CN115230266B - Multi-layer structure wide-temperature-range oil-resistant sealing product and preparation method and application thereof - Google Patents
Multi-layer structure wide-temperature-range oil-resistant sealing product and preparation method and application thereof Download PDFInfo
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- CN115230266B CN115230266B CN202110438822.8A CN202110438822A CN115230266B CN 115230266 B CN115230266 B CN 115230266B CN 202110438822 A CN202110438822 A CN 202110438822A CN 115230266 B CN115230266 B CN 115230266B
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- elastomer
- rubber
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- resistant
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- 238000007789 sealing Methods 0.000 title claims abstract description 45
- 239000010742 number 1 fuel oil Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229920001971 elastomer Polymers 0.000 claims abstract description 149
- 239000000806 elastomer Substances 0.000 claims abstract description 93
- 239000005060 rubber Substances 0.000 claims abstract description 56
- 150000001875 compounds Chemical class 0.000 claims abstract description 41
- 238000002156 mixing Methods 0.000 claims abstract description 34
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000003921 oil Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 20
- 238000004073 vulcanization Methods 0.000 claims abstract description 20
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 18
- 150000002367 halogens Chemical class 0.000 claims abstract description 18
- 239000007924 injection Substances 0.000 claims abstract description 9
- 238000002347 injection Methods 0.000 claims abstract description 8
- 150000002978 peroxides Chemical class 0.000 claims abstract description 6
- 230000001360 synchronised effect Effects 0.000 claims abstract description 4
- 150000003464 sulfur compounds Chemical class 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 52
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000006229 carbon black Substances 0.000 claims description 14
- 238000007599 discharging Methods 0.000 claims description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- OUBMGJOQLXMSNT-UHFFFAOYSA-N N-isopropyl-N'-phenyl-p-phenylenediamine Chemical compound C1=CC(NC(C)C)=CC=C1NC1=CC=CC=C1 OUBMGJOQLXMSNT-UHFFFAOYSA-N 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 235000021355 Stearic acid Nutrition 0.000 claims description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 11
- 230000003078 antioxidant effect Effects 0.000 claims description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 11
- 239000008117 stearic acid Substances 0.000 claims description 11
- 229910052717 sulfur Inorganic materials 0.000 claims description 11
- 239000011593 sulfur Substances 0.000 claims description 11
- 239000011787 zinc oxide Substances 0.000 claims description 11
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 10
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 10
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 10
- 230000003712 anti-aging effect Effects 0.000 claims description 10
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 8
- 238000001746 injection moulding Methods 0.000 claims description 8
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 claims description 7
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims description 7
- 238000010074 rubber mixing Methods 0.000 claims description 7
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 claims description 6
- IPJGAEWUPXWFPL-UHFFFAOYSA-N 1-[3-(2,5-dioxopyrrol-1-yl)phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC(N2C(C=CC2=O)=O)=C1 IPJGAEWUPXWFPL-UHFFFAOYSA-N 0.000 claims description 6
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 6
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 6
- 229920001973 fluoroelastomer Polymers 0.000 claims description 6
- 229920005560 fluorosilicone rubber Polymers 0.000 claims description 6
- 229920001084 poly(chloroprene) Polymers 0.000 claims description 6
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 claims description 5
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 5
- 244000043261 Hevea brasiliensis Species 0.000 claims description 5
- 239000005062 Polybutadiene Substances 0.000 claims description 5
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- 229920003052 natural elastomer Polymers 0.000 claims description 5
- 229920001194 natural rubber Polymers 0.000 claims description 5
- 229920002857 polybutadiene Polymers 0.000 claims description 5
- 229960002447 thiram Drugs 0.000 claims description 5
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 5
- 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 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- 229920002681 hypalon Polymers 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- LZDOYVMSNJBLIM-UHFFFAOYSA-N 4-tert-butylphenol;formaldehyde Chemical compound O=C.CC(C)(C)C1=CC=C(O)C=C1 LZDOYVMSNJBLIM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004709 Chlorinated polyethylene Substances 0.000 claims description 3
- KEQFTVQCIQJIQW-UHFFFAOYSA-N N-Phenyl-2-naphthylamine Chemical compound C=1C=C2C=CC=CC2=CC=1NC1=CC=CC=C1 KEQFTVQCIQJIQW-UHFFFAOYSA-N 0.000 claims description 3
- 229920000459 Nitrile rubber Polymers 0.000 claims description 3
- 229920005557 bromobutyl Polymers 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920002379 silicone rubber Polymers 0.000 claims description 3
- 239000004945 silicone rubber Substances 0.000 claims description 3
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 3
- 239000003784 tall oil Substances 0.000 claims description 3
- KPAPHODVWOVUJL-UHFFFAOYSA-N 1-benzofuran;1h-indene Chemical compound C1=CC=C2CC=CC2=C1.C1=CC=C2OC=CC2=C1 KPAPHODVWOVUJL-UHFFFAOYSA-N 0.000 claims description 2
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims description 2
- 229920006228 ethylene acrylate copolymer Polymers 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- NEYNBSGIXOOZGZ-UHFFFAOYSA-L zinc;butoxymethanedithioate Chemical compound [Zn+2].CCCCOC([S-])=S.CCCCOC([S-])=S NEYNBSGIXOOZGZ-UHFFFAOYSA-L 0.000 claims description 2
