CN116855224B - Structural adhesive for automobile silent tire and preparation method thereof - Google Patents
Structural adhesive for automobile silent tire and preparation method thereof Download PDFInfo
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- CN116855224B CN116855224B CN202310895799.4A CN202310895799A CN116855224B CN 116855224 B CN116855224 B CN 116855224B CN 202310895799 A CN202310895799 A CN 202310895799A CN 116855224 B CN116855224 B CN 116855224B
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- epoxy resin
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 65
- 239000000853 adhesive Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title description 28
- 239000004005 microsphere Substances 0.000 claims abstract description 176
- 239000003822 epoxy resin Substances 0.000 claims abstract description 35
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 35
- 239000004793 Polystyrene Substances 0.000 claims abstract description 20
- 229920002223 polystyrene Polymers 0.000 claims abstract description 20
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 19
- 229920002050 silicone resin Polymers 0.000 claims abstract description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 30
- 229920000642 polymer Polymers 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 239000000178 monomer Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 14
- 239000000839 emulsion Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 150000003505 terpenes Chemical class 0.000 claims description 7
- 235000007586 terpenes Nutrition 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000006482 condensation reaction Methods 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 25
- 230000009467 reduction Effects 0.000 abstract description 23
- 229920000742 Cotton Polymers 0.000 abstract description 19
- 239000011521 glass Substances 0.000 abstract description 12
- -1 polyethylene Polymers 0.000 abstract description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 8
- 229920001568 phenolic resin Polymers 0.000 abstract description 8
- 239000005011 phenolic resin Substances 0.000 abstract description 8
- 229920000767 polyaniline Polymers 0.000 abstract description 8
- 239000011257 shell material Substances 0.000 abstract description 5
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 4
- 239000004698 Polyethylene Substances 0.000 abstract description 2
- 239000004743 Polypropylene Substances 0.000 abstract description 2
- 229920000573 polyethylene Polymers 0.000 abstract description 2
- 229920001155 polypropylene Polymers 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 11
- 239000004593 Epoxy Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- 239000007822 coupling agent Substances 0.000 description 4
- 239000003981 vehicle Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical group NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000011496 polyurethane foam Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229960001124 trientine Drugs 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- NBJODVYWAQLZOC-UHFFFAOYSA-L [dibutyl(octanoyloxy)stannyl] octanoate Chemical compound CCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCC NBJODVYWAQLZOC-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- SKWZHINXPDOQDF-UHFFFAOYSA-N disilanyl(ethenyl)silane Chemical compound [SiH3][SiH2][SiH2]C=C SKWZHINXPDOQDF-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000030279 gene silencing Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SFMJNHNUOVADRW-UHFFFAOYSA-N n-[5-[9-[4-(methanesulfonamido)phenyl]-2-oxobenzo[h][1,6]naphthyridin-1-yl]-2-methylphenyl]prop-2-enamide Chemical compound C1=C(NC(=O)C=C)C(C)=CC=C1N1C(=O)C=CC2=C1C1=CC(C=3C=CC(NS(C)(=O)=O)=CC=3)=CC=C1N=C2 SFMJNHNUOVADRW-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/18—Spheres
- C08L2205/20—Hollow spheres
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Abstract
The invention discloses a structural adhesive for a mute tire of an automobile, which comprises 0.1-10% by mass of hollow microspheres, wherein the shell material of the hollow microspheres comprises polystyrene, polyethylene, polypropylene, polyaniline, polymethylaniline, phenolic resin, epoxy resin, silicone resin, glass and SiO 2 、TiO 2 . The structural adhesive provided by the invention has an auxiliary effect on the noise reduction effect of the sound absorbing cotton in the mute tire, can further reduce the noise intensity of the tire between 200 and 250Hz, and is good in toughness and high in adhesive strength.
Description
Technical Field
The invention belongs to the technical field of structural adhesives for automobiles, and particularly relates to a structural adhesive for a silent tire of a new energy automobile and a preparation method of the structural adhesive.
Background
Vehicles are becoming increasingly popular as a everyday vehicle. With the improvement of the living standard of people, vehicles are not just a simple transportation means, and more are enjoyment of traveling. At the moment of the strong development of new energy automobiles, tire noise has become one of the main factors affecting the comfort of automobiles. Therefore, reducing tire noise has become an important consumer demand for automobile comfort.
