CN112724924A - Silicone structural adhesive for hollow glass and preparation method thereof - Google Patents
Silicone structural adhesive for hollow glass and preparation method thereof Download PDFInfo
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- CN112724924A CN112724924A CN202011590306.9A CN202011590306A CN112724924A CN 112724924 A CN112724924 A CN 112724924A CN 202011590306 A CN202011590306 A CN 202011590306A CN 112724924 A CN112724924 A CN 112724924A
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- parts
- component
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- structural adhesive
- hollow glass
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 77
- 239000000853 adhesive Substances 0.000 title claims abstract description 64
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 64
- 239000011521 glass Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000004014 plasticizer Substances 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- 239000000945 filler Substances 0.000 claims abstract description 19
- 229920002545 silicone oil Polymers 0.000 claims abstract description 19
- 239000006229 carbon black Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 239000007822 coupling agent Substances 0.000 claims abstract description 17
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 17
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 62
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 42
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 42
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 40
- -1 polydimethylsiloxane Polymers 0.000 claims description 36
- 239000002131 composite material Substances 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 33
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 229940008099 dimethicone Drugs 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical group CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 5
- 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 5
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 claims description 4
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 claims description 4
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 4
- NBJODVYWAQLZOC-UHFFFAOYSA-L [dibutyl(octanoyloxy)stannyl] octanoate Chemical compound CCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCC NBJODVYWAQLZOC-UHFFFAOYSA-L 0.000 claims description 4
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 claims description 4
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- PXGZUMCOTGAVEC-UHFFFAOYSA-N 3-[dimethoxy(penta-1,4-dien-3-yloxy)silyl]propane-1,1,1-triamine Chemical compound C(=C)C(O[Si](OC)(OC)CCC(N)(N)N)C=C PXGZUMCOTGAVEC-UHFFFAOYSA-N 0.000 claims description 3
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 claims description 3
- MNFGEHQPOWJJBH-UHFFFAOYSA-N diethoxy-methyl-phenylsilane Chemical compound CCO[Si](C)(OCC)C1=CC=CC=C1 MNFGEHQPOWJJBH-UHFFFAOYSA-N 0.000 claims description 3
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 3
- YLBPOJLDZXHVRR-UHFFFAOYSA-N n'-[3-[diethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CCO[Si](C)(OCC)CCCNCCN YLBPOJLDZXHVRR-UHFFFAOYSA-N 0.000 claims description 3
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 3
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 claims description 3
- VNBLTKHUCJLFSB-UHFFFAOYSA-N n-(trimethoxysilylmethyl)aniline Chemical compound CO[Si](OC)(OC)CNC1=CC=CC=C1 VNBLTKHUCJLFSB-UHFFFAOYSA-N 0.000 claims description 3
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 3
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 claims description 2
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical group O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims 2
- 229940083037 simethicone Drugs 0.000 claims 2
- 230000014759 maintenance of location Effects 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000035699 permeability Effects 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 239000000565 sealant Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000003292 glue Substances 0.000 description 7
- 238000007789 sealing Methods 0.000 description 5
- 229910021383 artificial graphite Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- FUXUUPOAQMPKOK-UHFFFAOYSA-N diethoxy-methyl-[2-(oxiran-2-ylmethoxy)ethyl]silane Chemical compound CCO[Si](C)(OCC)CCOCC1CO1 FUXUUPOAQMPKOK-UHFFFAOYSA-N 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000004590 silicone sealant Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- ZNXDCSVNCSSUNB-UHFFFAOYSA-N trimethoxy-[2-(oxiran-2-ylmethoxy)ethyl]silane Chemical compound CO[Si](OC)(OC)CCOCC1CO1 ZNXDCSVNCSSUNB-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- PWPGWRIGYKWLEV-UHFFFAOYSA-N dimethoxy-methyl-[2-(oxiran-2-ylmethoxy)ethyl]silane Chemical compound CO[Si](C)(OC)CCOCC1CO1 PWPGWRIGYKWLEV-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- RWJUTPORTOUFDY-UHFFFAOYSA-N triethoxy-[2-(oxiran-2-ylmethoxy)ethyl]silane Chemical compound CCO[Si](OCC)(OCC)CCOCC1CO1 RWJUTPORTOUFDY-UHFFFAOYSA-N 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- 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
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a silicone structural adhesive for hollow glass and a preparation method thereof. The silicone structural adhesive for the hollow glass comprises a component A and a component B, wherein the component A is prepared from the following components in parts by weight: 100 parts of organopolysiloxane polymer, 60-150 parts of filler and 5-25 parts of plasticizer; the component B is prepared from the following raw materials in parts by weight: 100 parts of dimethyl silicone oil, 50-150 parts of carbon black, 60.5-10 parts of KS-, 15-60 parts of a cross-linking agent, 15-60 parts of a coupling agent and 0.1-1.5 parts of a catalyst. The silicone structural adhesive for the hollow glass has high bonding strength, low water vapor permeability and high-temperature strength retention rate.