- PGNWIWKMXVDXHP-UHFFFAOYSA-L zinc;1,3-benzothiazole-2-thiolate Chemical compound [Zn+2].C1=CC=C2SC([S-])=NC2=C1.C1=CC=C2SC([S-])=NC2=C1 PGNWIWKMXVDXHP-UHFFFAOYSA-L 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 24
- 239000010410 layer Substances 0.000 description 103
- 239000000047 product Substances 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 13
- 230000006835 compression Effects 0.000 description 8
- 238000007906 compression Methods 0.000 description 8
- 239000004636 vulcanized rubber Substances 0.000 description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 6
- 230000032683 aging Effects 0.000 description 6
- 229920002725 thermoplastic elastomer Polymers 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/18—Layered products comprising a layer of natural or synthetic rubber comprising butyl or halobutyl rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/042—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of natural rubber or synthetic rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/08—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/12—Layered products comprising a layer of natural or synthetic rubber comprising natural rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/14—Layered products comprising a layer of natural or synthetic rubber comprising synthetic rubber copolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/16—Layered products comprising a layer of natural or synthetic rubber comprising polydienes homopolymers or poly-halodienes homopolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
Landscapes
- Sealing Material Composition (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a preparation method of a multi-layer structure wide-temperature-range oil-resistant sealing product, which uses a high-temperature-resistant and oil-resistant elastomer as an outer layer of the multi-layer structure, uses tackifying resin and a halogen-containing elastomer as a co-vulcanization bonding layer in an intermediate layer, uses a low-temperature-resistant elastomer material in an inner layer, uses a peroxide and sulfur compound vulcanization system to crosslink, and prepares the multi-layer structure wide-temperature-range oil-resistant sealing product through synchronous vulcanization. Mixing the outer layer elastomer, the filler and the auxiliary agent to obtain an outer layer elastomer mixed rubber; mixing the halogen elastomer, tackifying resin, filler and auxiliary agent to obtain intermediate layer elastomer mixed rubber; mixing the inner-layer low-temperature-resistant elastomer, the filler and the auxiliary agent to obtain inner-layer elastomer mixed rubber; and (3) adopting a multilayer injection process to inject and mold the multilayer elastomer rubber compound to prepare the vulcanized multilayer elastomer sealing test piece and the product. The multi-layer sealing product prepared by the method has greatly improved oil resistance and high temperature resistance, and simultaneously retains the low temperature resistance of the inner layer elastomer product.
Description
Technical Field
The invention relates to a multi-layer structure wide-temperature-range oil-resistant sealing product, a preparation method and application thereof, belongs to the rubber processing technology, and particularly relates to a preparation method of a multi-layer structure elastomer mixture and a molding process thereof in multi-layer injection and compression molding.
Background
The performance requirements on high-end products are higher and higher nowadays, and the products are required to have excellent low temperature resistance and certain high temperature resistance and oil resistance. However, the rubber/elastomer material is prepared under the structural and polymerization conditions and cannot have low temperature resistance, oil resistance and high temperature resistance simultaneously, so that a sealing product with low temperature resistance and high temperature resistance and oil resistance simultaneously is urgently needed in the market. The invention takes the low temperature resistant elastomer material as the inner layer, which endows the product with excellent low temperature resistance; the high-temperature-resistant and oil-resistant elastomer is used as an outer layer, so that the product has high-temperature-resistant and oil-resistant properties; the tackifying resin and the halogen-containing elastomer are used as the bonding layer, so that the functional layer is effectively bonded, and the mechanical property of the material is improved; and finally, synchronously vulcanizing the multi-layer material by a coinjection technology to prepare the multi-layer structure wide-temperature-range oil-resistant sealing product. The sealing product prepared by the invention has high temperature resistance, low temperature resistance and oil resistance, and meets the use requirement of high-end products.
Disclosure of Invention
In order to solve the problems existing in the prior art, the invention provides a preparation method of a multi-layer structure wide-temperature-range sealing product.
The invention provides a preparation method of a multi-layer structure wide-temperature-range oil-resistant sealing product, which is characterized in that a high-temperature-resistant and oil-resistant elastomer is used as an outer layer of the multi-layer structure, a tackifying resin and a halogen-containing elastomer are used as a co-vulcanization bonding layer in an intermediate layer, a low-temperature-resistant elastomer material is used as an inner layer, a peroxide and sulfur compound vulcanization system is used for crosslinking, and the multi-layer structure wide-temperature-range oil-resistant sealing product is prepared by synchronous vulcanization (synchronous vulcanization refers to a technical means that the vulcanization dynamics curves of the multi-layer rubber are consistent or the vulcanization processes are consistent through the regulation of the formulas of several layers of rubber).