The noise of the tire mainly contacts with the rugged road surface in the rotation process of the tire, so that the air in the cavity of the tire resonates due to the vibration of the tire, and when the resonant frequency reaches a specific hertz, the noise causes discomfort. To this end, vehicle manufacturers have improved NVH (noise, vibration and harshness) performance by various means, such as improving overall stiffness, employing silent tires, and the like.
A special porous polyurethane sponge is stuck on the inner side of the tire to prepare a silent tire type noise reduction mode which is widely applied at present. The Michelin sound silencing technology, the German horse brand ContiSilent tire noise reduction technology and the Gu special noise covering technology are all to attach a piece of sound absorbing cotton made of special materials on the inner side of the tire to achieve noise reduction, and the function mechanism is that noise generated by impact of the tire and a road surface can be repeatedly refracted in the tire and finally gradually absorbed by the sound absorbing cotton, and meanwhile, the noise generated by extrusion of the road surface to the air in the tire can be reduced by the sound absorbing cotton.
Patent document CN 110450583A discloses a silent tire and a preparation method thereof, wherein a rubber composition and a tire body are co-vulcanized, so that a foaming layer and the tire body form a crosslinked integrated structure, and the foaming layer is not easy to fall off in the high-temperature and dynamic use process. This idea is good, but the real problem is that the silent tire produced according to this method is more like disposable, increasing the difficulty of tire repair, since the foam layer is integral with the tire body. Those skilled in the art know that the sound absorbing cotton in a conventional mute tire is stuck on the inner side of the tire through structural adhesive, and can be taken down when the tire needs to be maintained, and can be stuck again after the tire is repaired, so that the continuous use of the tire is not influenced. Therefore, it is necessary to develop a structural adhesive that has strong adhesive properties and contributes to noise reduction.
As a special structural adhesive for the mute tire, the structural adhesive is required to have stronger cohesiveness and toughness at first, so that the conditions of tearing, shifting and the like can not occur when the tire passes through a pit at a high speed to deform. Secondly, the use of the structural adhesive should not weaken the noise reduction effect of the silent tire as much as possible.
Patent document CN 116285806A discloses a structural adhesive for automobiles and a preparation method thereof, wherein the structural adhesive comprises the following components: polyurethane prepolymer modified epoxy resin, core-shell toughening material, high-temperature resistant modified resin, filler, coupling agent, curing agent, dispersing agent and anti-aging agent. According to the text, the adhesive is mainly suitable for automobile clutches, and solves the defect that the adhesive of a conventional clutch is easily affected by factors such as temperature, humidity, mechanical vibration and the like to cause the reduction of bonding strength.
The technical staff of the invention find that the traditional structural adhesive is used for sticking the sound absorbing cotton on the tire, the structural adhesive has negative influence on the noise reduction effect of the mute tire, and the thicker the adhesive layer is, the larger the influence on the noise reduction effect of the mute tire is. The technical staff searches and discovers that a structural adhesive specially used for attaching sound absorbing cotton to a silent tire is not discovered at present, and the structural adhesive special for the silent tire is good in adhesive property, mechanical strength and synergism on noise reduction of the silent tire.
Disclosure of Invention
The density of the sound-absorbing cotton material is large, and a large number of tiny communicated holes are formed in the sound-absorbing cotton material, so that vibration can be absorbed, and the sound-insulating effect can be achieved. The sound absorbing cotton material comprises polyurethane foam, glass cotton, rock cotton, mineral cotton and plant fiber, wherein the polyurethane foam is most commonly used. The invention aims to provide the special structural adhesive for the mute tire, which has good bonding property and toughness on the sound-absorbing cotton, and can not cause the phenomenon of tearing or shifting of the sound-absorbing cotton due to the mechanical external force of the tire, and meanwhile, the structural adhesive provided by the invention can increase the noise reduction effect of the mute tire. The structural adhesive provided by the invention has good extrudability at normal temperature, has moderate surface drying time (15-20 min), and meets the requirement of the sound-absorbing cotton pasting operation time.
The invention comprises the following technical scheme:
in a first aspect, the invention provides a structural adhesive for a silent tire of an automobile, which is characterized by comprising 0.1-10% of hollow microspheres by mass, wherein the hollow microspheres are one or a combination of more than two of polymer hollow microspheres or inorganic hollow microspheres, and the particle size of the hollow microspheres is 20-200 μm.
