CN115230266A - Multilayer structure wide-temperature-range oil-resistant sealing product and preparation method and application thereof - Google Patents
Multilayer structure wide-temperature-range oil-resistant sealing product and preparation method and application thereof Download PDFInfo
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- CN115230266A CN115230266A CN202110438822.8A CN202110438822A CN115230266A CN 115230266 A CN115230266 A CN 115230266A CN 202110438822 A CN202110438822 A CN 202110438822A CN 115230266 A CN115230266 A CN 115230266A
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- elastomer
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- SZRLKIKBPASKQH-UHFFFAOYSA-N dibutyldithiocarbamic acid Chemical compound CCCCN(C(S)=S)CCCC SZRLKIKBPASKQH-UHFFFAOYSA-N 0.000 claims description 2
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- NEYNBSGIXOOZGZ-UHFFFAOYSA-L zinc;butoxymethanedithioate Chemical compound [Zn+2].CCCCOC([S-])=S.CCCCOC([S-])=S NEYNBSGIXOOZGZ-UHFFFAOYSA-L 0.000 claims description 2
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 claims description 2
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Images
Classifications
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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 multilayer-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 a multilayer 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 in an inner layer, a peroxide and sulfur compound vulcanization system is used for crosslinking, and the multilayer-structure wide-temperature-range oil-resistant sealing product is prepared through synchronous vulcanization. Mixing the outer-layer elastomer, the filler and the auxiliary agent to obtain outer-layer elastomer rubber compound; mixing the halogen elastomer, tackifying resin, filler and auxiliary agent to obtain an intermediate layer elastomer rubber compound; mixing the inner-layer low-temperature-resistant elastomer, the filler and the auxiliary agent to obtain inner-layer elastomer rubber compound; and (3) performing injection molding on the multilayer elastomer rubber compound by adopting a multilayer injection process to obtain the vulcanized multilayer elastomer sealing test piece and the vulcanized multilayer elastomer sealing product. The oil resistance and the high temperature resistance of the multilayer sealing product prepared by the method are greatly improved, and the low temperature resistance of the inner layer elastomer product is kept.
Description
Technical Field
The invention relates to a multilayer 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 multilayer structure elastomer mixture and a forming process of the multilayer structure elastomer mixture in multilayer injection and mould pressing.
Background
Nowadays, the performance requirements of high-end products are higher and higher, 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 structure and the polymerization condition, and cannot simultaneously have low temperature resistance, oil resistance and high temperature resistance, so that a sealing product which has both low temperature resistance and high temperature resistance and oil resistance is urgently needed in the market. The invention takes the low temperature resistant elastomer material as the inner layer, and endows the product with excellent low temperature resistance; the high-temperature-resistant and oil-resistant elastomer is used as the outer layer, so that the product has high-temperature-resistant and oil-resistant properties; tackifying resin and halogen-containing elastomer are used as adhesive layers to effectively bond the functional layers, so that the mechanical property of the material is improved; and finally, synchronously vulcanizing the multilayer material by a coinjection technology to prepare the multilayer structure wide-temperature-range oil-resistant sealing product. The sealing product prepared by the invention has the performances of high temperature resistance, low temperature resistance and oil resistance, and meets the use requirements of high-end products.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a multilayer wide-temperature-range sealing product.
The invention discloses a preparation method of a multilayer 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 a multilayer structure, a tackifying resin and a halogen-containing elastomer are used as co-vulcanization adhesive layers for an intermediate layer, a low-temperature-resistant elastomer material is used for an inner layer, a peroxide and sulfur compound vulcanization system is used for crosslinking, and the multilayer 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 multilayer structure are consistent or the vulcanization process is consistent by adjusting the formula of several layers of rubber.