The preparation method comprises the following steps and conditions of preparing the multi-layer structure wide-temperature-range oil-resistant sealing product:
(a) According to the outer layer elastomer: and (3) filling: active agent: vulcanization accelerators: vulcanizing agent: the mass ratio of the anti-aging agent is 100: 20-100: 3 to 5:1 to 3:1 to 5: 1-3, putting the outer layer elastomer, filler and auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 50-70 ℃ and a rotor rotating speed of 40-60 r/min, and discharging the rubber compound after mixing for 5-10 minutes to obtain the outer layer elastomer rubber compound;
(b) According to halogen-containing elastomers: tackifying resin: and (3) filling: active agent: vulcanization accelerators: vulcanizing agent: the mass ratio of the anti-aging agent is 100: 50-150: 5-20: 3 to 5:1 to 3:1 to 5: 1-3, putting a halogen elastomer, tackifying resin, filler and auxiliary agent into an open rubber mixing mill, mixing at an initial temperature of 40-50 ℃ and a roll spacing of 3-5 mm, and discharging the rubber compound after mixing for 15-20 minutes to obtain an intermediate layer elastomer rubber compound;
(c) According to the inner layer low temperature resistant elastomer: and (3) filling: active agent: vulcanization accelerators: vulcanizing agent: the mass ratio of the anti-aging agent is 100: 20-50: 3 to 5:1 to 3:1 to 5: 1-3, putting the inner-layer low-temperature-resistant elastomer, filler and auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 50-70 ℃ and a rotor rotating speed of 40-60 rpm, and discharging the rubber compound after mixing for 5-10 minutes to obtain an inner-layer elastomer rubber compound;
(d) And (3) adopting a multilayer injection process to perform injection molding on the outer layer, the middle layer and the inner layer elastomer rubber compound layer by layer to obtain multilayer rubber compound, and co-vulcanizing the molded multilayer rubber compound at 135-150 ℃ and 10-15 MPa for 10-30 min to obtain the multilayer structure wide temperature range oil-resistant sealing product.
The outer layer elastomer is Fluororubber (FR), silicone rubber (QR), fluorosilicone rubber (FVMQ), hydrogenated nitrile rubber (HNBR), polyacrylate rubber (ACM) or a mixture of ethylene acrylic ester copolymer (AEM) and filler auxiliary agent;
in the invention, the intermediate layer is a mixture of tackifying resin, halogen-containing elastomer and filler aid;
the inner layer is a mixture of a low-temperature resistant elastomer and a filler auxiliary agent;
the crosslinking system is a peroxide and sulfur biphase composite crosslinking system, and can improve the mechanical property and the ageing resistance of the vulcanized elastomer.
The filler is one or more of carbon black N220, N330, N339, N550, N660, N774, precipitated white carbon 175MP, gas phase white carbon A200 and magnesium oxide;
the active agent is a mixture of zinc oxide and stearic acid, and the mass ratio is 5:0.5 to 3;
the vulcanization accelerators are hexamethylenetetramine/accelerator H, diphenylguanidine/accelerator D, tetramethylthiuram disulfide/accelerator TMTD, 2-mercaptobenzothiazole/accelerator M, zinc dimethyldithiocarbamate/accelerator ZDMC, zinc butylxanthate/accelerator ZBX, N-cyclohexyl-2-benzothiazole sulfenamide/accelerator CZ, ethylene thiourea/accelerator (NA-22) and peroxide accelerator: one or more of triallyl isocyanurate (accelerator TAIC), N' -m-phenylene bismaleimide (HVA 2), trimethylolpropane trimethacrylate (TMPTMA), and the like;
the vulcanizing agent is one or more of sulfur, dicumyl peroxide (DCP), benzoyl Peroxide (BPO), 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane (bis 2-5), di-tert-butyl peroxide (DTBP) and the like;
the antioxidant is one or more of N-phenyl-beta-naphthylamine (antioxidant D), 2, 4-trimethyl-1, 2-dihydroquinoline polymer (antioxidant RD), 2-mercaptobenzimidazole (antioxidant MB), nickel N, N-di-N-butyldithiocarbamate (antioxidant NBC) and N-isopropyl-N' -phenyl-p-phenylenediamine (antioxidant 4010 NA).
The halogen-containing elastomer is one or more of chloroprene rubber, chlorinated polyethylene, chlorosulfonated polyethylene and brominated butyl rubber.
The tackifying resin is one or more of tall oil rosin, esterified rosin, alpha-terpene resin, C5/C9 petroleum resin, coumarone-indene resin, octyl phenolic tackifying resin (203 resin) and p-tertiary butyl phenol formaldehyde resin (2402 resin).