Description
Technical Field
The invention relates to the field of adhesives, in particular to a silicone structural adhesive for hollow glass and a preparation method thereof.
Background
At present, the national attention on energy-saving and environment-friendly materials is higher and higher, the application of hollow glass in building material decoration, energy conservation, vehicles, refrigeration equipment and other aspects is gradually improved, the requirements of users on the quality and the price of the hollow glass are stricter, the hollow glass is required to deform along with the shape of a sealing surface, the hollow glass is not easy to flow, the cohesiveness is strong, and the service life is long. The silicone structural adhesive is an adhesive used for filling a structural gap to play a role in sealing, and has the functions of leakage prevention, water prevention, vibration prevention, sound insulation, heat insulation and the like. However, the existing sealant is easy to fall off and turn yellow under the influence of the environment or the structure of the sealant, and has low strength and large structural change at high temperature. The performance needs to be significantly improved and the production costs to be reduced, which is compelling to national and industrial standards.
The hollow glass is a glass product formed by uniformly separating two or more pieces of glass by effective support and bonding and sealing the periphery of the glass so as to form a dry gas space between glass layers. The main materials are glass, warm edge spacing strips, angle bending bolts and silicone structural adhesive. The outer sealant is an important material for forming the hollow glass unit, and the quality of the outer sealant directly influences the service life of the hollow glass unit. Therefore, in order to prolong the service life of the hollow glass, the adhesiveness and stability of the external sealant are required to be improved. Silica is a reinforcing material for structural adhesives and also a good tackifying filler. The sealant needs to be reasonably adjusted between strength and viscosity, so that higher strength is achieved and good bonding performance is achieved. The existing hollow glass sealant has poor strength and viscosity capability, low high-temperature strength retention rate and short service life, so that expensive maintenance cost is consumed and potential safety hazards are increased. Therefore, the development of the hollow glass outer channel sealant with excellent performance, strong adhesion, low water vapor permeability and high-temperature strength retention rate can integrally improve the quality of the hollow glass, prolong the service life of the hollow glass and have great practical significance and economic value.
In patent CN 106281205A, a graphene oxide two-dimensional layered nano material is introduced to modify a silicone sealant, so that the barrier property and the mechanical strength of the silicone sealant are improved, but the preparation method is complex and the graphene is easy to agglomerate, which is not beneficial to actual production. In the patent CN 107090257A, the comprehensive performance of the structural adhesive is improved by introducing the modified butyl rubber, but the resin adhesive is introduced to cause the slow curing rate of the structural adhesive, which is not beneficial to actual construction. The patent CN 107057584A improves the mechanical property of the sealant by adding the nanometer copper powder, which also increases the manufacturing cost obviously.
Disclosure of Invention
Accordingly, an object of the present invention is to provide a silicone structural adhesive for hollow glass, which has high adhesive strength, low water vapor permeability, and high-temperature strength retention.
In order to achieve the purpose, the invention adopts the following scheme:
the silicone structural adhesive for hollow glass comprises a component A and a component B, wherein the component A is prepared from the following components in parts by weight:
organopolysiloxane polymer 100 parts
60-150 parts of filler
5-25 parts of a plasticizer;
the component B is prepared from the following raw materials in parts by weight:
in some embodiments, the component A is prepared from the following components in parts by weight:
organopolysiloxane polymer 100 parts
90-110 parts of filler
8-12 parts of a plasticizer;
the component B is prepared from the following raw materials in parts by weight:
in some embodiments, the component A is prepared from the following components in parts by weight:
organopolysiloxane polymer 100 parts
100 portions of filler
10 parts of a plasticizer;
the component B is prepared from the following raw materials in parts by weight:
in some of the embodiments, the mass ratio of the component A to the component B is 9-14: 1.