Wherein, the shell material of the polymer hollow microsphere comprises polystyrene, polyethylene, polypropylene, polyaniline, polymethylaniline, phenolic resin, epoxy resin and silicone resin; the inorganic hollow microsphere shell material comprises glass and SiO 2 、TiO 2 。
Preferably, the structural adhesive for the automobile silent tire further comprises the following components in parts by mass: 30-40 parts of organopolysiloxane polymer, 30-45 parts of terpene resin, 10-40 parts of filler and amorphous SiO 2 10-15 parts of coupling agent, 2-20 parts of catalyst, 0.5-2 parts of solvent oil and 10-30 parts of solvent oil.
The organopolysiloxane polymer is one or more of hydroxyl-terminated polydimethylsiloxane, alkoxy-terminated polydimethylsiloxane, and alkyl-terminated polydimethylsiloxane.
In a specific embodiment of the present invention, the organopolysiloxane polymer is a hydroxy-terminated polydimethylsiloxane having a CAS number of 63148-60-7.
The coupling agent is selected from any one of vinyl triethoxysilane, vinyl trimethoxysilane and vinyl trisilane.
The catalyst is selected from one or more of dibutyl tin dilaurate, dibutyl tin diacetate, dibutyl tin dioctanoate, isopropyl titanate and n-butyl titanate.
The filler is nano active calcium carbonate, and the particle size is 50-200nm.
In the specific embodiment of the invention, the structural adhesive for the mute tire of the automobile comprises the following components in parts by weight: 30-40 parts of organopolysiloxane polymer, 30-40 parts of terpene resin, 10-20 parts of nano active calcium carbonate and amorphous SiO 2 10-15 parts of hollow microspheres, 2-15 parts of vinyl trimethoxy silane, 2-10 parts of isopropyl titanate, 0.5-1 part of solvent oil and 10-30 parts of solvent oil.
Preferably, the hollow microsphere is a combination of a polymer hollow microsphere and an inorganic hollow microsphere, and the polymer hollow microsphere comprises one or more than two of polyaniline hollow microsphere, epoxy resin hollow microsphere and silicone resin hollow microsphere; the inorganic hollow microsphere comprises SiO 2 Hollow microsphere and TiO 2 One or more than two hollow microspheres.
More preferably, the polymeric hollow microspheres comprise one or a combination of two of epoxy hollow microspheres, silicone hollow microspheres; the inorganic hollow microsphere comprises TiO 2 Hollow microspheres.
In a specific embodiment of the present invention, the hollow microsphere is TiO 2 The hollow microsphere and the silicone hollow microsphere are combined, and the mass ratio of the hollow microsphere to the silicone hollow microsphere is (10-1): 1.
in another embodiment of the present invention, the hollow microsphere is TiO 2 Hollow microsphere and epoxy treeThe lipid hollow microsphere is combined, and the mass ratio of the lipid hollow microsphere to the lipid hollow microsphere is (10-1): 1.
in a most preferred embodiment of the present invention, the hollow microspheres are TiO 2 And the mass ratio of the hollow microsphere to the silicone hollow microsphere is 3:2.
The hollow microspheres according to the present invention may be prepared by methods conventional in the art, including template methods, emulsion methods, self-assembly methods, etc., or purchased commercially.
In a specific embodiment of the invention, the silicone hollow microspheres are prepared by the following method:
(1) The organic silicon monomer is subjected to hydrolysis reaction in formic acid aqueous solution with the mass fraction of 0.01-0.02% to form silanol solution; then condensation reaction is carried out under the alkaline condition,
(2) Dispersing the polystyrene solid microspheres modified by concentrated sulfuric acid into silanol solution, adding ammonia water solution, polymerizing organic silicon monomers on the surfaces of the polystyrene solid microspheres, and dissolving a polystyrene template by DMF to obtain the silicone hollow microspheres.
Wherein the organic silicon monomer in the step (1) comprises one or more than two of methyltrimethoxysilane, methyltriethoxysilane and vinyltrimethoxysilane.
