CN116218457A - Silicone structural sealant and preparation method and application thereof - Google Patents
Silicone structural sealant and preparation method and application thereof Download PDFInfo
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- CN116218457A CN116218457A CN202310194136.XA CN202310194136A CN116218457A CN 116218457 A CN116218457 A CN 116218457A CN 202310194136 A CN202310194136 A CN 202310194136A CN 116218457 A CN116218457 A CN 116218457A
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- mesoporous silica
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 96
- 239000000565 sealant Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 242
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 108
- 239000006185 dispersion Substances 0.000 claims abstract description 72
- 229920002050 silicone resin Polymers 0.000 claims abstract description 58
- 239000007788 liquid Substances 0.000 claims abstract description 55
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 53
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 53
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 52
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 52
- 150000001875 compounds Chemical class 0.000 claims abstract description 41
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 229920005601 base polymer Polymers 0.000 claims abstract description 19
- 239000004014 plasticizer Substances 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 18
- 239000011148 porous material Substances 0.000 claims description 64
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 50
- 238000000034 method Methods 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 25
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 24
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 15
- 239000006229 carbon black Substances 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 14
- 239000003431 cross linking reagent Substances 0.000 claims description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229940083037 simethicone Drugs 0.000 claims description 5
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 4
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- ZOTKGMAKADCEDH-UHFFFAOYSA-N 5-triethoxysilylpentane-1,3-diamine Chemical compound CCO[Si](OCC)(OCC)CCC(N)CCN ZOTKGMAKADCEDH-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 claims description 3
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 12
- 230000008569 process Effects 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 19
- 229920005989 resin Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 12
- 230000001965 increasing effect Effects 0.000 description 7
- 230000003014 reinforcing effect Effects 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 230000032683 aging Effects 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000009396 hybridization Methods 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 4
- 239000002808 molecular sieve Substances 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- 230000035882 stress Effects 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012229 microporous material Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000001066 destructive effect Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 229920001558 organosilicon polymer Polymers 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000006178 methyl benzyl group Chemical group 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- MKTRXTLKNXLULX-UHFFFAOYSA-P pentacalcium;dioxido(oxo)silane;hydron;tetrahydrate Chemical compound [H+].[H+].O.O.O.O.[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O MKTRXTLKNXLULX-UHFFFAOYSA-P 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
- H01L31/0481—Encapsulation of modules characterised by the composition of the encapsulation material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/204—Applications use in electrical or conductive gadgets use in solar cells
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention provides a silicone structural sealant, a preparation method and application thereof, and relates to the technical field of sealants. The silicone structural sealant includes: a component A and a component B; the component A comprises the following components: 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler; the compound intermediate comprises: 9.9 to 19.6 parts of cubic mesoporous silica, 98.7 to 99.1 parts of alpha, omega-dihydroxy polydimethylsiloxane and 10.4 to 14.1 parts of phenyl silicone resin; the cubic phase mesoporous silica, the alpha, omega-dihydroxyl polydimethylsiloxane and the phenyl silicone resin are dispersed in a dispersion liquid, and then the dispersion liquid is removed after blending, so as to form a compound intermediate. The silicone structural sealant has excellent creep resistance, mechanical property, strength, elongation and strength retention.
Description
Technical Field
The invention relates to the technical field of sealants, in particular to a silicone structural sealant and a preparation method and application thereof.
Background
Silicone structural sealants are generally required to bear large dynamic and static loads, and the application environments are complex and variable, and the silicone structural sealants themselves are required to have excellent heat resistance, ultraviolet resistance, damp heat resistance, acid and alkali resistance, creep resistance and durable high-strength retention.
The main resin of the silicone structural sealant is hydroxyl-terminated polydimethylsiloxane, and the hydroxyl-terminated polydimethylsiloxane has a flexible macromolecular chain structure, and has lower modulus and poorer creep resistance after colloid curing. In addition, in the use process of the silicone structural sealant, gravity, load and the like can aggravate creep of the silicone structural sealant, and finally the safety of a system is affected.
Disclosure of Invention
The invention provides a silicone structure sealant and a preparation method and application thereof, and aims to solve the problems of low modulus and poor creep resistance of the traditional silicone structure sealant.
In a first aspect of the present invention, there is provided a silicone structural sealant comprising:
a component A and a component B;
the A component comprises the following components in parts by weight: 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler; wherein, by weight, the compound intermediate comprises: 9.9 to 19.6 parts of cubic mesoporous silica, 98.7 to 99.1 parts of alpha, omega-dihydroxy polydimethylsiloxane and 10.4 to 14.1 parts of phenyl silicone resin; the cubic phase mesoporous silica, the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin are dispersed in a dispersion liquid, and then the dispersion liquid is removed after blending to form the compound intermediate; the component B comprises the following components in parts by weight: 105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst.