In some of the embodiments, the mass ratio of the component A to the component B is 9-11: 1.
In some of these embodiments, the mass ratio of the a component to the B component is 10: 1.
In some of these embodiments, the organopolysiloxane polymer is one or more of a hydroxyl terminated polydimethylsiloxane, an alkoxy terminated polydimethylsiloxane, an alkyl terminated polydimethylsiloxane.
In some of these embodiments, the organopolysiloxane polymer is a hydroxyl terminated polydimethylsiloxane having a viscosity of 10000 to 60000 mPa-s at 25 ℃.
In some of these embodiments, the organopolysiloxane polymer is a low viscosity terminal hydroxyl terminated polydimethylsiloxane having a viscosity of 15000mPa · s to 25000mPa · s at 25 ℃ and a high viscosity terminal hydroxyl terminated polydimethylsiloxane having a viscosity of 45000mPa · s to 55000mPa · s at 25 ℃.
In some of the embodiments, the mass ratio of the low viscosity end hydroxyl terminated polydimethylsiloxane to the high viscosity end hydroxyl terminated polydimethylsiloxane is 1: 1.2-1.8.
In some of these embodiments, the filler is nano-activated calcium carbonate.
In some of the embodiments, the nano active calcium carbonate has a particle size of 50 to 500 nm.
In some of the embodiments, the nano active calcium carbonate has a particle size of 50 to 200 nm.
In some of the embodiments, the nano active calcium carbonate has a particle size of 50-150 nm.
In some embodiments, the nano active calcium carbonate has a particle size of 80-120 nm.
In some embodiments, the nano active calcium carbonate has a particle size of 90-110 nm.
In some embodiments, the filler is small-particle nano active calcium carbonate and large-particle nano active calcium carbonate, the small-particle nano active calcium carbonate has a particle size of 50-120 nm, and the large-particle nano active calcium carbonate has a particle size of 180-220 nm.
In some embodiments, the mass ratio of the small-particle-size nano active calcium carbonate to the large-particle-size nano active calcium carbonate is 1: 0.8-1.2.
In some of these embodiments, the plasticizer is one or more of dimethicone, methylphenyl silicone oil, and hydroxy silicone oil.
In some of these embodiments, the plasticizer is a dimethicone having a viscosity of from 200 to 1200 mPa-s at 25 ℃.
In some of these embodiments, the plasticizer is a low viscosity dimethylsilicone oil having a viscosity of 300 to 500 mPa.s at 25 ℃ and a high viscosity dimethylsilicone oil having a viscosity of 800 to 1100 mPa.s at 25 ℃.
In some embodiments, the mass ratio of the low-viscosity dimethyl silicone oil to the high-viscosity dimethyl silicone oil is 1: 1.2-1.8.
In some of these embodiments, the dimethicone of the B component has a viscosity of from 300 to 1500mPa s at 25 ℃.
In some of these embodiments, the dimethicone of the B component has a viscosity of from 800 to 1200mPa s at 25 ℃.
In some of these embodiments, the crosslinking agent is one or more of ethyl orthosilicate, propyl orthosilicate, polyethyl silicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, polymethyltriethoxysilane oligomer, phenyltrimethoxysilane, phenyltriethoxysilane, methylphenyldimethoxysilane, methylphenyldiethoxysilane, diphenyldimethoxysilane, and diphenyldiethoxysilane.
In some of these embodiments, the coupling agent is gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, epoxycyclohexylmethyldimethoxysilane, epoxycyclohexylmethyldiethoxysilane, 3-chloropropyltrimethoxysilane, 3-chloropropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, gamma-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-, One or more of N- (2-aminoethyl) -3-aminopropyltriethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldiethoxysilane, phenylaminomethyltrimethoxysilane, phenylaminomethyltriethoxysilane, and divinyltriaminopropyltrimethoxysilane.
In some of these embodiments, the catalyst is one or more of dibutyl tin dilaurate, dibutyl tin diacetate, dibutyl tin dioctoate, isopropyl titanate, and n-butyl titanate.
The invention also provides a preparation method of the silicone structural adhesive for hollow glass.