Preparing a multilayer wide-temperature-range oil-resistant sealing product, which comprises the following steps and conditions:
(a) According to the outer layer elastomer: filling: active agent(s): vulcanization accelerator (b): vulcanizing agent: the mass ratio of the anti-aging agent is 100:20 to 100:3 to 5:1 to 3:1 to 5: 1-3, putting the outer-layer elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing at the initial temperature of 50-70 ℃ and the rotor rotation speed of 40-60 r/min for 5-10 minutes, and discharging the rubber compound to obtain outer-layer elastomer rubber compound;
(b) According to the halogen-containing elastomer: tackifying resin: filling: active agent(s): vulcanization accelerator (b): vulcanizing agent: the mass ratio of the anti-aging agent is 100:50 to 150:5 to 20:3 to 5:1 to 3:1 to 5: 1-3, putting the halogen elastomer, the tackifying resin, the filler and the auxiliary agent into an open rubber mixing mill, mixing at the initial temperature of 40-50 ℃ for 15-20 minutes at a roller spacing of 3-5 mm, and discharging the rubber mixture to obtain an intermediate layer elastomer rubber mixture;
(c) According to the inner layer low temperature resistant elastomer: filling: active agent(s): vulcanization accelerator (b): vulcanizing agent: the mass ratio of the anti-aging agent is 100:20 to 50:3 to 5:1 to 3:1 to 5: 1-3, putting the inner-layer low-temperature-resistant elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing for 5-10 minutes at the initial temperature of 50-70 ℃ and the rotor speed of 40-60 r/min, and discharging the rubber compound to obtain inner-layer elastomer rubber compound;
(d) And (3) performing injection molding on the elastomer rubber compound of the outer layer, the middle layer and the inner layer by adopting a multilayer injection process to obtain multilayer rubber compound, and co-vulcanizing the molded multilayer rubber compound for 10-30 min at the temperature of 135-150 ℃ and under the pressure of 10-15 MPa to obtain the multilayer-structure wide-temperature-range oil-resistant sealing product.
The outer layer elastomer is a mixture of Fluororubber (FR), silicone rubber (QR), fluorosilicone rubber (FVMQ), hydrogenated nitrile rubber (HNBR), polyacrylate rubber (ACM) or ethylene acrylate copolymer (AEM) and a filler additive;
in the present invention, the intermediate layer is a mixture of a tackifying resin, a halogen-containing elastomer, and a 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 two-phase composite crosslinking system, and can improve the mechanical property and the aging resistance of the vulcanized elastomer at the same time.
The filler is one or more of carbon black N220, N330, N339, N550, N660, N774 and precipitated silica 175MP, fumed silica A200 and magnesium oxide;
the activating agent is a mixture of zinc oxide and stearic acid, and the mass ratio of the activating agent to the stearic acid is 5:0.5 to 3;
the vulcanization accelerator is hexamethylenetetramine/accelerator H, diphenylguanidine/accelerator D, tetramethylthiuram disulfide/accelerator TMTD, 2-thiol benzothiazole/accelerator M, zinc dimethyldithiocarbamate/accelerator ZDMC, zinc butylxanthate/accelerator ZBX, N-cyclohexyl-2-benzothiazole sulfonamide/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 anti-aging agent is one or more of N-phenyl-beta-naphthylamine (anti-aging agent D), 2, 4-trimethyl-1, 2-dihydroquinoline polymer (anti-aging agent RD), 2-thiol benzimidazole (anti-aging agent MB), N, N-di-N-butyl dithio-nickel carbamate (anti-aging agent NBC) and N-isopropyl-N' -phenyl p-phenylenediamine (anti-aging agent 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-tert 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 multilayer-structure wide-temperature-range oil-resistant sealing product prepared by the invention can be made into various rubber sealing products such as sealing rings, sealing strips, sealing lines, pouring sealants and the like, and is widely applied to the fields of aviation, aerospace, high-speed rail, ships and automobiles.
The invention has the beneficial effects that:
according to the multilayer-structure wide-temperature-range oil-resistant sealing product, the high-temperature-resistant and oil-resistant outer layer material, the low-temperature-resistant inner layer material and the middle layer are bonded, and the blending ratio and the process conditions are combined, so that the original good oil resistance and high-temperature resistance of the outer layer material and the original excellent low-temperature resistance of the inner layer material are kept. Meanwhile, the multilayer material can integrate the mechanical property advantages of three materials in the aspect of mechanical property, and has the using effects of wide temperature range (capable of being used in the temperature range of-50 ℃ to 200 ℃), strong sealing and good mechanical property.
