adopts a sulfur vulcanization system instead of steam oxygen-discharging vulcanization. Different from the existing mould pressing mode, the invention is steam vulcanization after extrusion, the raw rubber of the invention can not contain a large amount of oil-extended ethylene-propylene rubber, and simultaneously, the carbon black system adopts carbon black with medium grain diameter, does not need N330 to increase the mechanical property, and has better mechanical property. The mixing process does not adopt a back-mixing process method but adopts a two-stage process method, the mixing time is short, and the scorching risk is avoided.
4. The method of the invention needs extrusion production, so the extrusion performance can be obviously improved by adding the paraffin oil, and the processing performance is poorer if the part of the paraffin oil is less, so the part of the paraffin oil added by the invention is very critical; in addition, the invention mainly adopts a sulfur vulcanization system, and the sulfur is not added as an auxiliary effect but is a very key sulfur system.
5. The invention has higher heat-resistant grade and excellent comprehensive performance; the aging resistance of the invention is 125 ℃ for 336h and 150 ℃ for 168 h; the invention comprehensively considers the properties of product smell, production process and the like; the method of the invention has a proposal that sulfur-free donors and only a small amount of sulfur are used as vulcanizing agents, MDB sulfur donors are used as vulcanizing agents, and the proposal mainly aims at improving the product odor and simultaneously has various auxiliary agents such as fatty acid derivatives and the like to improve the processing performance and the like; in addition, the plasticizer content is higher, the extrusion performance can be effectively improved, and the corresponding pressure-variable performance is improved from a filler system and a vulcanization system; the invention does not adopt PZ accelerant because the vulcanization speed of the accelerant is too high, the accelerant has adverse effect on extrusion, has the risk of extruding dead glue and is not suitable for the water pipe process extrusion; moreover, the PZ frosting is very severe, and the product appearance is greatly influenced; in addition, the content of the antioxidant and zinc oxide is also very critical.
Detailed description of the preferred embodiments
The present invention will be described in further detail below by way of examples, but the present invention is not limited to only the following examples.
Example 1:
a high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system comprises the following components in parts by weight:
ethylene propylene diene monomer A: 100 carbon black 550: 120
Carbon black N762: 40 paraffin oil 2280: 90
Zinc oxide: 8, stearic acid: 1
Anti-aging agent RD: 1 antiager MB:2
Sulfur: 0.7 accelerator TMTD: 1.2
Accelerator EZ: 3.5 Accelerator CZ:1
The preparation method of the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system comprises the following steps of:
(1) preparing a rubber compound: preparing materials according to the formula of claim 1, and sequentially putting ethylene propylene diene monomer, other auxiliary agents, an anti-aging agent, zinc oxide, stearic acid, an inorganic filler, carbon black and paraffin oil into an internal mixer, wherein the rubber discharging temperature is 130-150 ℃, and the time is 2-4 min. (ii) a
(2) Preparation of a two-stage rubber compound: and filtering the first-stage rubber compound, standing at room temperature for 16 hours after filtering, putting into an internal mixer, adding sulfur, a sulfur donor, a thiuram accelerator and the like, discharging rubber at 100-120 ℃ for 0.5-1 min, and discharging rubber and obtaining the ethylene-propylene rubber composite material.
Example 2:
a high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system comprises the following components in parts by weight:
ethylene propylene diene monomer A: 100 carbon black 550: 150
Paraffin oil T16: 70 PEG 4000: 1.5
Zinc oxide: 5, stearic acid: 1
Sulfur donor DTDC: 2, promoter TMTD: 1.5
Accelerator BZ: 3.0
The preparation method of the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system comprises the following steps of:
(1) preparing a rubber compound: preparing materials according to the formula of claim 1, and sequentially putting ethylene propylene diene monomer, other auxiliary agents, an anti-aging agent, zinc oxide, stearic acid, an inorganic filler, carbon black and paraffin oil into an internal mixer, wherein the rubber discharging temperature is 130-150 ℃, and the time is 2-4 min. (ii) a
(2) Preparation of a two-stage rubber compound: and filtering the first-stage rubber compound, standing at room temperature for 16 hours after filtering, putting into an internal mixer, adding sulfur, a sulfur donor, a thiuram accelerator and the like, discharging rubber at 100-120 ℃ for 0.5-1 min, and discharging rubber and obtaining the ethylene-propylene rubber composite material.