The low temperature resistant elastomer is one or more of butadiene rubber, natural rubber, butadiene-isoprene copolymer, ethylene propylene rubber and styrene butadiene rubber.
The multi-layer structure wide-temperature-range oil-resistant sealing product prepared by the invention can be prepared into various rubber sealing products such as sealing rings, sealing strips, sealing lines, pouring sealants and the like, and has wide application in the fields of aviation, aerospace, high-speed rail, ships and automobiles.
The invention has the beneficial effects that:
according to the multi-layer structure wide-temperature-range oil-resistant sealing product, the high-temperature-resistant and oil-resistant materials of the outer layer, the low-temperature-resistant materials of the inner layer and the middle layer are bonded, and the good oil resistance and high-temperature resistance of the original outer layer material and the excellent low-temperature resistance of the inner layer material are reserved by combining the proportioning ratio and the process conditions. Meanwhile, the multilayer material can integrate the mechanical property advantages of three materials in mechanical property, and has the use effects of wide temperature range (the multilayer material can be used in the temperature range of-50 ℃ to 200 ℃), strong sealing and good mechanical property.
Drawings
FIG. 1 is a schematic diagram of a multi-layer structure wide temperature range oil resistant seal product test strip;
FIG. 2 is a schematic diagram of a multi-layer wide temperature range oil resistant seal product-seal ring structure.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
The manufacturer and model of the closed rubber mixer used in the invention are ML-4.5L of Nanjing Chuanbo mechanical equipment Co., ltd; the manufacturer and model of the open rubber mixing mill are KL-8 of Nanjing Chuangbo mechanical equipment Co. Those skilled in the art can select a suitable device according to actual needs.
The test of the embodiment of the invention is as the national standard test piece size: the specification is 150mm multiplied by 150mm, the total thickness is 2mm, wherein the outer layer is 0.2 mm, the inner layer is 1.4 mm, and the middle layer is 0.1 mm.
The specification of the sealing ring prepared in the embodiment of the invention is as follows according to national standard test standard: the internal diameter is 30+/-0.34 mm, the section diameter is 3.55+/-0.10 mm, and the hydraulic pneumatic O-shaped sealing rings are G series. The thickness of the invention requires that the outer layer accounts for 20 to 35 percent of the total thickness, preferably 25 to 30 percent; the inner layer accounts for 60-75% of the total thickness, preferably 65-70%; the thinner the bonding layer is, the better the bonding effect is, and the thickness of the intermediate layer is about 5 percent.
Those skilled in the art can implement the technical scheme of the invention according to actual needs.
Example 1:
the preparation method comprises the following steps and conditions of preparing the multi-layer structure wide-temperature-range oil-resistant sealing product:
(a) According to Fluororubber (FR): carbon black N330 and precipitated white carbon 175MP (mass ratio 1:2): zinc oxide and stearic acid mixture (mass ratio 5:1): tetramethylthiuram disulfide/accelerator TMTD and triallyl isocyanurate (accelerator TAIC) mixture (mass ratio 1:2): sulfur and dicumyl peroxide (DCP) mixture (mass ratio 1:2): the mass ratio of the N-phenyl-beta-naphthylamine (anti-aging agent D) is 100:20:3:1:1:1, adding an outer layer elastomer, a filler and an auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 50 ℃ at a rotor rotating speed of 40 rpm, and discharging the rubber compound after mixing for 5 minutes to obtain an outer layer elastomer rubber compound;
(b) According to the halogen-containing elastomer neoprene: tall oil rosin: carbon black N660 and magnesia mixture (mass ratio 10:1): zinc oxide and stearic acid mixture (mass ratio 5:2): ethylene thiourea/accelerator (NA-22) and N, N' -m-phenylene bismaleimide (HVA 2) (mass ratio 1:2): sulfur and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5) (mass ratio 1:2): the mass ratio of the 2, 4-trimethyl-1, 2-dihydroquinoline polymer (antioxidant RD) is 100:50:5:3:1:1:1, putting a halogen elastomer, tackifying resin, filler and auxiliary agent into an open rubber mixing mill, mixing at an initial temperature of 40 ℃ and a roll spacing of 3mm, and discharging the rubber compound after mixing for 15 minutes to obtain an intermediate layer elastomer rubber compound;
(c) According to butadiene rubber: carbon black N550 and fumed silica A200 (mass ratio 2:1): zinc oxide and stearic acid mixture (mass ratio 5:2): 2-mercaptobenzothiazole/accelerator M: sulfur and Benzoyl Peroxide (BPO) mixture (mass ratio 1:2): the mass ratio of the 2-thiol benzimidazole (antioxidant MB) is 100:20:3:1:1:1, putting an inner-layer low-temperature-resistant elastomer, a filler and an auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 50 ℃ at a rotor rotating speed of 40 rpm, and discharging the rubber compound after mixing for 5 minutes to obtain an inner-layer elastomer rubber compound;
(d) According to the structures shown in fig. 1 and 2, the outer layer, the intermediate layer and the inner layer elastomer compound were injection molded by a multi-layer injection process, and the molded multi-layer compound was co-vulcanized at 135 ℃ and 10MPa for 30 minutes to prepare vulcanized multi-layer elastomer sealing test pieces and sealing ring products, the properties of which are shown in tables 1 and 2.