Drawings
FIG. 1 is a schematic view of a test strip for a wide temperature range oil-resistant sealing product with a multi-layer structure;
fig. 2 is a schematic structural diagram of a sealing ring of a multi-layer wide-temperature-range oil-resistant sealing product.
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 closed rubber mixing mill used in the invention is produced by a closed rubber mixing mill manufacturer and has a model number of ML-4.5L of Nanjing Chuangbo mechanical equipment Limited company; the open type rubber mixing mill manufacturer and the model thereof are KL-8 of Nanjing Chuangbo mechanical equipment Limited. The skilled person can select suitable equipment according to actual needs.
The test of the embodiment of the invention is the size of a national standard test piece: 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: 30 +/-0.34 mm of inner diameter, 3.55 +/-0.10 mm of section diameter and a hydraulic pneumatic O-shaped sealing ring G series. The thickness of the invention requires that the outer layer accounts for 20-35%, preferably 25-30% of the total thickness; the inner layer accounts for 60 to 75 percent of the total thickness, preferably 65 to 70 percent; the middle layer is an adhesive layer, so that the thinner the adhesive layer is, the better the adhesive effect is, and the adhesive layer accounts for about 5% of the total thickness.
The technical scheme of the invention can be adopted by the technical personnel in the field according to the actual needs.
Example 1:
the preparation method of the multilayer wide-temperature-range oil-resistant sealing product comprises the following steps and conditions:
(a) According to Fluororubber (FR): carbon black N330 and precipitated silica 175MP (mass ratio 1: zinc oxide and stearic acid mixture (mass ratio 5: tetramethylthiuram disulfide/accelerator TMTD and triallyl isocyanurate (accelerator TAIC) mixture (mass ratio 1: sulfur and dicumyl peroxide (DCP) mixture (mass ratio 1: the mass ratio of the N-phenyl-beta-naphthylamine (anti-aging agent D) is 100:20:3:1:1:1, putting an outer-layer elastomer, a filler and an auxiliary agent into an internal rubber mixing mill, mixing at an initial temperature of 50 ℃ and a rotor rotating speed of 40 rpm for 5 minutes, and discharging rubber compound to obtain outer-layer elastomer rubber compound;
(b) According to the halogen-containing elastomer neoprene: tall oil rosin: carbon black N660 and magnesium oxide mixture (mass ratio 10: zinc oxide and stearic acid mixture (mass ratio 5: ethylenethiourea/accelerator (NA-22) and N, N' -m-phenylenebismaleimide (HVA 2) (mass ratio 1: sulfur and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5) (mass ratio 1: 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, a filler and an auxiliary agent into an open rubber mixing mill, mixing at an initial temperature of 40 ℃ and a roll gap of 3mm for 15 minutes, and discharging rubber compound to obtain middle-layer elastomer rubber compound;
(c) According to the weight ratio of the butadiene rubber: carbon black N550 and fumed silica a200 (mass ratio 2: zinc oxide and stearic acid mixture (mass ratio 5: 2-thiol benzothiazole/accelerator M: mixture of sulfur and Benzoyl Peroxide (BPO) (mass ratio 1: the mass ratio of the 2-thiol benzimidazole (anti-aging agent MB) is 100:20:3:1:1:1, putting the inner-layer low-temperature-resistant elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing at the initial temperature of 50 ℃ and the rotor speed of 40 rpm for 5 minutes, and discharging rubber compound to obtain inner-layer elastomer rubber compound;
(d) According to the structure shown in the figures 1 and 2, the outer layer elastomer compound, the middle layer elastomer compound and the inner layer elastomer compound are injected and molded by adopting a multilayer injection process, and the molded multilayer elastomer compound is vulcanized for 30min at the temperature of 135 ℃ and under the pressure of 10MPa to prepare a vulcanized multilayer elastomer sealing test piece and a sealing ring product, wherein the performances of the test piece and the sealing ring product are shown in tables 1 and 2.