In the embodiment of the invention, firstly, the cubic mesoporous silica, the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin are dispersed in the dispersion liquid, the phenyl silicone resin can increase the compatibility of the cubic mesoporous silica and the alpha, omega-dihydroxypolydimethylsiloxane, and the blending of the cubic mesoporous silica, the main resin of the silicone structural sealant, namely the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin is realized in a proper solution environment, so that the three are mixed more uniformly. Secondly, because the pore morphology structure of the cubic mesoporous silica is a regular cubic three-dimensional pore canal structure, the main resin alpha, omega-dihydroxy polydimethylsiloxane molecules of the silicone structure sealant are easier to diffuse, adsorb and penetrate in the dispersing and crosslinking curing process, the molecular size of the phenyl silicone resin is larger than the pore diameter of the pore structure of the mesoporous silica, the phenyl silicone resin basically does not occupy the pore structure of the mesoporous silica, the size of the alpha, omega-dihydroxy polydimethylsiloxane molecules is smaller than or equal to the pore diameter of the pore structure of the cubic mesoporous silica, so that part of alpha, omega-dihydroxy polydimethylsiloxane molecular chains can penetrate through the pore structure of the cubic mesoporous silica to form a meshed structure of the cubic mesoporous silica and alpha, omega-dihydroxy polydimethylsiloxane molecular chain hybridization interpenetrating, entangled and interlocked, the strong interface bonding energy is formed, the free movement of the main resin alpha, omega-dihydroxyl polydimethylsiloxane molecular chain segments of the silicone structural sealant is limited and blocked, and the stress transmission is facilitated, when the silicone structural sealant is acted by external force, the cubic mesoporous silica can induce the microcracks of the surrounding organosilicon polymers such as alpha, omega-dihydroxyl polydimethylsiloxane and can block the expansion of the cracks, meanwhile, the existence of the mesopores can also effectively promote the crack to terminate or further expand, absorb more energy and finally block destructive cracking, so that the creep resistance of the silicone structural sealant is greatly improved, the tensile strength, the elongation and the strength retention rate are also obviously increased, therefore, the mechanical strength of the silicone structural sealant is greatly improved, improving creep resistance. And moreover, as the cubic mesoporous silica has higher specific surface area, the contact area between the molecular chain of the alpha, omega-dihydroxypolydimethylsiloxane of the main resin of the silicone structural sealant and the mesoporous silica is greatly increased, so that the strength of the cured colloid is improved. Finally, the added phenyl silicone resin can introduce a rigid functional group, so that the sliding of a molecular chain of the silicone structural sealant under the condition of external force is limited, and the creep process of the silicone structural sealant can be slowed down by cooperating with the cubic mesoporous silica. In conclusion, the silicone structural sealant disclosed by the invention has the advantages of excellent creep resistance, better mechanical property, excellent strength and elongation, excellent strength retention rate and higher safety coefficient in long-term use and aging processes.
Optionally, the mass ratio of the component A to the component B is: (8.5 to 11.5): 1.
optionally, the specific surface area of the cubic mesoporous silica is 800g/m 2 To 1000g/m 2 The porosity is 95 to 97 percent, and the pore diameter is 2.5 to 5nm.
Optionally, the phenyl silicone comprises: at least one of methyl phenyl silicone resin and vinyl phenyl silicone resin.
Optionally, the base polymer comprises: polydimethyl siloxane with viscosity of 10000mpa.s to 20000 mpa.s;
and/or, the plasticizer comprises: at least one of dimethyl silicone oil with viscosity of 100mpa.s to 350mpa.s and branched silicone oil with viscosity of 100mpa.s to 350 mpa.s;
and/or, the filler comprises: at least one of nano active calcium carbonate, heavy calcium carbonate, precipitated white carbon black and gas phase white carbon black;
and/or the color paste is prepared by stirring and defoaming carbon black and simethicone according to the mass ratio of 1 (2 to 3) in a high-speed dispersing machine to 140 ℃ with the vacuum degree being more than or equal to minus 0.095MPa for 2.5 to 3.5 hours;
and/or the cross-linking agent is at least one of methyltrimethoxysilane, tetraethoxysilane, an oligomer of polymethyl triethoxysilane and propyl trimethoxysilane;
And/or the coupling agent is at least one of gamma-aminopropyl triethoxysilane, 3- (2-aminoethyl) aminopropyl triethoxysilane, gamma-glycidoxypropyl triethoxysilane and beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane;
and/or the catalyst is at least one of dibutyl tin diacetate, dibutyl tin dilaurate and stannous octoate.
Optionally, the particle size of the nano activated calcium carbonate is 40nm to 80nm;
and/or the oil absorption value of the carbon black in the color paste is greater than or equal to 120ml/100g, and the viscosity of the dimethyl silicone oil in the color paste is 12000mpa.s to 13000mpa.s.
In a second aspect of the present invention, a method for preparing a silicone structural sealant as described in any one of the foregoing is provided, including:
preparing a compound intermediate; 9.9 to 19.6 parts of cubic mesoporous silica, 98.7 to 99.1 parts of alpha, omega-dihydroxypolydimethylsiloxane and 10.4 to 14.1 parts of phenyl silicone resin are dispersed in a dispersion liquid by weight, and then the dispersion liquid is removed after blending to form the compound intermediate; preparing a component A; uniformly mixing 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler by weight;
Preparing a component B; uniformly mixing 105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst by weight;
and mixing the component A and the component B in proportion.