Example 2:
the preparation method comprises the following steps and conditions of preparing the multi-layer structure wide-temperature-range oil-resistant sealing product:
(a) Fluorosilicone rubber (FVMQ): carbon black N330 and fumed silica A200 mixture (mass ratio 2:1): zinc oxide and stearic acid mixture (mass ratio 5:0.5): diphenyl guanidine/accelerator D and trimethylolpropane trimethacrylate (TMPTMA) mixture (mass ratio 1:2): sulfur and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5) (mass ratio 1:2): the mass ratio of the N, N-di-N-butyl-nickel dithiocarbamate (anti-aging agent NBC) is 100:40:4:2:3:2, putting the outer layer elastomer, the filler and the auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 60 ℃ at a rotor rotating speed of 50 revolutions per minute, and discharging the rubber compound after mixing for 8 minutes to obtain an outer layer elastomer rubber compound;
(b) According to chlorosulfonated polyethylene: C5/C9 Petroleum resin: precipitation white carbon 175MP: zinc oxide and stearic acid mixture (mass ratio 5:0.5): n-cyclohexyl-2-benzothiazole sulfenamide/accelerator CZ and peroxide accelerator triallyl isocyanurate (accelerator TAIC) mixture (mass ratio 1:1): sulfur and di-tert-butyl peroxide (DTBP) mixture (mass ratio 1:1): the mass ratio of the N-isopropyl-N' -phenyl-p-phenylenediamine (anti-aging agent 4010 NA) is 100:100:15:4:2:3:2, putting the halogen elastomer, tackifying resin, filler and auxiliary agent into an open rubber mixing mill, mixing at an initial temperature of 45 ℃ and a roll spacing of 4mm, and discharging the rubber compound after mixing for 18 minutes to obtain an intermediate layer elastomer rubber compound;
(c) According to the butadiene-isoprene copolymer: n550 and precipitated silica 175MP (mass ratio 1:1): zinc oxide and stearic acid mixture (mass ratio 5:2): tetramethylthiuram disulfide/accelerator TMTD and N, N' -m-phenylene bismaleimide (HVA 2) mixture (mass ratio 1:1): sulfur and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5) mixture (mass ratio 1:1): the mass ratio of the N-isopropyl-N' -phenyl-p-phenylenediamine (anti-aging agent 4010 NA) is 100:30:4:2:4:1, putting an inner-layer low-temperature-resistant elastomer, a filler and an auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 60 ℃ at a rotor rotating speed of 50 revolutions per minute, and discharging rubber compound after mixing for 8 minutes to obtain an inner-layer elastomer rubber compound;
(d) According to the structures shown in fig. 1 and 2, the outer layer, the intermediate layer and the inner layer elastomer compound were injection molded by a multi-layer injection molding process, and the molded multi-layer elastomer compound was co-vulcanized at 145 ℃ and 10MPa for 20 minutes to prepare vulcanized multi-layer elastomer sealing test pieces and products, the properties of which are shown in tables 1 and 2.