The specific technical scheme is as follows:
the preparation method of the silicone structural adhesive for hollow glass comprises the following steps:
preparation of component A: stirring and mixing the organic polysiloxane polymer, the plasticizer and the filler for 10-200 min at the temperature of 60-120 ℃ to obtain the composite material;
preparation of the component B: stirring and mixing the dimethyl silicone oil, the KS-6 and the carbon black for 10-60 min at the temperature of 80-140 ℃, then adding the cross-linking agent, the coupling agent and the catalyst, and stirring for 10-100 min at the temperature of 80-140 ℃ under the protection of nitrogen to obtain the composite material;
and then uniformly mixing the component A and the component B to obtain the silicone structural adhesive for the hollow glass.
In some embodiments, the preparation method of the silicone structural adhesive for hollow glass comprises the following steps:
preparation of component A: mixing the organic polysiloxane polymer and a plasticizer, adding the filler in the stirring process to enable the organic polysiloxane polymer and the plasticizer to cover the powder to form a self-leveling base material, and stirring and mixing the obtained base material for 40-80 min at the temperature of 70-90 ℃ to obtain the composite material;
preparation of the component B: stirring and mixing the dimethyl silicone oil, the KS-6 and the carbon black for 20-40 min at the temperature of 90-110 ℃ and the vacuum degree of-0.09-0.1 MPa, then adding the cross-linking agent, the coupling agent and the catalyst, and stirring for 10-20 min at the temperature of 90-110 ℃ under the protection of nitrogen to obtain the composite material;
and then uniformly mixing the component A and the component B under the condition that the vacuum degree is-0.09 to-0.1 MPa to obtain the silicone structural adhesive for the hollow glass.
Compared with the prior art, the invention has the following beneficial effects:
the invention aims at solving the problems of low strength, short service life and low high-temperature strength retention rate of the existing silicone structural adhesive, a certain amount of organopolysiloxane polymer, filler and plasticizer are used for preparing the component A, and a small amount of KS-6 is added to the raw materials for preparing the component B to replace partial carbon black on the basis of a certain amount of dimethyl silicone oil, carbon black, a crosslinking agent, a coupling agent and a catalyst, so that the prepared silicone structural adhesive has high bonding strength, low water vapor permeability and high-temperature strength retention rate. KS-6 is an artificial graphite, which is a focused form of nanoscale primary particles, has a high strength structure, has a moderate specific surface area and a high anisotropy, and has a size in the single crystal range ten times larger than that of carbon black particles. The addition of a small amount of KS-6 can improve the connectivity and the dispersibility between the carbon black and each component, thereby improving the tensile strength, the high-temperature tensile strength retention rate and the water-soaking cohesiveness of the obtained silicone structural adhesive under the standard condition and the low-temperature condition, and meeting the requirements of special buildings, automobiles, electronic and electric appliances and the like in various aspects.
Furthermore, the types, the use amounts and the viscosities of the organopolysiloxane polymer and the plasticizer in the component A and the types and the particle sizes of the fillers are optimized, the fillers with different particle sizes, the organopolysiloxane polymer and the plasticizer with different viscosities are selected for compounding, a synergistic effect can be generated, and the strength and the high-temperature strength retention rate of the silicone structural adhesive under standard conditions and low-temperature conditions can be further improved.
The silicone structural adhesive for hollow glass has the advantages of simple synthesis process, strong cohesiveness and controllable production process, is suitable for batch continuous production, and can meet the use requirements in various aspects.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to only those steps or modules listed, but may alternatively include other steps not listed or inherent to such process, method, article, or device.
The "plurality" referred to in the present invention means two or more. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
The viscosity in the present invention means a viscosity at 25 ℃.
The composite cross-linking agent can be any one of ethyl orthosilicate, propyl orthosilicate, polyethyl silicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, polymethyltriethoxysilane oligomer, phenyltrimethoxysilane, phenyltriethoxysilane, methylphenyldimethoxysilane, methylphenyldiethoxysilane, diphenyldimethoxysilane and diphenyldiethoxysilane, or a mixture of any two or more of the two or more of. The composite cross-linking agent in the following examples is specifically: the mixture is prepared by compounding tetraethoxysilane, phenyltrimethoxysilane and diphenyldimethoxysilane in a mass ratio of 1:1: 1.