In a specific embodiment of the invention, the epoxy resin hollow microspheres are prepared by the following method:
(1) Uniformly mixing an epoxy resin monomer, a curing agent and a surfactant at 40 ℃, and adding water in a stirring state to form emulsion;
(2) Dripping the emulsion into ethylene glycol at 50-60 ℃ to form composite emulsion;
(3) Heating the composite emulsion to 100 ℃ to react for 1h, solidifying the epoxy resin, filtering and washing to obtain the water-containing epoxy resin microspheres;
(4) And (3) carrying out vacuum drying on the aqueous epoxy resin for 24 hours, and removing the water to obtain the epoxy resin hollow microspheres.
Wherein the epoxy resin monomer is selected from one or more than two of bisphenol A type epoxy resin, bisphenol F type epoxy resin and bisphenol S type epoxy resin.
The curing agent and the surfactant are all common reagents for the person skilled in the art and can be freely selected according to the needs, and in a specific embodiment, the curing agent is triethylene tetramine, and the surfactant is alkylphenol ethoxylate.
In a second aspect, the invention provides a method for preparing a structural adhesive for a silent tire of an automobile, which is characterized by comprising the following steps:
(1) Mixing organopolysiloxane polymer, terpene resin and solvent oil, adding filler and amorphous SiO during stirring 2 And hollow microspheres, stirring and mixing at 60-70deg.C for 20-30min;
(2) Placing the mixture into a vacuum stirrer, adding coupling agent and catalyst, stirring for 20-30min under vacuum, and sealing and packaging.
The structural adhesive for the automobile mute tire has the auxiliary effect on the noise reduction effect of the sound absorbing cotton due to the hollow microspheres contained in the components, and can further reduce the noise intensity of the tire between 200 and 250 Hz. In addition, the invention finds that the inorganic hollow microsphere has more advantages in noise reduction through experiments, and the polymer hollow microsphere can increase the toughness of the adhesive. Therefore, the technicians mix the inorganic hollow microspheres with the polymer hollow microspheres, and optimize the combination mode for improving the mechanical property and the noise reduction effect in a balanced way.
Drawings
FIG. 1 is a view of a polyaniline hollow microsphere under a microscope.
FIG. 2 is a view of a phenolic resin hollow microsphere under a microscope.
FIG. 3 is a view under a microscope of a silicone hollow microsphere.
FIG. 4 is a view under a microscope of epoxy hollow microsphere.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Glass hollow microsphere and SiO used in the specific embodiment of the invention 2 Hollow microsphere and TiO 2 The hollow microsphere is obtained from Siamiliaz biotechnology Co., ltd, has particle diameter of 10-50 μm, and bulk density of 0.2-0.5g/cm 3 。
Preparation of Polymer hollow microspheres
Preparation example 1 preparation of polyaniline hollow microspheres
S1: in a four-necked polymerization bottle, 60g of polyethylene glycol is dissolved in 90% ethanol water solution with the volume being 10 times that of the polyethylene glycol, nitrogen is introduced, the mixture is reacted for 10min at the constant temperature of 70 ℃, 180g of styrene monomer and 50g of benzoyl peroxide initiator are added, the mixture is stirred and polymerized for 10h at the temperature of 70 ℃, the temperature is raised to 80 ℃ to evaporate residual monomers and solvents, and the mixture is cooled to the room temperature to obtain polystyrene solid microspheres;
s2: modifying the surface of a polystyrene solid microsphere by using concentrated sulfuric acid, adding the modified polystyrene solid microsphere into an aniline monomer hydrochloric acid solution with the concentration of 0.5g/mL, polymerizing an aniline monomer on the surface of the polystyrene solid microsphere by using the polystyrene solid microsphere as a template, and dissolving the polystyrene template by using DMF (dimethyl formamide), thereby preparing the polyaniline hollow microsphere.
The microscopic image of the polyaniline hollow microsphere prepared by the invention is shown in figure 1, and the particle size of the hollow microsphere is 100-200 mu m.
Preparation example 2 preparation method of phenolic resin hollow microspheres
Adding 50g of azodiisobutyric acid serving as a foaming agent into a stirring container, adding 10g of tween-20 and 50g of deionized water, stirring for 20-30min, adding 500g of liquid phenolic aldehyde, stirring for 1h, heating to 80 ℃ to form a foam-like structure, spraying the foam into a preheated gas medium through an ejector, solidifying and drying in a drying box, wherein the inlet temperature of the drying box is 350-400 ℃, and preparing the phenolic resin hollow microspheres.