Example 3:
the preparation method comprises the following steps and conditions of preparing the multi-layer structure wide-temperature-range oil-resistant sealing product:
(a) According to the outer layer elastomer ethylene acrylate copolymer (AEM): carbon black N330 and N660 mixture (mass ratio 2:1): zinc oxide and stearic acid mixture (mass ratio 5:1): n-cyclohexyl-2-benzothiazole sulfenamide/accelerator CZ and trimethylolpropane trimethacrylate (TMPTMA) mixture (mass ratio 2:1): sulfur and dicumyl peroxide (DCP) mixture (mass ratio 2:1): the mass ratio of the mixture of the antioxidant RD and the antioxidant 4010NA (mass ratio of 1:1) is 100:50:5:2:4:2, putting the outer layer elastomer, the filler and the auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 70 ℃ and a rotor rotating speed of 60 r/min, and discharging the rubber compound after mixing for 10 minutes to obtain an outer layer elastomer rubber compound;
(b) According to the mixture of chloroprene rubber and brominated butyl rubber (mass ratio 2:1): octyl phenolic tackifying resin (203 resin) and p-tert-butylphenol formaldehyde resin (2402 resin) mixture (mass ratio 1:1): carbon black N220, magnesium oxide and precipitated white carbon 175MP mixture (mass ratio 5:1:10): zinc oxide and stearic acid mixture (mass ratio 5:1): ethylene thiourea/accelerator (NA-22) and triallyl isocyanurate (accelerator TAIC) mixture (mass ratio 1:1): sulfur and dicumyl peroxide (DCP) mixture (mass ratio 1:1): the mass ratio of the mixture (mass ratio 1:1) of the 2, 4-trimethyl-1, 2-dihydroquinoline polymer (antioxidant RD) and N-isopropyl-N' -phenyl-p-phenylenediamine (antioxidant 4010 NA) is 100:150:20:5:3:5:3, putting the halogen elastomer, tackifying resin, filler and auxiliary agent into an open rubber mixing mill, mixing at an initial temperature of 50 ℃ and a roll spacing of 5mm, and mixing for 20 minutes, and then mixing the rubber compound to obtain an intermediate layer elastomer rubber compound;
(c) According to the natural rubber and butadiene-isoprene copolymer mixture (mass ratio 1:2): carbon black N330: zinc oxide and stearic acid mixture (mass ratio 5:2): the preparation method comprises the steps of (1) adding a mixture of tetramethylthiuram disulfide/accelerator TMTD and trimethylolpropane trimethacrylate (TMPTMA) (mass ratio 1:1) into a closed rubber mixing machine, mixing an inner low temperature resistant elastomer, a filler and an auxiliary agent at an initial temperature of 70 ℃, a rotor rotating speed of 50 revolutions per minute, and discharging a rubber compound after 8 minutes of mixing, wherein the mass ratio of the mixture of sulphur and a mixture of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane (bis 2-5) (mass ratio 1:1) is 100:30:4:2:4:2;
(d) According to the structures shown in fig. 1 and 2, the outer layer, the intermediate layer and the inner layer elastomer compound were injection molded by a multi-layer injection molding process, and the molded multi-layer elastomer compound was co-vulcanized at 150 ℃ and 10MPa for 30 minutes to prepare vulcanized multi-layer elastomer sealing test pieces and products, the properties of which are shown in tables 1 and 2.
Example 4:
the outer layer of elastomer material was silicone rubber (QR), a mixture of neoprene and chlorinated polyethylene for halogen-containing elastomer (mass ratio 2:1), and a mixture of butadiene rubber and natural rubber for low temperature resistant elastomer (mass ratio 2:1), and the other steps were the same as in example 3, and the properties of the test piece and the gasket product are shown in tables 1 and 2.
Example 5:
the outer layer elastomer material was hydrogenated nitrile rubber (HNBR), a mixture of neoprene and chlorosulfonated polyethylene for halogen-containing elastomer (mass ratio 2:1), and a mixture of butadiene rubber and natural rubber for low temperature resistant elastomer for inner layer (mass ratio 2:1), and the properties of the test piece and seal ring product are shown in Table 1 and Table 2, in the same manner as in example 3.
Example 6:
the outer layer of elastomer material was polyacrylate rubber (ACM), the inner layer of low temperature resistant elastomer was a mixture of butadiene-isoprene copolymer and styrene-butadiene rubber (mass ratio 2:1), and the properties of the test piece and the seal ring product were the same as in example 3 and are shown in tables 1 and 2.
Comparative example 1:
the procedure and process parameters of example 3 were followed, omitting the intermediate elastomer mixture, and injection molding the outer and inner low temperature resistant elastomer mixtures using an injection process, with reference to the structures of fig. 1 and 2, and the properties of the test pieces and seal ring products are shown in tables 1 and 2. The total thickness of the test piece is still 2mm, wherein the outer layer is 0.3 mm, the inner layer is 1.4 mm, the size of the sealing ring is still 30+/-0.34 mm in inner diameter and 3.55+/-0.10 mm in section diameter, and the omitted thickness of the middle layer is increased to the outer layer, so that the size of the sealing ring is unchanged. This comparative example mainly examines the effect of the intermediate layer on the performance of the sealing article.
Comparative example 2:
the procedure and process parameters of example 3 were followed, omitting the intermediate layer elastomer mixture and the inner layer low temperature resistant elastomer mixture, and referring to the structures of fig. 1 and 2, by injection molding the outer layer elastomer compound alone, the properties of the test piece and the seal ring product are shown in tables 1 and 2. The thickness of the test piece is still 2mm, the size of the sealing ring is still 30+/-0.34 mm in inner diameter and 3.55+/-0.10 mm in section diameter, and the performance of the sealing product made of the single outer layer material is mainly examined in the comparative example.
Comparative example 3:
the procedure and process parameters of example 3 were followed, omitting the outer and intermediate elastomer mixes, and referring to the structures of FIGS. 1 and 2, by injection molding the inner low temperature resistant elastomer mix alone, and the properties of the test pieces and seal ring products are shown in tables 1 and 2. The thickness of the test piece is still 2mm, the size of the sealing ring is still 30+/-0.34 mm in inner diameter, and the diameter of the section is 3.55+/-0.10 mm, and the performance of the sealing product made of the single inner layer material is mainly examined in the comparative example.