The composite coupling agent can be gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, epoxycyclohexylmethyldimethoxysilane, epoxycyclohexylmethyldiethoxysilane, 3-chloropropyltrimethoxysilane, 3-chloropropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidyloxyethyltriethoxysilane, gamma-glycidyloxyethyltrimethoxysilane, glycidyloxyethylmethyldiethoxysilane, glycidyloxyethyltriethoxysilane, glycidyloxyethyltrimethoxysilane, glycidyloxypropyltriethoxysilane, glycidyloxyethyltrimethoxysilane, glycidyloxypropyltriethoxysilane, glycidyloxyethylmethyldimethoxysilane, glycidyloxyethylmethyldiethoxysilane, glycidyloxy, Any one of N- (2-aminoethyl) -3-aminopropyltriethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldiethoxysilane, phenylaminomethyltrimethoxysilane, phenylaminomethyltriethoxysilane and divinyltriaminopropyltrimethoxysilane, or a mixture of any two or more thereof compounded in any ratio. The composite coupling agent in the following examples is specifically: gamma-glycidoxypropyltrimethoxysilane, 3-chloropropyltrimethoxysilane and N- (2-aminoethyl) -3-aminopropyltrimethoxysilane are compounded according to the mass ratio of 1:1: 1.
The composite catalyst can be any one of dibutyl tin dilaurate, dibutyl tin diacetate, dibutyl tin dioctoate, isopropyl titanate and n-butyl titanate, or a mixture of any two or more of dibutyl tin dilaurate, dibutyl tin diacetate, dibutyl tin dioctoate, isopropyl titanate and n-butyl titanate which are compounded in any proportion. The composite catalyst in the following examples is specifically: the mixture is prepared by compounding dibutyl tin dilaurate and isopropyl titanate according to the mass ratio of 1:1.
The following are specific examples.
Example 1:
the component A comprises the following components in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas and 10 parts of dimethicone with the viscosity of 400 mPas are taken and added into a kneader to be stirred and dispersed, after 5min, 100 parts of nano active calcium carbonate with the particle size of 100nm is added into the kneader in the stirring process, so that glue (namely the hydroxyl-terminated polydimethylsiloxane and the dimethicone) completely covers the powder to form a self-leveling base material, the reaction temperature is controlled to be 80 ℃, and the component A is obtained by stirring and mixing for 1h and is used for grinding.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s, 4 parts of artificial graphite KS-6 and 96 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
Example 2:
the component A comprises the following components in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas and 10 parts of dimethicone with the viscosity of 400 mPas are added into a kneader to be stirred and dispersed, after 5min, 100 parts of nano active calcium carbonate with the particle size of 200nm is added into the kneader in the stirring process to ensure that the glue completely covers the powder to form a self-leveling base material, the reaction temperature is controlled at 80 ℃, and the mixture is stirred and mixed for 1h to obtain a component A which is ground for later use.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s, 4 parts of KS-6 and 96 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
Example 3:
the component A comprises the following components in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas and 10 parts of dimethicone with the viscosity of 400 mPas are added into a kneader to be stirred and dispersed, 50 parts of 100nm nano active calcium carbonate with the particle size of 50nm and 200nm is added into the kneader after 5min in the stirring process to ensure that the glue completely covers the powder to form a self-leveling base material, the reaction temperature is controlled at 80 ℃, and the components A are obtained by stirring and mixing for 1h and are ground for later use.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s, 4 parts of KS-6 and 96 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
Example 4:
the component A comprises the following components in parts by weight:
adding 40 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas, 60 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 50000 mPas and 10 parts of dimethicone with the viscosity of 400 mPas into a kneader, stirring and dispersing, adding 50 parts of 100nm and 50 parts of 200nm nano active calcium carbonate into the mixture in the stirring process after 5min to ensure that the glue completely covers the powder to form a self-leveling base material, controlling the reaction temperature to be 80 ℃, stirring and mixing for 1h to obtain a component A, and grinding for later use.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s, 4 parts of KS-6 and 96 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
Example 5:
the component A comprises the following components in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas and 4 parts of dimethicone with the viscosity of 400 mPas and 6 parts of dimethicone with the viscosity of 1000 mPas are added into a kneader to be stirred and dispersed, 50 parts of 100nm and 50 parts of 200nm nano active calcium carbonate are added into the mixture in the stirring process after 5min, so that the glue completely covers the powder to form a self-leveling base material, the reaction temperature is controlled to be 80 ℃, and the mixture is stirred and mixed for 1h to obtain a component A which is ground for later use.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s, 4 parts of KS-6 and 96 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
Example 6:
the component A comprises the following components in parts by weight:
adding 40 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas, 60 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 50000 mPas and 4 parts of dimethylsilicone with the viscosity of 400 mPas and 6 parts of dimethylsilicone with the viscosity of 1000 mPas into a kneader, stirring and dispersing, adding 50 parts of 100nm and 50 parts of 200nm nano active calcium carbonate into the mixture in the stirring process after 5min to ensure that the glue completely covers the powder to form a self-leveling base material, controlling the reaction temperature to be 80 ℃, stirring and mixing for 1h to obtain a component A, and grinding the component A for later use.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s, 4 parts of KS-6 and 96 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
Comparative example 1:
the component A comprises the following components in parts by weight:
100 parts of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas and 10 parts of dimethicone with the viscosity of 400 mPas are added into a kneader to be stirred and dispersed, after 5min, 100 parts of nano active calcium carbonate with the particle size of 100nm is added into the kneader in the stirring process to ensure that the glue completely covers the powder to form a self-leveling base material, the reaction temperature is controlled to be 80 ℃, the mixture is stirred and mixed for 1h to obtain a base material A, and the base material A is ground for later use.