The microscopic image of the hollow microsphere of the phenolic resin prepared by the invention is shown in figure 2, and the microscopic image shows that the hollow microsphere of the phenolic resin prepared by the invention has serious polymerization, and the inventor can not overcome the polymerization problem by a plurality of technical improvements on the basis of the prior art, so the invention abandons the use of the hollow microsphere of the phenolic resin.
Preparation example 3 preparation of hollow microspheres of Silicone resin
S1: the polystyrene solid microspheres are prepared according to the method disclosed in the preparation example 1 and dispersed for standby;
s2: 100g of methyltrimethoxysilane is placed in a reaction kettle, 2 times of formic acid aqueous solution with the mass fraction of 0.01-0.02% is added, and the mixture is stirred and reacted for 3 hours at 50-55 ℃;
s3: and (2) modifying the surface of the polystyrene solid microsphere by using concentrated sulfuric acid, dispersing the modified polystyrene solid microsphere into the solution in the step (S2), adding ammonia water solution, polymerizing methyltrimethoxysilane monomer on the surface of the polystyrene solid microsphere by using the polystyrene solid microsphere as a template, and dissolving the polystyrene template by using DMF (dimethyl formamide), thereby preparing the silicone resin hollow microsphere.
The microscopic image of the hollow microsphere of the silicon resin prepared by the invention is shown in figure 3, and the particle size of the hollow microsphere is 20-100 mu m.
Preparation example 4 preparation of epoxy hollow microspheres
S1: taking 100g of bisphenol A epoxy resin monomer E-51 g, 12g of triethylene tetramine and 7g of alkylphenol ethoxylate, uniformly mixing at 40 ℃, and adding 40g of water under a stirring state to form emulsion;
s2: dripping the emulsion into ethylene glycol at 50-60 ℃ to form composite emulsion;
s3: heating the composite emulsion to 100 ℃ to react for 1h, solidifying the epoxy resin, filtering and washing to obtain the water-containing epoxy resin microspheres;
s4: and (3) carrying out vacuum drying on the aqueous epoxy resin for 24 hours, and removing the water to obtain the epoxy resin hollow microspheres.
The microscopic image of the epoxy resin hollow microsphere prepared by the invention is shown in figure 4, and the particle size of the hollow microsphere is 120-200 mu m.
Preparation of structural adhesive for automobile silent tire
Example 1
The components are as follows: hydroxyl-terminated polydimethylsiloxane 40 parts, terpene resin 30 parts, nano active calcium carbonate 20 parts, amorphous SiO 2 10 parts of glass hollow microspheres, 10 parts of vinyl trimethoxy silane, 5 parts of isopropyl titanate, 0.5 part of solvent oil and 20 parts of solvent oil.
The preparation method comprises the following steps: (1) Mixing organopolysiloxane polymer, terpene resin and solvent oil, adding filler and amorphous SiO during stirring 2 And hollow microspheres, stirring and mixing at 60 ℃ for 30min;
(2) Placing the mixed material into a vacuum stirrer, adding vinyl trimethoxy silane and isopropyl titanate, vacuumizing and stirring for 30min, and sealing and packaging.
Example 2
The preparation method is the same as in example 1, except that the glass hollow microspheres are replaced with the same mass fraction of SiO 2 Hollow microspheres.
Example 3
The preparation method is the same as in example 1, except that the glass hollow microspheres are replaced with the same mass fraction of TiO 2 Hollow microspheres.
Example 4
The preparation method is the same as in example 1, except that the glass hollow microspheres are replaced with the polyaniline hollow microspheres prepared in preparation example 1 in the same mass fraction.
Example 5
The preparation method was the same as in example 1 except that the glass hollow microspheres were replaced with the same mass fraction of the silicone hollow microspheres prepared in preparation example 3.
Example 6
The preparation method was the same as in example 1 except that the glass hollow microspheres were replaced with the same mass fraction of the epoxy resin hollow microspheres prepared in preparation example 4.
Comparative example 1
The preparation process was the same as in example 1, except that the raw materials did not contain glass hollow microspheres.
Effect examples
1. Adhesive property detection
The structural adhesives prepared in examples 1 to 6 and comparative example 1 were tested for performance data in accordance with GB/T528-1998 and the results are shown in the following table.