Example 3:
a high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system comprises the following components in parts by weight:
ethylene propylene diene monomer A: 60 ethylene propylene diene monomer B: 70
Carbon black N550: 120 silica powder: 40
Paraffin oil 2280: 90 coupling agent SI 69: 2
Zinc oxide: 10, stearic acid: 1.5
Anti-aging agent RD: 1.5 antioxidant MB:3
Sulfur: 0.2 sulfur donor MDB; 2
Accelerator TMTD: 0.5 accelerator DPTT: 1.0
Accelerator BZ: 2.5 Accelerator NS:1
The preparation method of the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system comprises the following steps of:
(1) preparing a rubber compound: preparing materials according to the formula of claim 1, and sequentially putting ethylene propylene diene monomer, other auxiliary agents, an anti-aging agent, zinc oxide, stearic acid, an inorganic filler, carbon black and paraffin oil into an internal mixer, wherein the rubber discharging temperature is 130-150 ℃, and the time is 2-4 min. (ii) a
(2) Preparation of a two-stage rubber compound: filtering the first-stage rubber compound, standing at room temperature for 16h after filtering, putting into an internal mixer, adding sulfur, sulfur donor, thiuram accelerator and the like, wherein the rubber discharging temperature is 100-120 ℃, the time is 0.5-1 min, and discharging rubber and obtaining the ethylene-propylene rubber composite material after sheet discharging
Example 4:
a high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system comprises the following components in parts by weight:
ethylene propylene diene monomer A: 40 ethylene propylene diene monomer B: 105
Carbon black N550: 140 siliconized powder: 20
Paraffin oil 2280: 50 parts of zinc oxide: 10
Stearic acid: 1.5 Sulfur: 0.3
Sulfur donor DTDM: 2, promoter TMTD: 1.5
Accelerator DPTT: 1.0 accelerator BZ: 3.5
The preparation method of the high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by the sulfur system comprises the following steps of:
(1) preparing a rubber compound: preparing materials according to the formula of claim 1, and sequentially putting ethylene propylene diene monomer, other auxiliary agents, an anti-aging agent, zinc oxide, stearic acid, an inorganic filler, carbon black and paraffin oil into an internal mixer, wherein the rubber discharging temperature is 130-150 ℃, and the time is 2-4 min. (ii) a
(2) Preparation of a two-stage rubber compound: and filtering the first-stage rubber compound, standing at room temperature for 16 hours after filtering, putting into an internal mixer, adding sulfur, a sulfur donor, a thiuram accelerator and the like, discharging rubber at 100-120 ℃ for 0.5-1 min, and discharging rubber and obtaining the ethylene-propylene rubber composite material.
The rubber materials obtained in examples 1 to 4 were subjected to property tests, and the test results are shown in the following table 1:
TABLE 1 Performance parameters of the samples of examples 1-4
According to the experimental data, the proper raw materials are selected, the proportion of the raw materials is adjusted, the performance of the raw materials is synergistically promoted, and the obtained automobile radiator water pipe outer layer material with high temperature resistance and long-time aging resistance has excellent performances of high temperature resistance and long-time hot air aging resistance, low compression permanent deformation, high stretching resistance, low temperature resistance and the like. Meanwhile, the product has the properties of small smell, improved fatigue performance and the like.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The high temperature resistant and low pressure variable radiator water pipe material vulcanized by a sulfur system is characterized in that: the preparation raw materials of the material comprise the following components in parts by weight: ethylene propylene diene monomer A: 40-100 parts by weight of ethylene propylene diene monomer B: 0-105 parts by weight of carbon black: 100-160 parts by weight of an inorganic filler: 0-50 parts by weight, paraffin oil: 30-100 parts by weight of zinc oxide: 2-15 parts by weight of stearic acid: 1-2 parts by weight of an antioxidant: 2-5.0 parts by weight, sulfur: 0 to 1.0 part by weight, a sulfur donor: 0-2.5 parts by weight, a thiuram accelerator: 1-2.5 parts by weight, carbamate and derivative accelerator: 2.0-5.0 parts by weight of a sulfenamide accelerator: 0 to 2.5 parts by weight of other additives and 1 to 5 parts by weight of other additives.
2. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the ethylene propylene diene monomer A is ethylene propylene diene monomer with Mooney viscosity ML (1+4) at 125 ℃ of 75-85, ethylene content of 50-60%, ENB content of 5-6% and oil charge of 0; the ethylene-propylene-diene monomer B is ethylene-propylene-diene monomer with Mooney viscosity ML (1+4) at 125 ℃ of 45-55, ethylene content of 60-70%, ENB content of 4-5% and oil charge of 75%.
3. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the carbon black is one or a combination of several of N550, N762 and N774; the inorganic filler is one or the combination of two of silicon powder and carbofuran powder; the paraffin oil is one or a combination of more of high flash point paraffin oil 2280, 2240 and T16; the zinc oxide is indirect zinc oxide.
4. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the anti-aging agent is one or the combination of two of RD and MB.
5. The high temperature and low pressure resistant radiator water pipe material vulcanized by a sulfur system according to claim 4, which is characterized in that: the RD: 0-2.0 parts by weight, MB: 0 to 3 parts by weight, and the mass ratio of the two is 1:1 to 2.
6. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the sulfur donor is one or a combination of DTDM, DTDC and MDB.
7. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the thiuram accelerator is one or the combination of TMTD and DPTT.
8. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the carbamate and the derivative accelerator are one or a combination of two of BZ and EZ.
9. The high-temperature-resistant low-pressure-change-resistant radiator water pipe material vulcanized by a sulfur system according to claim 1, which is characterized in that: the sulfenamide accelerator is one or a combination of CZ and NS; the other auxiliary agents are one or a combination of more of silane coupling agents SI69, polyethylene glycol PEG400 and fatty acid derivatives WB 42.
10. A preparation method of a high-temperature-resistant low-pressure-change radiator water pipe material vulcanized by a sulfur system is characterized by comprising the following steps of: the preparation method comprises the following steps:
(1) preparing a rubber compound: preparing raw materials according to a formula proportion, and sequentially putting ethylene propylene diene monomer, other auxiliary agents, an anti-aging agent, zinc oxide, stearic acid, an inorganic filler, carbon black and paraffin oil into an internal mixer, wherein the rubber discharging temperature is 130-150 ℃, and the time is 2-4 min;
(2) preparation of a two-stage rubber compound: and filtering the first-stage rubber compound, standing at room temperature for 16 hours after filtering, putting into an internal mixer, adding other raw materials such as sulfur, sulfur donor, thiuram accelerators and the like, discharging rubber at 100-120 ℃ for 0.5-1 min, and discharging rubber and obtaining the ethylene-propylene rubber composite material.
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