The component B (in parts by weight) is as follows:
adding 100 parts of dimethyl silicone oil with the viscosity of 1000mPa & s and 100 parts of carbon black into a planetary machine, stirring in vacuum (the vacuum degree is-0.095 MPa), keeping the temperature at 100 ℃ for 30min after the temperature is stabilized, adding 50 parts of composite cross-linking agent, 50 parts of composite coupling agent and 1 part of composite catalyst, and stirring for 10min at constant 100 ℃ under the protection of nitrogen to obtain a component B;
and uniformly mixing the component A and the component B in a planetary stirrer according to the mixing volume ratio of 10:1 by vacuumizing (the vacuum degree is-0.095 MPa), so as to obtain the silicone structural adhesive for the hollow glass, and preparing the silicone structural adhesive into an H-shaped test piece for detecting the tensile cohesiveness of the test piece.
The silicone structural adhesives for hollow glass prepared in examples 1 to 6 and comparative example 1 were tested according to GB-24266 and the results are shown in Table 1 below.
TABLE 1
As can be seen from the data in Table 1: the silicone structural adhesive for the hollow glass has high tensile bonding strength under standard conditions and low temperature conditions, has higher high-temperature strength retention rate, can prolong the service life of the structural adhesive in harsh environments, has good sealing effect and high water-soaking bonding property, can effectively maintain the stability of an interlayer in the hollow glass, and prolongs the service life of the hollow glass.
Compared with the example 1, the tensile bonding strength of the prepared silicone structural adhesive under the standard condition and the tensile bonding strength under the high and low temperature conditions are both obviously lower than that of the example 1 due to the fact that the artificial graphite KS-6 is not added, and the water-soaking bonding property is also obviously reduced, which shows that the mechanical property and the water-soaking sealing property of the silicone structural adhesive can be obviously improved after the artificial graphite KS-6 is introduced into the component B. The main reason is that the KS-6 is favorable for the dispersion of the carbon black, and the unique scale structure on the surface of the KS-6 is favorable for the reaction between the KS-6 and different components, so that the overall strength of the sealant can be improved.
Comparing the performance data of the examples 1 to 3, it can be known that the particle size of the nano activated calcium carbonate has an influence on the mechanical properties of the obtained silicone structural adhesive, the filling effect of the 100nm nano activated calcium carbonate is better, and the mechanical properties of the silicone structural adhesive added with the 100nm nano activated calcium carbonate are better than those of the silicone structural adhesive added with the 200nm nano activated calcium carbonate; and when two kinds of nano active calcium carbonate with different sizes (100nm and 200nm) are mixed, the mechanical property of the obtained silicone structural adhesive is obviously improved, a certain synergistic effect is provided between the nano active calcium carbonate with different particle sizes, and a gap filling effect exists between particles, so that the nano active calcium carbonate is in full contact with polydimethylsiloxane in the stirring process, and the integral strength of the sealant can be obviously improved.