TABLE 1 structural adhesive performance data for silent tires
| Group of | Time of surface drying (min) | Tensile bond Strength (MPa) | Tear strength (KN/m) | Elongation at maximum strength (%) |
| Example 1 | 14 | 1.70 | 8.7 | 226 |
| Example 2 | 16 | 1.67 | 8.7 | 222 |
| Example 3 | 14 | 1.74 | 8.8 | 229 |
| Example 4 | 18 | 1.72 | 9.0 | 232 |
| Example 5 | 16 | 1.73 | 9.3 | 237 |
| Example 6 | 16 | 1.78 | 9.3 | 239 |
| Comparative example 1 | 20 | 1.70 | 9.0 | 230 |
As can be seen from the data in table 1, the addition of hollow microspheres to the adhesive reduced the tack-free time compared to the data in comparative example 1, and the inorganic hollow microspheres were more effective in reducing the tack-free time, as analyzed by the skilled artisan to be that the addition of hollow microspheres reduced the gel density and reduced the tack-free time. From the mechanical data of the adhesive, the adhesive strength of the adhesive is not remarkably improved by different hollow microsphere shell materials, and a fixing rule is not found in multiple parallel experiments. However, it is obvious that the addition of the hollow polymeric microspheres can increase the toughness of the adhesive, so that the elongation at break of the adhesive is increased, and the hollow silicone microspheres and the hollow epoxy microspheres are the most obvious. The addition of the inorganic hollow particles reduces the toughness of the adhesive. The tear resistance of the adhesive is positively correlated with the toughness change, namely, the polymer hollow microspheres can increase the tear resistance of the adhesive, and the inorganic hollow microspheres can reduce the tear resistance.
2. Tyre drum noise test
In general, when the running speed of the automobile exceeds 60km/h, tire noise will become one of the main noise sources of the automobile, which is generated because the air in the closed cavity inside the tire is excited by the road surface to generate resonance of a specific frequency, and the resonance is transmitted to the automobile body through the axle and the suspension system, so that low-frequency structural noise of 200-250Hz is formed in the automobile, and the NVH characteristics of the automobile are affected. The invention defines the noise data collected in the frequency range of 200-250Hz as the resonant noise of the tire cavity.
Test purpose: whether the structural adhesive prepared by the method has influence on the resonance noise of the tire cavity is detected.
The test method comprises the following steps: according to the early pre-experiment, the technical staff finds that the tire drop noise belongs to instant noise and can not well show the effect of the adhesive on improving the tire noise, and therefore, the invention explores the influence rule of the structural adhesive on the near-field noise of the rotating tire through the test of the tire indoor drum noise.
The test was carried out in a full noise elimination laboratory, the noise signal acquisition was carried out using an LMS multichannel signal acquisition system, an aluminum rim 6J X17 was used, the tire was 225/45R19 in the sun, the conventional polyurethane sound absorbing cotton was adhered to the inside of the tire using the structural adhesives prepared in examples 1-6 and comparative example 1 of the present invention, and the adhesive thickness was controlled at 3.+ -. 0.2mm. Tire air pressure 230KP, the tire after dynamic balance test is static on a test bench for 1h, and microphones are placed on the front and the side of the tire in the rotation direction by referring to GB/T32789-2016. Setting the tire load of 400kg, stabilizing the drum speed at 80km/h, starting noise test, testing 1 group of data every 1min, taking sound pressure value difference not exceeding 0.2dB as effective data, mainly analyzing noise with the frequency of 200-250Hz, and counting noise peaks in the frequency interval, wherein the results are shown in the following table.
