CN103059775A - Heat vulcanized adhesive for adhering vulcanized rubber or thermoplastic rubber with hard panel - Google Patents
Heat vulcanized adhesive for adhering vulcanized rubber or thermoplastic rubber with hard panel Download PDFInfo
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- CN103059775A CN103059775A CN2013100264325A CN201310026432A CN103059775A CN 103059775 A CN103059775 A CN 103059775A CN 2013100264325 A CN2013100264325 A CN 2013100264325A CN 201310026432 A CN201310026432 A CN 201310026432A CN 103059775 A CN103059775 A CN 103059775A
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- thermovulcanizate
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- plate material
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Abstract
The invention discloses a heat vulcanized adhesive for adhering a vulcanized rubber or a thermoplastic rubber with a hard panel. The heat vulcanized adhesive comprises a crosslinking agent N,N'-dinitroso-p-phenylene dihydroxy disodium, halogenated rubber, metal oxide such as zinc oxide or magnesium oxide, inertia stuffing such as carbon black or titanium dioxide, a solvent such as aromatic hydrocarbon, chloride solvent or ketone solvent, a polybismaleimide compound such as N,N'-m-phenylene bismaleimide or diphenylmethane bismaleimide, and a vulcanizing agent such as sulphur, selenium or tellurium. The heat vulcanized adhesive has the characteristics that the heat vulcanized adhesive does not comprise aromatic polynitroso compound, adduct of perhalogenated cyclic conjugated diene/olefinic unsaturated dienophile, and copolymer formed by halogenated butadiene monomer/alpha-halogen substituted monomeric compound, and also does not comprise any one of alkoxy silane/polymer of nitrosobenzene or nitrosobenzene precursor combination; meanwhile, the heat vulcanized adhesive has pre-heating-resistance or is suitable for the requirement of injection molding process, and has the slat mist resistance and boiled water resistance.
Description
Technical field
The present invention relates to a kind of thermovulcanizate stick for bonding vulcanized rubber or thermoplastic elastomer and hard plate material, this thermovulcanizate stick is used for bonding vulcanized rubber or thermoplastic elastomer and hard plate material.
Technical background
Having developed on the market many kinds provides the thermovulcanizate stick of bonding vulcanized rubber or thermoplastic elastomer and hard plate material.For example, the CN200580019624.7 of Lord Corp. discloses the rubber to metal adhesive that a kind of solid is scattered in volatile carrier liquid, this tackiness agent contains the solid particulate of dispersion, and this solid particulate contains the incompressible spheroidal particle of inertia of nitroso compound, halogenated polyolefin, acid acceptor and 5～35wt%.A kind of thermovulcanizate stick that contains Halogen polyolefine, aromatic nitroso compound, polymaleimide compounds and metal oxide is disclosed among the CN93114420.5.But many nitroso compounds of aromatic series particularly preferably all wherein.
Under the comparatively high temps that nowadays injection molding technique is commonly used, the many nitroso compounds of aromatic series tend to distillation, make the rubber mass that is injected into the many nitroso compound reactions of aromatic series, and it cures before material fills up injection molding, and on the metallic surface, react with tackiness agent, the rubber of this prevulcanized can be with remaining rubber mix in mould, thereby causes forming weak interface layer, and then causes the goods after the sulfuration to damage too early.
CN92102610.2 has narrated a kind of resistant to elevated temperatures hot sulfurization adhesive system, this tackiness agent contains the Diels-Alder adducts that is generated above the unsaturated dienophile reaction of 50% olefinic by perhalogeno cyclic conjugated diene hydrocarbon and contents of ethylene, resol, aromatic hydroxy compound, formaldehyde is to body, be subjected to the unsaturated elastic body linking agent of thermal activation, vulcanizing agent, and metal oxide.