Example 2:
preparing a multilayer wide-temperature-range oil-resistant sealing product, which comprises the following steps and conditions:
(a) Fluorosilicone rubber (FVMQ): a mixture of carbon black N330 and fumed silica A200 (mass ratio 2: zinc oxide and stearic acid mixture (mass ratio 5: diphenylguanidine/accelerator D and trimethylolpropane trimethacrylate (TMPTMA) mixture (mass ratio 1: sulfur and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5) (mass ratio 1: the mass ratio of the N, N-di-N-butyl dithiocarbamic acid nickel (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 mixing mill, mixing at the initial temperature of 60 ℃ and the rotor speed of 50 rpm for 8 minutes, and discharging the rubber compound to obtain outer-layer elastomer rubber compound;
(b) According to the formula of chlorosulfonated polyethylene: C5/C9 Petroleum resin: precipitated silica 175MP: zinc oxide and stearic acid mixture (mass ratio 5: n-cyclohexyl-2-benzothiazolesulfenamide/accelerator CZ and peroxide accelerator triallylisocyanurate (accelerator TAIC) mixture (mass ratio 1: sulfur and di-tert-butyl peroxide (DTBP) mixture (mass ratio 1: the mass ratio of N-isopropyl-N' -phenyl p-phenylenediamine (anti-aging agent 4010 NA) is 100:100:15:4:2:3:2, putting the halogen elastomer, the tackifying resin, the filler and the auxiliary agent into an open rubber mixing mill, mixing at the initial temperature of 45 ℃ and the roller spacing of 4mm for 18 minutes, and discharging the rubber compound to obtain an intermediate layer elastomer rubber compound;
(c) According to the butadiene-isoprene copolymer: a mixture of N550 and precipitated silica 175MP (mass ratio 1: zinc oxide and stearic acid mixture (mass ratio 5: tetramethylthiuram disulfide/accelerator TMTD and N, N' -m-phenylene bismaleimide (HVA 2) mixture (mass ratio 1: a mixture of sulfur and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (bis 2-5) (mass ratio 1: the mass ratio of N-isopropyl-N' -phenyl p-phenylenediamine (anti-aging agent 4010 NA) is 100:30:4:2:4:1, putting the inner-layer low-temperature-resistant elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing at the initial temperature of 60 ℃ and the rotor speed of 50 rpm for 8 minutes, and discharging the rubber compound to obtain inner-layer elastomer rubber compound;
(d) According to the structure shown in the figures 1 and 2, the outer layer elastomer compound, the middle layer elastomer compound and the inner layer elastomer compound are injected and molded by adopting a multilayer injection process, and the molded multilayer elastomer compound is vulcanized for 20min at the temperature of 145 ℃ and under the pressure of 10MPa to prepare the vulcanized multilayer elastomer sealing test piece and the vulcanized multilayer elastomer sealing ring product, wherein the performances of the test piece and the vulcanized multilayer elastomer sealing ring product are shown in tables 1 and 2.