TABLE 1-1 test piece Properties of examples and comparative examples
| Project | Tensile Strength, MPa | Elongation at break% |
| Example 1 | 16.4 | 329.6 |
| Example 2 | 17.3 | 350.2 |
| Example 3 | 18.4 | 398.0 |
| Comparative example 1 | 17.0 | 331.1 |
| Comparative example 2 | 14.6 | 325.4 |
| Comparative example 3 | 19.9 | 430.5 |
| Example 4 | 15.6 | 342.2 |
| Example 5 | 18.2 | 361.2 |
| Example 6 | 17.9 | 388.0 |
* The physical and mechanical properties are carried out according to the standard 'GB/T528-2009 determination of tensile stress strain properties of vulcanized rubber or thermoplastic rubber', and the cutter is of type I.
Tables 1-2 test piece properties of examples and comparative examples
* The physical and mechanical properties are carried out according to the standard 'GB/T528-2009 determination of tensile stress strain properties of vulcanized rubber or thermoplastic rubber', and the cutter is of type I. The oil field aging test is performed according to the standard GB/T1690-2010 vulcanized rubber or thermoplastic rubber liquid resistance test method;
* The oil resistance is calculated according to the following formula: the tensile strength (MPa) before oil domain aging is multiplied by the elongation at break (%) before oil domain aging is multiplied by 100%/the tensile strength after oil domain aging is multiplied by the elongation at break (%) after oil domain aging is multiplied by the tensile strength at break (%);
* And judging that the oil resistance of the oil field oil resistance test is lower than 85 percent to be intolerant to the type of oil.
Tables 1 to 3 test piece properties of examples and comparative examples
* The high temperature resistance is implemented according to the standard 'GB/T1683-2018 method for measuring constant deformation compression set of vulcanized rubber', the compression amount is 25%, and the temperature is 150 ℃;
* The low temperature resistance was carried out according to the standard "HG/T3866-2006 determination of the compression cold resistance coefficient of vulcanized rubber", at a temperature of-50 ℃.
TABLE 2 sealing ring product Properties of examples and comparative examples
* Testing with a sealing ring product;
* Compression set is carried out according to the standard 'GB/T1683-2018 method for measuring constant deformation compression set of vulcanized rubber', the compression amount is 25%, and the temperature is 200 ℃;
* The compression cold resistance coefficient was carried out according to the standard "HG/T3866-2006 determination of compression cold resistance coefficient of vulcanized rubber", at a temperature of-50 ℃.
From the data comparison of table 1 and table 2, it can be seen that the test piece and the sealing product (O-ring) with the multilayer structure prepared by the invention retain the good oil resistance and high temperature resistance of the original outer layer material and the excellent low temperature resistance of the inner layer material. Meanwhile, the multilayer material can integrate the advantages of the mechanical properties of three materials in mechanical properties, and has the use effects of wide temperature range, strong sealing and good mechanical properties.
The foregoing is merely an embodiment of the present invention and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, expansion, etc. made within the spirit and principle of the present invention are included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the multi-layer structure wide-temperature-range oil-resistant sealing product is characterized in that a high-temperature-resistant and oil-resistant elastomer is used as an outer layer of the multi-layer structure, a tackifying resin and a halogen-containing elastomer are used as co-vulcanization bonding layers in an intermediate layer, a low-temperature-resistant elastomer material is used as an inner layer, and a peroxide and sulfur compound vulcanization crosslinking system is used for preparing the multi-layer structure wide-temperature-range oil-resistant sealing product through synchronous vulcanization of the multi-layer structure;
the steps and conditions are as follows:
(a) According to the outer layer elastomer: and (3) filling: active agent: vulcanization accelerators: vulcanizing agent: the mass ratio of the anti-aging agent is 100: 20-100: 3 to 5: 1-3: 1-5: 1-3, putting the outer layer elastomer, the filler and the auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 50-70 ℃ at a rotor rotating speed of 40-60 r/min, and discharging the rubber compound after mixing for 5-10 minutes to obtain an outer layer elastomer rubber compound;
(b) According to halogen-containing elastomers: tackifying resin: and (3) filling: active agent: vulcanization accelerators: vulcanizing agent: the mass ratio of the anti-aging agent is 100: 50-150: 5-20: 3-5: 1-3: 1-5: 1-3, putting a halogen-containing elastomer, tackifying resin, filler and auxiliary agent into an open rubber mixing mill, mixing at an initial temperature of 40-50 ℃ for 3-5 mm, and discharging the rubber mixture after mixing for 15-20 minutes to obtain an intermediate layer elastomer rubber mixture;
(c) According to the inner layer low temperature resistant elastomer: and (3) filling: active agent: vulcanization accelerators: vulcanizing agent: the mass ratio of the anti-aging agent is 100: 20-50: 3 to 5: 1-3: 1-5: 1-3, putting the inner-layer low-temperature-resistant elastomer, filler and auxiliary agent into an internal rubber mixer, mixing at an initial temperature of 50-70 ℃ at a rotor rotating speed of 40-60 rpm, and discharging the rubber compound after mixing for 5-10 minutes to obtain an inner-layer elastomer rubber compound;
(d) And (3) adopting a multilayer injection process to perform layer-by-layer injection molding on the outer layer, the middle layer and the inner layer elastomer rubber compound to obtain a multilayer rubber compound, and co-vulcanizing the molded multilayer rubber compound for 10-30 min at the temperature of 135-150 ℃ and the pressure of 10-15 MPa to obtain the multilayer structure wide temperature range oil-resistant sealing product.