Comparing the performance data of the examples 1 and 4-6, it is known that the overall mechanical properties of the obtained silicone structural adhesive can be further improved by selecting two polydimethylsiloxanes with different viscosities from the component A and mixing the two polydimethylsiloxanes with different viscosities, and the tensile adhesive strength under the standard condition and the low temperature condition and the strength retention rate under the high temperature condition can be further improved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The silicone structural adhesive for hollow glass is characterized by comprising a component A and a component B, wherein the component A is prepared from the following components in parts by weight:
organopolysiloxane polymer 100 parts
60-150 parts of filler
5-25 parts of a plasticizer;
the component B is prepared from the following raw materials in parts by weight:
2. the silicone structural adhesive for hollow glass according to claim 1, wherein the component A is prepared from the following components in parts by weight:
organopolysiloxane polymer 100 parts
90-110 parts of filler
8-12 parts of a plasticizer;
the component B is prepared from the following raw materials in parts by weight:
3. the silicone structural adhesive for hollow glass according to claim 2, wherein the component A is prepared from the following components in parts by weight:
organopolysiloxane polymer 100 parts
100 portions of filler
10 parts of a plasticizer;
the component B is prepared from the following raw materials in parts by weight:
4. the silicone structural adhesive for hollow glass according to claim 1, wherein the mass ratio of the component A to the component B is 9-14: 1, preferably 9-11: 1, and more preferably 10: 1.
5. The silicone structural adhesive for hollow glass according to claim 1, wherein the organopolysiloxane polymer is one or more of hydroxyl-terminated polydimethylsiloxane, alkoxy-terminated polydimethylsiloxane, and alkyl-terminated polydimethylsiloxane;
preferably, the organopolysiloxane polymer is a hydroxyl-terminated polydimethylsiloxane having a viscosity of 10000 to 60000 mPa-s at 25 ℃;
preferably, the organopolysiloxane polymer is a low viscosity terminal hydroxyl terminated polydimethylsiloxane having a viscosity of 15000mPa · s to 25000mPa · s at 25 ℃ and a high viscosity terminal hydroxyl terminated polydimethylsiloxane having a viscosity of 45000mPa · s to 55000mPa · s at 25 ℃;
preferably, the mass ratio of the low-viscosity end hydroxyl-terminated polydimethylsiloxane to the high-viscosity end hydroxyl-terminated polydimethylsiloxane is 1: 1.2-1.8.
6. The silicone structural adhesive for hollow glass according to claim 1, wherein the filler is nano activated calcium carbonate;
preferably, the particle size of the nano active calcium carbonate is 50-500 nm, more preferably 50-200 nm, and more preferably 50-150 nm;
preferably, the filler is small-particle-size nano active calcium carbonate and large-particle-size nano active calcium carbonate, the particle size of the small-particle-size nano active calcium carbonate is 50-120 nm, and the particle size of the large-particle-size nano active calcium carbonate is 180-220 nm;
preferably, the mass ratio of the small-particle-size nano active calcium carbonate to the large-particle-size nano active calcium carbonate is 1: 0.8-1.2.
7. The silicone structural adhesive for hollow glass according to claim 1, wherein the plasticizer is one or more of dimethicone, methylphenyl silicone oil and hydroxy silicone oil;
preferably, the plasticizer is simethicone, and the viscosity of the simethicone at 25 ℃ is 200-1200 mPas;
preferably, the plasticizer is low-viscosity dimethylsilicone oil having a viscosity of 300 to 500 mPa.s at 25 ℃ and high-viscosity dimethylsilicone oil having a viscosity of 800 to 1100 mPa.s at 25 ℃;
preferably, the mass ratio of the low-viscosity dimethyl silicone oil to the high-viscosity dimethyl silicone oil is 1: 1.2-1.8.
8. The silicone structural adhesive for hollow glass according to any one of claims 1 to 7, wherein the viscosity of the dimethylsilicone oil in the B component at 25 ℃ is 300 mPa-s to 1500 mPa-s; and/or the presence of a gas in the gas,
the cross-linking agent is one or more of ethyl orthosilicate, propyl orthosilicate, polyethyl silicate, methyltrimethoxysilane, methyltriethoxysilane, vinyl trimethoxysilane, polymethyltriethoxysilane oligomer, phenyltrimethoxysilane, phenyltriethoxysilane, methylphenyldimethoxysilane, methylphenyldiethoxysilane, diphenyldimethoxysilane and diphenyldiethoxysilane; and/or the presence of a gas in the gas,
the coupling agent is gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, epoxycyclohexylmethyldimethoxysilane, epoxycyclohexylmethyldiethoxysilane, 3-chloropropyltrimethoxysilane, 3-chloropropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltriethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, one or more of N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldiethoxysilane, phenylaminomethyltrimethoxysilane, phenylaminomethyltriethoxysilane, and divinyltriaminopropyltrimethoxysilane; and/or the presence of a gas in the gas,
the catalyst is one or more of dibutyl tin dilaurate, dibutyl tin diacetate, dibutyl tin dioctoate, isopropyl titanate and n-butyl titanate.