CN92102679.X has narrated another hot sulfurization adhesive system, this tackiness agent is with the polymeric material of some Halofunctional monomeric material modification, by bond properties and the relatively large additional binder ingredients of release that improves elastomerics one adhesive interface, for example nitroso-group or carbamate compounds improve the bounding force of elastic matrix and metallic surface significantly.A preferred embodiment comprises the multipolymer that a kind of monomeric compound that is replaced by halogenated succinimide alkene monomer and α-halogen forms, wherein the consumption of the compound that replaces of α-halogen accounts for approximately 0.1-10% of multipolymer amount, preferably 2-8%(weight).
Luo Ketaite (R﹠amp; D) CN200980109605.1 of company limited provides a kind of compound, at least one structure division that it comprises at least one organoalkoxysilane structure division and is selected from nitrosobenzene or nitrosobenzene precursor and combination thereof, and it is used for polymkeric substance to metal, and especially rubber is to the bonding of metal.
The hot sulfurization adhesive system that the present invention also provides a kind of " anti-hot in advance ".So-called " anti-hot in advance " refers to be coated with the at a certain temperature preheating of metal of tackiness agent before vulcanized rubber or thermoplastic elastomer adding and sulfuration, to accelerate the volatilization of solvent, enhances productivity.Vulcanized rubber or thermoplastic elastomer break, and to reach for 100% required warm up time longer, then anti-pre-hot better, thereby the thermovulcanizate stick is also better.
Hot sulfurization adhesive system of the present invention is a kind of new system that is different from above several tackiness agent, neither contain the multipolymer that the monomeric compound that adducts, halogenated succinimide alkene monomer/α-halogen replaces of the many nitroso compounds of aromatic series, the unsaturated dienophile of perhalogeno cyclic conjugated diene hydrocarbon/olefinic forms, wherein any of the polymkeric substance that does not also contain organoalkoxysilane/nitrosobenzene or nitrosobenzene combination of precursors, have simultaneously the performance of " anti-preheating " or the requirement of suitable injection molding technique, also have salt spray resistance and resistant to boiling water performance.
Summary of the invention
The object of the present invention is to provide the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material, its maximum is characterised in that and contains linking agent N, the N'-dinitroso-to phenylene dihydroxyl disodium:
N, the N'-dinitroso-to phenylene dihydroxyl disodium
Content of the present invention comprises:
The thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material is characterized in that, this thermovulcanizate stick mainly contains following compositions in weight percentage and makes:
Linking agent 1.5-10%
Halogenated rubber 5-30%
Metal oxide 0.5-5%
Polymaleimide compounds 0.5-5%
Vulcanizing agent 0.5-5%
Inertia color stuffing 2-30%
The solvent surplus
Said components weight percent sum is 100%.This thermovulcanizate stick preferred weight percent is:
N, the N'-dinitroso-to phenylene dihydroxyl disodium 4-10%
Maleic anhydride modified Chlorinated Polypropylene III 5-15%
Zinc oxide 0.5-3%
N, a N '-penylene bismaleimides 0.5-3%
Selenium 0.5-3%
Carbon black 2-8%
The dimethylbenzene surplus
Said components weight percent sum is 100%.
Being suitable for linking agent of the present invention is N, the N'-dinitroso-to phenylene dihydroxyl disodium:
N, the N'-dinitroso-to phenylene dihydroxyl disodium
Being suitable for halogenated rubber of the present invention is chlorosulfonated polyethylene, chlorinated natural rubber, Chlorinated Polypropylene III, maleic anhydride modified Chlorinated Polypropylene III, epoxy resin modification Chlorinated Polypropylene III, ethylene chloride/acetate ethylene copolymer or chlorinatedpolyethylene, further preferred maleic anhydride modified Chlorinated Polypropylene III.
Being suitable for metal oxide of the present invention is zinc oxide or magnesium oxide, further preferential oxidation zinc.
Being suitable for polymaleimide compounds of the present invention is N, N '-penylene bismaleimides or diphenyl methane dimaleimide, further preferred N, a N '-penylene bismaleimides.
Being suitable for vulcanizing agent of the present invention is sulphur, selenium or tellurium, further preferred selenium.
Being suitable for inertia color stuffing of the present invention is carbon black or titanium dioxide, further preferred carbon black.