Table 2 peaks of cavity noise in 200-250Hz tires
| Group of | Microphone (front)/dB | Microphone (side)/dB |
| Example 1 | 62.8 | 62.8 |
| Example 2 | 62.3 | 62.5 |
| Example 3 | 61.9 | 62.0 |
| Example 4 | 63.4 | 63.2 |
| Example 5 | 62.4 | 62.9 |
| Example 6 | 63.0 | 62.8 |
| Comparative example 1 | 64.7 | 65.5 |
From the above table data, it can be seen that the use of adhesives of different formulations to adhere the sound absorbing cotton has different effects on the noise reduction effect of the silent tire at frequencies between 200 Hz and 250 Hz. Comparing the noise peaks of the front microphone and the side microphone can find that the addition of the hollow microspheres in the structural adhesive can reduce the noise peaks, which indicates that the hollow microspheres have positive auxiliary effect on noise reduction of the silent tire. The skilled person considers that the hollow microsphere can reduce the quality of the silent tire, and the hollow microsphere has a damping effect and partially eliminates the noise intensity. From the noise peak data in the table above, it can be seen that the noise reduction effect of the inorganic hollow microspheres is better than that of the polymer resin hollow microspheres, and the technical analysis considers that the hollow microspheres have a conduction and absorption effect on a part of heat energy converted by acoustic energy in addition to a damping effect. In particular with TiO 2 The hollow microsphere is made of shell material, and the noise reduction effect is most obvious.
Combining the mechanical property test and tire drum noise test results of the structural adhesive, the present inventors selected the silicone hollow microspheres or epoxy hollow microspheres which are optimal for mechanical property improvement, and the TiO which is optimal for noise reduction effect, respectively 2 The hollow microspheres are used as an additive to prepare the structural adhesive.
The optimized scheme of the hollow microsphere addition mode is shown in the following table, and the preparation method is the same as that of example 1, except that 10 parts of the glass hollow microsphere in the original example 1 is replaced and combined as follows. The silicone hollow microspheres and epoxy hollow microspheres in the table refer to the products of preparation examples 3 and 4 of the present invention.
| TiO 2 Hollow microspheres/serving | Silicone hollow microspheres | |
| Scheme 1 | 9 | 1 |
| Scheme 2 | 8 | 2 |
| Scheme 3 | 6 | 4 |
| Scheme 4 | 5 | 5 |
| TiO 2 Hollow microspheres/serving | Hollow microsphere of epoxy resin | |
| Scheme 5 | 9 | 1 |
| Scheme 6 | 8 | 2 |
| Scheme 7 | 6 | 4 |
| Scheme 8 | 5 | 5 |
The mechanical properties of the structural adhesives prepared in schemes 1 to 8 were respectively verified according to the methods described above, and the noise reduction effect of the tire after application was confirmed.
3. Adhesive property detection
The structural adhesives prepared in schemes 1-8 were tested for performance data in accordance with GB/T528-1998 and the results are shown in the following table.
TABLE 3 structural adhesive performance data for silent tires
| Group of | Tensile bond Strength (MPa) | Tear strength (KN/m) | Elongation at maximum strength (%) |
| Scheme 1 | 1.72 | 8.8 | 232 |
| Scheme 2 | 1.74 | 9.1 | 232 |
| Scheme 3 | 1.73 | 9.2 | 236 |
| Scheme 4 | 1.73 | 9.2 | 236 |
| Scheme 5 | 1.73 | 9.0 | 236 |
| Scheme 6 | 1.75 | 9.0 | 236 |
| Scheme 7 | 1.73 | 9.2 | 237 |
| Scheme 8 | 1.76 | 9.3 | 236 |
4. Tyre drum noise test
The test method is the same as above, and the detection results are shown in the following table.