2. The method of claim 1, wherein the outer layer is a blend of Fluororubber (FR), silicone rubber (QR), fluorosilicone rubber (FVMQ), hydrogenated nitrile rubber (HNBR), polyacrylate rubber (ACM), ethylene acrylate copolymer (AEM), and filler aid.
3. The method according to claim 1, wherein the filler is one or more of carbon black N220, carbon black N330, carbon black N339, carbon black N550, carbon black N660, carbon black N774, precipitated white carbon 175MP, fumed white carbon a200, and magnesium oxide;
the active agent is a mixture of zinc oxide and stearic acid, and the mass ratio is 5: 0.5-3;
the vulcanization accelerator is one or more of hexamethylenetetramine, diphenyl guanidine, tetramethylthiuram disulfide, 2-mercaptobenzothiazole, zinc dimethyldithiocarbamate, zinc butylxanthate, N-cyclohexyl-2-benzothiazole sulfenamide, ethylene thiourea, triallyl isocyanurate (accelerator TAIC), N' -m-phenylene bismaleimide (HVA 2) and trimethylolpropane trimethacrylate (TMPTMA);
the vulcanizing agent is one or more of dicumyl peroxide (DCP), benzoyl Peroxide (BPO), 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane (bis 2-5) or di-tert-butyl peroxide (DTBP) and sulfur;
the antioxidant is one or more of N-phenyl-beta-naphthylamine (antioxidant D), 2, 4-trimethyl-1, 2-dihydroquinoline polymer (antioxidant RD), 2-mercaptobenzimidazole (antioxidant MB), nickel N, N-di-N-butyldithiocarbamate (antioxidant NBC) or N-isopropyl-N' -phenyl-p-phenylenediamine (antioxidant 4010 NA).
4. The method of claim 1, wherein the halogen-containing elastomer is one or more of neoprene, chlorinated polyethylene, chlorosulfonated polyethylene, or brominated butyl rubber;
the tackifying resin is one or more of tall oil rosin, esterified rosin, alpha-terpene resin, C5/C9 petroleum resin, coumarone-indene resin, octyl phenolic tackifying resin (203 resin) or p-tertiary butyl phenol formaldehyde resin (2402 resin);
the low temperature resistant elastomer is one or more of butadiene rubber, natural rubber, butadiene-isoprene copolymer, ethylene propylene rubber or styrene butadiene rubber.
5. The method of claim 1, wherein the multi-layer structured wide temperature range oil resistant seal comprises the following layer thicknesses: the outer layer accounts for 20% -35% of the total thickness; the inner layer accounts for 60% -75% of the total thickness; the thinner the bonding layer is, the better the bonding effect is, and the thickness of the intermediate layer is 5% of the total thickness.
6. The method of claim 5, wherein the outer layer comprises 25% -30% of the total thickness; the inner layer accounts for 65% -70% of the total thickness.
7. A multi-layer structured wide temperature range oil resistant seal made by the method of any one of claims 1-6.
8. Use of the multi-layer structured wide temperature range oil resistant seal of claim 7 as a sealed article.
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| WO2004029493A1 (en) * | 2002-09-25 | 2004-04-08 | Hutchinson | Pipe which is intended, in particular, for an air intake circuit in a motor vehicle engine |
| WO2014002009A2 (en) * | 2012-06-26 | 2014-01-03 | Teklas Kaucuk Sanayi Ve Ticaret Anonim Sirketi | A multi layer hose |
| CN108659282A (en) * | 2018-05-18 | 2018-10-16 | 青岛科技大学 | A kind of wide temperature zone high damping oil resistant yielding rubber composite material and preparation method |
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| WO2004029493A1 (en) * | 2002-09-25 | 2004-04-08 | Hutchinson | Pipe which is intended, in particular, for an air intake circuit in a motor vehicle engine |
| WO2014002009A2 (en) * | 2012-06-26 | 2014-01-03 | Teklas Kaucuk Sanayi Ve Ticaret Anonim Sirketi | A multi layer hose |
| CN108659282A (en) * | 2018-05-18 | 2018-10-16 | 青岛科技大学 | A kind of wide temperature zone high damping oil resistant yielding rubber composite material and preparation method |
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