Be suitable for solvent of the present invention and be aromatic hydrocarbons (for example dimethylbenzene, toluene, ethylbenzene), chlorinated solvent (for example trieline, zellon) or ketones solvent (for example methylethylketone, methyl iso-butyl ketone (MIBK), pimelinketone), further preferred dimethylbenzene.
Thermovulcanizate stick maximum of the present invention is characterised in that the multipolymer that monomeric compound that the adducts that neither contains the many nitroso compounds of aromatic series, the unsaturated dienophile of perhalogeno cyclic conjugated diene hydrocarbon/olefinic, halogenated succinimide alkene monomer/α-halogen replace forms, wherein any of the polymkeric substance that does not also contain organoalkoxysilane/nitrosobenzene or nitrosobenzene combination of precursors, have simultaneously the performance of " anti-preheating " or the requirement of suitable injection molding technique, also have salt spray resistance and resistant to boiling water performance.
Embodiment
Above explanation and the following examples are open and illustrate of the present inventionly, and the concrete consumption of wherein said each composition and combination are not in order to limit the scope of the present invention by claims defined.
Preparation as follows linking agent N of the present invention, the N'-dinitroso-to phenylene dihydroxyl disodium:
N, the N'-dinitroso-to phenylene dihydroxyl disodium
The 136g p-benzoqui(o)none dioxime is under agitation joined in 3, the 000 ml methyl alcohol to form suspensoid.After adding the 108.04g sodium methylate, slowly pass into nitric oxide gas 60.02g, so that the temperature of reaction mixture is no more than 27 ℃.After passing into the nitrogen protoxide end, restir reaction mixture 15 minutes.Use sodium hydroxide solution, add air, absorb excessive nitric oxide gas.With the throw out centrifugation, be suspended in the neutral water, after the filtration filter residue is used the neutral water washing and filtering repeatedly.Last filter residue is vacuumized drying under 50 ℃, obtain linking agent N, the N'-dinitroso-to phenylene dihydroxyl disodium 221.6g, productive rate is 93%.
Prepare thermovulcanizate stick of the present invention with the mixture of the linking agent A, the B that make above and C and following composition and solvent:
In order to make sample, will be through the steel disc degreasing of sandblasting with zellon steam, and drying.Steel disc is according to the requirement of GB/T 7760-2003 preparation, and thickness is 1.5mm ± 0.1mm, suitably thickens when using plastic plate or other sheet material, and the width of steel disc is 25mm ± 0.1mm, and length is 60mm ± 1mm.Before applying tackiness agent, hide 17.5 mm and 17.5 mm at steel disc test specimen two ends, can be used for being bonded on the rubber to prevent this zone, stay the wide central zone of 25 mm length and 25mm ± 0.1mm to be provided on the rubber.Then this steel disc is applied approximately 10 μ m(drying layer thickness) thick Polyton 810 is as primary coat, applies respectively approximately 13-25 μ m(drying layer thickness after the primary coat drying in the above) face of thick routine 1-4 is coated with.
At room temperature or at a certain temperature carry out drying.
Then with following rubber bound on the sample of band coating, the rubber that bond is as follows:
| Composition | Weight part |
| Natural rubber | 100 |
| ZnO | 5 |
| Stearic acid | 1 |
| Antioxidant 4010NA | 2 |
| Microcrystalline Wax OK1900 | 2 |
| Carbon black N-550 | 40 |
| Sulphur | 1.8 |
| Accelerant CZ | 2 |
Uncured above-mentioned natural rubber is placed on each test specimen, and sulfuration 15 minutes under 160 ℃, the pressure of 10MPa.
After sulfuration, will at room temperature place more than 16 hours through the sample of bonding, peel off afterwards test.
" coverage " is to peel off after the test, residual rubber per-cent on the metal substrate of bonding.100% rubber destroys and refers to destroy fully, and does not have rubber part to peel off (with being equivalent to 100% rubber destruction) from the metallic surface.
Good natural rubber-steel disc the assembly that then will bond is done the test of the following stated.