Table 4 peak 200-250Hz tire cavity noise
| Group of | Microphone (front)/dB | Microphone (side)/dB |
| Scheme 1 | 61.9 | 62.1 |
| Scheme 2 | 61.9 | 62.3 |
| Scheme 3 | 62.0 | 62.3 |
| Scheme 4 | 62.3 | 62.6 |
| Scheme 5 | 62.0 | 62.1 |
| Scheme 6 | 62.2 | 62.4 |
| Scheme 7 | 62.5 | 62.6 |
| Scheme 8 | 62.7 | 62.6 |
From the data of tables 3 and 4When the inorganic hollow microspheres and the organic resin hollow microspheres are combined and added into the adhesive, the adhesive has a neutralization effect which makes the best of the improvement of the mechanical and noise reduction effects of the adhesive. When combining the results of tables 3 and 4, when TiO 2 When the mass ratio of the hollow microspheres to the silicone hollow microspheres reaches 6:4, the improvement of the mechanical properties by adding the silicone hollow microspheres is not obvious, and the TiO is maintained 2 The amount of hollow microspheres helps to improve noise reduction, so TiO 2 The optimal combination ratio of the hollow microspheres to the silicone hollow microspheres is 6:4. Compared with the silicone hollow microsphere, the technical personnel find that the influence of the epoxy hollow microsphere on the noise reduction effect is more obvious, and the epoxy hollow microsphere is oriented to TiO 2 The hollow microspheres can obviously increase the resonance noise peak value of the tire by mixing the epoxy resin hollow microspheres in the hollow microspheres. Therefore, the most preferred polymeric hollow microspheres of the present invention are silicone hollow microspheres.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (4)
1. The structural adhesive for the automobile mute tire is characterized by comprising the following components in parts by weight: 30-40 parts of organopolysiloxane polymer, 30-40 parts of terpene resin, 10-20 parts of nano active calcium carbonate and amorphous SiO 2 10-15 parts of hollow microspheres, 2-15 parts of vinyl trimethoxy silane, 2-10 parts of isopropyl titanate, 0.5-1 part of solvent oil and 10-30 parts of solvent oil; the particle size of the hollow microspheres is 20-200 mu m, the hollow microspheres are the combination of polymer hollow microspheres and inorganic hollow microspheres, and the polymer hollow microspheres comprise one or the combination of two of epoxy resin hollow microspheres and silicone resin hollow microspheres; the inorganic hollow microsphere comprises TiO 2 Hollow microspheres;
the silicone hollow microsphere is prepared by the following method:
(1) The organic silicon monomer is subjected to hydrolysis reaction in formic acid aqueous solution with the mass fraction of 0.01-0.02% to form silanol solution; then condensation reaction is carried out under alkaline condition;
(2) Dispersing the polystyrene solid microspheres modified by concentrated sulfuric acid into silanol solution, adding ammonia water solution, polymerizing organic silicon monomers on the surfaces of the polystyrene solid microspheres, and dissolving a polystyrene template by DMF to obtain the silicone hollow microspheres;
wherein the organosilicon monomer comprises one or more than two of methyltrimethoxysilane, methyltriethoxysilane and vinyltrimethoxysilane;
the epoxy resin hollow microsphere is prepared by the following method:
(a) Uniformly mixing an epoxy resin monomer, a curing agent and a surfactant at 40 ℃, and adding water in a stirring state to form emulsion;
(b) Dripping the emulsion into ethylene glycol at 50-60 ℃ to form composite emulsion;
(c) Heating the composite emulsion to 100 ℃ to react for 1h, solidifying the epoxy resin, filtering and washing to obtain the water-containing epoxy resin microspheres;
(d) Vacuum drying the water-containing epoxy resin for 24 hours, and removing water to obtain epoxy resin hollow microspheres;
wherein the epoxy resin monomer is selected from one or more than two of bisphenol A type epoxy resin, bisphenol F type epoxy resin and bisphenol S type epoxy resin.
2. The structural adhesive of claim 1, wherein the hollow microspheres are TiO 2 The hollow microsphere and the silicone hollow microsphere are combined, and the mass ratio of the hollow microsphere to the silicone hollow microsphere is (10-1): 1 or the hollow microsphere is TiO 2 The hollow microsphere and the epoxy resin hollow microsphere are combined, and the mass ratio of the hollow microsphere to the epoxy resin hollow microsphere is (10-1): 1.
3. the structural adhesive of claim 2, wherein the hollow microspheres are TiO 2 And the mass ratio of the hollow microsphere to the silicone hollow microsphere is 3:2.
4. A method for preparing the structural adhesive for a silent tire of an automobile according to any one of claims 1 to 3, comprising the steps of:
(1) Mixing organopolysiloxane polymer, terpene resin and solvent oil, adding nano active calcium carbonate and amorphous SiO during stirring 2 And hollow microspheres, stirring and mixing at 60-70deg.C for 20-30min;
(2) Placing the mixture into a vacuum stirrer, adding vinyl trimethoxy silane and isopropyl titanate, vacuumizing, stirring for 20-30min, and sealing and packaging.
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| CN116285806A (en) * | 2022-11-15 | 2023-06-23 | 张家港爱科思汽车配件有限公司 | Structural adhesive for automobiles and preparation method thereof |
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| JPH1077409A (en) * | 1996-09-03 | 1998-03-24 | Yokohama Rubber Co Ltd:The | Silicone composition |
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