Example 3:
the preparation method of the multilayer wide-temperature-range oil-resistant sealing product comprises the following steps and conditions:
(a) According to the outer elastomeric ethylene acrylate copolymer (AEM): carbon black N330 and N660 mixture (mass ratio 2: zinc oxide and stearic acid mixture (mass ratio 5: n-cyclohexyl-2-benzothiazolesulfenamide/accelerator CZ and trimethylolpropane trimethacrylate (TMPTMA) mixture (mass ratio 2: sulfur and dicumyl peroxide (DCP) mixture (mass ratio 2: the mass ratio of the mixture of the antioxidant RD and the antioxidant 4010NA (mass ratio 1: 50:5:2:4:2, putting the outer-layer elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing at the initial temperature of 70 ℃ and the rotor speed of 60 rpm for 10 minutes, and discharging the rubber compound to obtain outer-layer elastomer rubber compound;
(b) According to the weight ratio of a chloroprene rubber and brominated butyl rubber mixture (mass ratio 2: octyl phenol-formaldehyde tackifying resin (203 resin) and p-tert-butylphenol formaldehyde resin (2402 resin) mixture (mass ratio 1: carbon black N220, magnesium oxide and precipitated silica 175MP mixture (mass ratio 5: zinc oxide and stearic acid mixture (mass ratio 5: ethylenethiourea/accelerator (NA-22) and triallylisocyanurate (accelerator TAIC) mixtures (mass ratio 1: sulfur and dicumyl peroxide (DCP) mixture (mass ratio 1: the mass ratio of the mixture of 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, the tackifying resin, the filler and the auxiliary agent into an open rubber mixing mill, mixing at the initial temperature of 50 ℃ and the roller spacing of 5mm for 20 minutes, and then mixing the rubber compound to obtain a sheet to obtain an intermediate layer elastomer rubber compound;
(c) According to the mass ratio of a natural rubber and butadiene-isoprene copolymer mixture (1: carbon black N330: zinc oxide and stearic acid mixture (mass ratio 5: the mass ratio of a tetramethylthiuram disulfide/accelerator TMTD to trimethylolpropane trimethacrylate (TMPTMA mixture (mass ratio of 1);
(d) According to the structure shown in the figures 1 and 2, the outer layer elastomer compound, the middle layer elastomer compound and the inner layer elastomer compound are injected and molded by adopting a multilayer injection process, and the molded multilayer elastomer compound is vulcanized for 30min at the temperature of 150 ℃ and under the pressure of 10MPa to prepare the vulcanized multilayer elastomer sealing test piece and the vulcanized multilayer elastomer sealing ring product, wherein the performances of the test piece and the sealing ring product are shown in tables 1 and 2.
Example 4:
the outer layer elastomer material adopts silicon rubber (QR), the halogen-containing elastomer adopts a mixture of chloroprene rubber and chlorinated polyethylene (mass ratio 2.
Example 5:
the outer layer elastomer material is Hydrogenated Nitrile Butadiene Rubber (HNBR), the mixture of chloroprene rubber and chlorosulfonated polyethylene for halogen-containing elastomer (mass ratio 2.
Example 6:
the outer layer elastomer material adopts polyacrylate rubber (ACM), the inner layer low temperature resistant elastomer adopts a mixture of butadiene-isoprene copolymer and styrene butadiene rubber (mass ratio is 2.
Comparative example 1:
the properties of the test piece and the seal ring product are shown in tables 1 and 2 by injection molding the outer layer elastomer mixture and the inner layer low temperature resistant elastomer mixture according to the procedure and process parameters of example 3 with the middle layer elastomer mixture omitted and with reference to the structures of fig. 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 cross section, and the thickness of the omitted middle layer is increased into the outer layer to ensure that the size of the sealing ring is not changed. This comparative example mainly examined the effect of the intermediate layer on the properties of the sealing article.
Comparative example 2:
the middle layer elastomer mixture and the inner layer low temperature resistant elastomer mixture were omitted according to the procedure and process parameters of example 3, only the outer layer elastomer mixture was injection molded alone with reference to the structures of fig. 1 and 2, and the properties of the test pieces and the 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 3.55 +/-0.10 mm in cross section, and the performance of a sealing product made of a single outer layer material is mainly considered in the comparative example.
Comparative example 3:
the procedure and process parameters of example 3 were followed, the outer elastomer compound and the intermediate elastomer compound were omitted, only the inner low temperature resistant elastomer compound was injection molded alone with reference to the structures of FIGS. 1 and 2, and the properties of the test pieces and the 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 3.55 +/-0.10 mm in cross section, and the performance of a sealing product made of a single inner layer material is mainly considered in the comparative example.
Tables 1-1 test piece Properties of examples and comparative examples
| Item | 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 were carried out according to the standard "determination of tensile stress-strain properties of vulcanized rubber or thermoplastic rubber" GB/T528-2009, with a cutter type I.