Initial bonding strength
According to 90 ° of footmark standards of GB/T 7760-2003, use Instron testing installation (Instron tester, model 5500R), under the steady load speed of 50mm/min, test each sample, until separate fully.Record is peeled off " coverage " after the test.
Anti-prefiring
This test is very similar with initial bonding strength test, and unique difference is in this test, natural rubber add and sulfuration before, be coated with the respectively preheating 5 minutes, 10 minutes, 15 minutes under 160 ℃ of conditions of pair steel disc of the tackiness agent that are coated with.
Salt-fog resistant test
The assembly that bonding is good is polished at the edge of emery wheel.Then rubber is bundled on the metal with Stainless Steel Wire is counter.Binder layer is drained in the environment cruelly.Impel with blade delineation binder layer and to break.Be hung in assembly on the Stainless Steel Wire again and put into a salt spray booth (load-carrying 2KG).Indoor environment is 38 ℃ of temperature, and relative humidity 100% is dissolved with 5% salt in the spray saline solution, and is dispersed in whole indoor.Assembly was indoor maintenance 72 hours.After the taking-up, with the same metal-stripping of rubber, measuring the per-cent that rubber keeps on the assembly with hand vice.
Boiling water test
The assembly that bonding is good is polished at the edge of emery wheel.Then rubber is bundled on the metal with Stainless Steel Wire is counter.Binder layer is drained in the environment cruelly.Impel with blade delineation binder layer and to break.Be hung in assembly on the Stainless Steel Wire again and put into 95 ℃ boiling water (load-carrying 2KG).Assembly kept in boiling water 2 hours.After the taking-up, with the same metal-stripping of rubber, measuring the per-cent that rubber keeps on the assembly with hand vice.
Prescription listed above, the result is as follows:
Can find out from above prescription and data, thermovulcanizate stick of the present invention is a kind of new system, neither contain the multipolymer that the monomeric compound that adducts, halogenated succinimide alkene monomer/α-halogen replaces of the many nitroso compounds of aromatic series, the unsaturated dienophile of perhalogeno cyclic conjugated diene hydrocarbon/olefinic forms, wherein any of the polymkeric substance that does not also contain organoalkoxysilane/nitrosobenzene or nitrosobenzene combination of precursors, have simultaneously the performance of " anti-preheating " or the requirement of suitable injection molding technique, also have salt spray resistance and resistant to boiling water performance.
Claims (9)
1. the thermovulcanizate stick of a bonding vulcanized rubber or thermoplastic elastomer and hard plate material is characterized in that, this thermovulcanizate stick mainly contains following compositions in weight percentage and makes:
Linking agent 1.5-10%
Halogenated rubber 5-30%
Metal oxide 0.5-5%
Polymaleimide compounds 0.5-5%
Vulcanizing agent 0.5-5%
Inertia color stuffing 2-30%
The solvent surplus
Said components weight percent sum is 100%.
2. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 is characterized in that, this thermovulcanizate stick preferred weight percent is:
N, the N'-dinitroso-to phenylene dihydroxyl disodium 4-10%
Maleic anhydride modified Chlorinated Polypropylene III 5-15%
Zinc oxide 0.5-3%
N, a N '-penylene bismaleimides 0.5-3%
Selenium 0.5-3%
Carbon black 2-8%
The dimethylbenzene surplus
Said components weight percent sum is 100%.
3. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described linking agent is N, the N'-dinitroso-to phenylene dihydroxyl disodium.
4. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described halogenated rubber is selected from one or more in chlorosulfonated polyethylene, chlorinated natural rubber, Chlorinated Polypropylene III, maleic anhydride modified Chlorinated Polypropylene III, epoxy resin modification Chlorinated Polypropylene III, ethylene chloride/acetate ethylene copolymer, the chlorinatedpolyethylene.
5. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described metal oxide is zinc oxide or magnesium oxide.
6. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described polymaleimide compounds is N, N '-penylene bismaleimides or diphenyl methane dimaleimide.
7. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described vulcanizing agent is sulphur, selenium or tellurium.
8. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described inertia color stuffing is carbon black or titanium dioxide.