9. The preparation method of the silicone structural adhesive for hollow glass according to any one of claims 1 to 8, comprising the following steps:
preparation of component A: stirring and mixing the organic polysiloxane polymer, the plasticizer and the filler for 10-200 min at the temperature of 60-120 ℃ to obtain the composite material;
preparation of the component B: stirring and mixing the dimethyl silicone oil, the KS-6 and the carbon black for 10-60 min at the temperature of 80-140 ℃, then adding the cross-linking agent, the coupling agent and the catalyst, and stirring for 10-100 min at the temperature of 80-140 ℃ under the protection of nitrogen to obtain the composite material;
and then uniformly mixing the component A and the component B to obtain the silicone structural adhesive for the hollow glass.
10. The method for preparing the silicone structural adhesive for hollow glass according to claim 9, comprising the following steps:
preparation of component A: mixing the organic polysiloxane polymer and a plasticizer, adding the filler in the stirring process to enable the organic polysiloxane polymer and the plasticizer to cover the powder to form a self-leveling base material, and stirring and mixing the obtained base material for 40-80 min at the temperature of 70-90 ℃ to obtain the composite material;
preparation of the component B: stirring and mixing the dimethyl silicone oil, the KS-6 and the carbon black for 20-40 min at the temperature of 90-110 ℃ and the vacuum degree of-0.09-0.1 MPa, then adding the cross-linking agent, the coupling agent and the catalyst, and stirring for 10-20 min at the temperature of 90-110 ℃ under the protection of nitrogen to obtain the composite material;
and then uniformly mixing the component A and the component B under the condition that the vacuum degree is-0.09 to-0.1 MPa to obtain the silicone structural adhesive for the hollow glass.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114045150A (en) * | 2021-11-12 | 2022-02-15 | 湖北回天新材料股份有限公司 | Multifunctional silica gel for indoor decoration and preparation method thereof |
CN114773379A (en) * | 2022-05-10 | 2022-07-22 | 广州市白云化工实业有限公司 | Modified siloxane, heat-resistant silicone structural sealant and preparation method thereof |
CN115895584A (en) * | 2022-12-06 | 2023-04-04 | 江西晨光新材料股份有限公司 | Silicone elastic sealant for hollow glass and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104017534A (en) * | 2014-05-07 | 2014-09-03 | 深圳百丽春新材料科技有限公司 | Transparent organic silicon LED light bar pouring sealant and preparation method thereof |
CN106085342A (en) * | 2016-06-12 | 2016-11-09 | 江苏明昊新材料科技股份有限公司 | One pack system high thermal conductive silicon ketone glue and preparation method thereof |
-
2020
- 2020-12-29 CN CN202011590306.9A patent/CN112724924B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104017534A (en) * | 2014-05-07 | 2014-09-03 | 深圳百丽春新材料科技有限公司 | Transparent organic silicon LED light bar pouring sealant and preparation method thereof |
CN106085342A (en) * | 2016-06-12 | 2016-11-09 | 江苏明昊新材料科技股份有限公司 | One pack system high thermal conductive silicon ketone glue and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
杨华明等: "《矿尾废渣的材料化加工与应用》", 30 September 2017, 冶金工业出版社 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114045150A (en) * | 2021-11-12 | 2022-02-15 | 湖北回天新材料股份有限公司 | Multifunctional silica gel for indoor decoration and preparation method thereof |
CN114773379A (en) * | 2022-05-10 | 2022-07-22 | 广州市白云化工实业有限公司 | Modified siloxane, heat-resistant silicone structural sealant and preparation method thereof |
CN114773379B (en) * | 2022-05-10 | 2023-08-15 | 广州市白云化工实业有限公司 | Modified siloxane, heat-resistant silicone structural sealant and preparation method thereof |
CN115895584A (en) * | 2022-12-06 | 2023-04-04 | 江西晨光新材料股份有限公司 | Silicone elastic sealant for hollow glass and preparation method thereof |
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