Tables 1-2 test piece Properties of examples and comparative examples
* The physical and mechanical properties are measured according to the standard GB/T528-2009 determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber, and a cutting knife is of a type I. The oil field aging test is carried out 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: tensile strength (MPa) before oil field aging x elongation at break (%) before oil field aging x 100%/tensile strength (MPa) after oil field aging x elongation at break (%) after oil field aging;
* And judging that the oil resistance of the oil field oil resistance test is lower than 85 percent, and the oil is not resistant to the type of oil.
Tables 1-3 test piece Properties of examples and comparative examples
* The high temperature resistance is carried out according to the standard GB/T1683-2018 method for measuring the constant deformation compression set of vulcanized rubber, the compression amount is 25 percent, and the temperature is 150 ℃;
* The low temperature resistance was carried out according to the standard "determination of the compression cold resistance coefficient of vulcanized rubber HG/T3866-2006" at a temperature of-50 ℃.
TABLE 2 Properties of seal ring products of examples and comparative examples
* Testing with the seal ring product;
* The compression set is carried out according to the standard GB/T1683-2018 method for measuring the constant deformation compression set of vulcanized rubber, the compression amount is 25 percent, and the temperature is 200 ℃;
* The compression cold resistance coefficient was carried out according to the standard "determination of the compression cold resistance coefficient of vulcanized rubber HG/T3866-2006" at a temperature of-50 ℃.
The comparison of the data in tables 1 and 2 shows that the test piece and the sealing product (O-shaped sealing ring) with the multilayer structure, prepared by the invention, keep 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 disclosed by the invention can integrate the mechanical property advantages of three materials in terms of mechanical property, and has the using effects of wide temperature range, strong sealing and good mechanical property.
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, extension, 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 multilayer-structure wide-temperature-range oil-resistant sealing product is characterized in that a high-temperature-range oil-resistant elastomer is used as an outer layer of a multilayer 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 in an inner layer, a peroxide and sulfur compound vulcanization system is used for crosslinking, and the multilayer-structure wide-temperature-range oil-resistant sealing product is prepared by synchronously vulcanizing the multilayer structure.
2. The method of claim 1, wherein the outer layer is a mixture of a fluoro-rubber (FR), a silicone rubber (QR), a fluorosilicone rubber (FVMQ), a hydrogenated nitrile rubber (HNBR), a polyacrylate rubber (ACM), or an ethylene acrylate copolymer (AEM) with a filler aid;
the middle layer is a mixture of tackifying resin, halogen-containing elastomer and filler auxiliary agent;
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 two-phase composite crosslinking system, and simultaneously improves the mechanical property and the aging resistance of the vulcanized elastomer.
3. The method according to claim 1 or 2, characterized in that the steps and conditions are as follows:
(a) According to the elastomer of the outer layer: filling: active agent(s): vulcanization accelerator (b): vulcanizing agent: the mass ratio of the anti-aging agent is 100:20 to 100:3 to 5:1 to 3:1 to 5: 1-3, putting the outer-layer elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing at the initial temperature of 50-70 ℃ and the rotor rotation speed of 40-60 r/min for 5-10 minutes, and discharging the rubber compound to obtain outer-layer elastomer rubber compound;
(b) According to the halogen-containing elastomer: tackifying resin: filling: active agent(s): vulcanization accelerator (b): vulcanizing agent: the mass ratio of the anti-aging agent is 100:50 to 150:5 to 20:3 to 5:1 to 3:1 to 5: 1-3, putting the halogen elastomer, the tackifying resin, the filler and the auxiliary agent into an open rubber mixing mill, mixing at the initial temperature of 40-50 ℃ for 15-20 minutes at a roller spacing of 3-5 mm, and discharging the rubber compound to obtain an intermediate layer elastomer rubber compound;
(c) According to the inner layer low temperature resistant elastomer: filling: active agent(s): vulcanization accelerator (b): vulcanizing agent: the mass ratio of the anti-aging agent is 100:20 to 50:3 to 5:1 to 3:1 to 5: 1-3, putting the inner-layer low-temperature-resistant elastomer, the filler and the auxiliary agent into an internal rubber mixing mill, mixing at the initial temperature of 50-70 ℃ and the rotor rotation speed of 40-60 r/min for 5-10 minutes, and discharging rubber compound to obtain inner-layer elastomer rubber compound;
(d) And (3) performing injection molding on the elastomer rubber compound of the outer layer, the middle layer and the inner layer by adopting a multilayer injection process to obtain multilayer rubber compound, and co-vulcanizing the molded multilayer rubber compound for 10-30 min at the temperature of 135-150 ℃ and under the pressure of 10-15 MPa to obtain the multilayer-structure wide-temperature-range oil-resistant sealing product.