9. the thermovulcanizate stick of a kind of bonding vulcanized rubber or thermoplastic elastomer and hard plate material as claimed in claim 1 or 2, it is characterized in that: described solvent is aromatic hydrocarbons, chlorinated solvent or ketones solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100264325A CN103059775A (en) | 2013-01-24 | 2013-01-24 | Heat vulcanized adhesive for adhering vulcanized rubber or thermoplastic rubber with hard panel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100264325A CN103059775A (en) | 2013-01-24 | 2013-01-24 | Heat vulcanized adhesive for adhering vulcanized rubber or thermoplastic rubber with hard panel |
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| CN103059775A true CN103059775A (en) | 2013-04-24 |
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| CN2013100264325A Pending CN103059775A (en) | 2013-01-24 | 2013-01-24 | Heat vulcanized adhesive for adhering vulcanized rubber or thermoplastic rubber with hard panel |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165205A (en) * | 2016-12-08 | 2018-06-15 | 北京橡胶工业研究设计院有限公司 | A kind of hot-melt adhesive composition and its application method |
| CN109337590A (en) * | 2018-09-07 | 2019-02-15 | 上海普力通新材料科技有限公司 | A kind of shock insulation high-damping rubber tailored version Heat vulcanization adhesive |
| CN112812711A (en) * | 2021-01-25 | 2021-05-18 | 安徽普力通新材料科技有限公司 | High-reactivity metal-rubber heat-vulcanization adhesive and using method thereof |
| CN113292932A (en) * | 2021-06-01 | 2021-08-24 | 深圳博林新材料科技有限公司 | Environment-friendly double-component water-based hot vulcanization adhesive and preparation method thereof |
| CN115141581A (en) * | 2021-08-31 | 2022-10-04 | 上海普力通新材料科技有限公司 | High-impact-resistance single-coated metal-rubber hot vulcanization adhesive and using method thereof |
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2013
- 2013-01-24 CN CN2013100264325A patent/CN103059775A/en active Pending
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| GB936978A (en) * | 1959-12-14 | 1963-09-18 | Lord Mfg Co | N-nitroso-hydroxylamine derivatives and a process for the production thereof |
| JP2003221785A (en) * | 2002-01-29 | 2003-08-08 | Gates Unitta Asia Co | Adhesive of cord for rubber reinforcement, cord for rubber reinforcement, transmission belt and method for producing transmission belt |
| CN102206479A (en) * | 2010-03-31 | 2011-10-05 | 王平议 | Production method of polyurethane rubber adhesive |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165205A (en) * | 2016-12-08 | 2018-06-15 | 北京橡胶工业研究设计院有限公司 | A kind of hot-melt adhesive composition and its application method |
| CN109337590A (en) * | 2018-09-07 | 2019-02-15 | 上海普力通新材料科技有限公司 | A kind of shock insulation high-damping rubber tailored version Heat vulcanization adhesive |
| CN109337590B (en) * | 2018-09-07 | 2021-05-07 | 上海普力通新材料科技有限公司 | Special heat-vulcanized adhesive for shock-insulation high-damping rubber |
| CN112812711A (en) * | 2021-01-25 | 2021-05-18 | 安徽普力通新材料科技有限公司 | High-reactivity metal-rubber heat-vulcanization adhesive and using method thereof |
| CN113292932A (en) * | 2021-06-01 | 2021-08-24 | 深圳博林新材料科技有限公司 | Environment-friendly double-component water-based hot vulcanization adhesive and preparation method thereof |
| CN115141581A (en) * | 2021-08-31 | 2022-10-04 | 上海普力通新材料科技有限公司 | High-impact-resistance single-coated metal-rubber hot vulcanization adhesive and using method thereof |
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Inventor after: Yao Xiaoying Inventor after: Jiang Yonghua Inventor before: Yao Xiaoying |
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Free format text: CORRECT: INVENTOR; FROM: YAO XIAOYING TO: YAO XIAOYING JIANG YONGHUA |
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Application publication date: 20130424 |