4. The preparation method of claim 3, wherein the filler is one or more of carbon black N220, N330, N339, N550, N660, N774 or precipitated silica 175MP, fumed silica A200 and magnesium oxide;
the activating agent is a mixture of zinc oxide and stearic acid, and the mass ratio of the activating agent to the stearic acid is 5:0.5 to 3;
the vulcanization accelerator is hexamethylenetetramine/accelerator H, diphenylguanidine/accelerator D, tetramethylthiuram disulfide/accelerator TMTD, 2-thiol benzothiazole/accelerator M, zinc dimethyldithiocarbamate/accelerator ZDMC, zinc butylxanthate/accelerator ZBX, N-cyclohexyl-2-benzothiazole sulfenamide/accelerator CZ, ethylenethiourea/accelerator (NA-22) or peroxide accelerator: one or more of triallyl isocyanurate (accelerator TAIC), N' -m-phenylene bismaleimide (HVA 2), trimethylolpropane trimethacrylate (TMPTMA);
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) or di-tert-butyl peroxide (DTBP);
the anti-aging agent is one or more of N-phenyl-beta-naphthylamine (anti-aging agent D), 2, 4-trimethyl-1, 2-dihydroquinoline polymer (anti-aging agent RD), 2-thiol benzimidazole (anti-aging agent MB), N, N-di-N-butyl dithiocarbamic acid nickel (anti-aging agent NBC) or N-isopropyl-N' -phenyl p-phenylenediamine (anti-aging agent 4010 NA).
5. The method of claim 3, wherein the halogen-containing elastomer is one or more of neoprene, chlorinated polyethylene, chlorosulfonated polyethylene, or bromobutyl 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-tert 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.
6. The method for preparing the oil-resistant sealing product according to claim 1, wherein the thickness requirements of each layer of the multi-layer structure wide-temperature-range oil-resistant sealing product are as follows: the outer layer accounts for 20 to 35 percent of the total thickness, preferably 25 to 30 percent; the inner layer accounts for 60 to 75 percent of the total thickness, preferably 65 to 70 percent; the middle layer is an adhesive layer, so that the thinner the adhesive layer is, the better the adhesive effect is, and the adhesive layer accounts for about 5% of the total thickness.
7. A multilayer wide temperature range oil resistant sealing product prepared by the preparation method of any one of claims 1 to 6.
8. Use of the multilayer wide temperature range oil resistant sealing article of claim 7 as a sealing article.
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| CN116771918A (en) * | 2023-06-08 | 2023-09-19 | 上海芯密科技有限公司 | Multilayer sealing product for semiconductor and preparation method thereof |
| CN116771918B (en) * | 2023-06-08 | 2024-03-26 | 上海芯密科技有限公司 | Multilayer sealing product for semiconductor and preparation method thereof |
| CN117070006A (en) * | 2023-10-17 | 2023-11-17 | 广东粤港澳大湾区黄埔材料研究院 | Low-temperature-resistant crystallization-resistant butadiene rubber composition, preparation method thereof and rubber sealing product |
| CN117070006B (en) * | 2023-10-17 | 2024-01-05 | 广东粤港澳大湾区黄埔材料研究院 | Low-temperature-resistant crystallization-resistant butadiene rubber composition, preparation method thereof and rubber sealing product |
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| CN115230266B (en) | 2023-11-17 |
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