Optionally, the step of preparing the compound intermediate includes:
dispersing 10 to 20 parts by weight of cubic phase mesoporous silica in 1000 parts by weight of first dispersion liquid, and carrying out ultrasonic treatment to obtain cubic phase mesoporous silica dispersion liquid;
1000 parts by weight of the cubic mesoporous silica dispersion liquid is added into 1100 parts of mixed dispersion solution, and the mixed solution is obtained by stirring; the mixed dispersion solution includes: alpha, omega-dihydroxy polydimethylsiloxane, phenyl silicone and a second dispersion; in the mixed dispersion solution, the mass ratio of the alpha, omega-dihydroxy polydimethylsiloxane to the phenyl silicone to the second dispersion liquid is (95 to 105): 10 to 15): 950 to 1050;
and adding the mixed solution into an extractant, washing and separating the mixed solution, and performing reduced pressure distillation to obtain the compound intermediate.
Optionally, the step of preparing the cubic mesoporous silica dispersion includes:
adding 10 to 20 parts by weight of cubic mesoporous silica into 1000 parts by weight of first dispersion liquid, stirring in a dispersing machine, and carrying out ultrasonic treatment for 1.5 to 2.5 hours at ultrasonic power of 120 to 150W at the rotating speed of 800 to 1000r/min to obtain cubic mesoporous silica dispersion liquid;
The step of preparing the mixed liquor comprises the following steps:
adding 1000 parts by weight of the cubic mesoporous silica dispersion liquid into 1100 parts by weight of the mixed dispersion solution, stirring in a dispersing machine, wherein the rotating speed of the dispersing machine is 200r/min to 300r/min, and continuously stirring at the rotating speed of 800r/min to 1000r/min for 55min to 65min to obtain the mixed solution;
the mixed solution is added into an extractant to be washed and separated, and the compound intermediate is obtained after reduced pressure distillation, and the method comprises the following steps:
pouring the mixed solution into an extractant, separating the solution after stirring, and distilling under reduced pressure at the temperature of 60-80 ℃ and the vacuum degree of-0.05 Mpa to-0.095 Mpa; the volume ratio of the mixed solution to the extractant is as follows: 1 (2) to 4).
Optionally, the first dispersion liquid includes: at least one of toluene and tetrahydrofuran;
the second dispersion liquid includes: at least one of toluene and tetrahydrofuran;
the extractant comprises: at least one of ethanol and isopropanol.
Optionally, the step of preparing the a component includes:
80 to 100 parts by weight of base polymer, 3 to 5 parts by weight of plasticizer and 80 to 100 parts by weight of the compound intermediate are stirred for 20 to 30 minutes under the vacuum degree of more than or equal to minus 0.095MPa, 180 to 220 parts by weight of filler are added in portions, and the mixture is dispersed and stirred for 55 to 65 minutes under the vacuum degree of more than or equal to minus 0.095 MPa.
Optionally, the step of preparing the B component includes:
105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst by weight are stirred and defoamed for 55 to 65 minutes under the vacuum degree of more than or equal to minus 0.095 MPa.
In a third aspect, the invention provides a silicone structural sealant as defined in any one of the preceding claims, for use in a photovoltaic product.
The silicone structural sealant and the preparation method and application thereof have the same or similar beneficial effects, and are not repeated here.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments of the present invention will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a flowchart of steps of a method for preparing a silicone structural sealant according to an embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are some, but not all embodiments of the invention. 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.
The invention provides a silicone structural sealant which comprises an A component and a B component. The A component comprises the following components in parts by weight: 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler. The component B comprises the following components in parts by weight: 105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst.
The base polymer comprises: the host resin of the silicone structural sealant, i.e., the base polymer, comprises polydimethylsiloxane. The filler in the component A has the reinforcing effect, and can also play the roles of increasing weight and reducing cost. Color paste in the component B has the color mixing function, and in the mixing process of the component A and the component B, whether the components are uniformly mixed can be checked simply and conveniently through the color paste, and on the other hand, the color paste can be used as an adsorption auxiliary agent in the component B, so that the viscosity of the component B can be regulated, and the mixing of the component A and the component B is more uniform. The extractant mainly aims at removing the first dispersion liquid and the second dispersion liquid in the mixed liquid. The reduced pressure distillation mainly aims at removing the extractant in the mixed liquid.
The compound intermediate in the component A comprises the following components in parts by weight: 9.9 to 19.6 parts of cubic mesoporous silica, 98.7 to 99.1 parts of alpha, omega-dihydroxy polydimethylsiloxane and 10.4 to 14.1 parts of phenyl silicone resin. And dispersing cubic mesoporous silica, alpha, omega-dihydroxypolydimethylsiloxane and phenyl silicone resin in a dispersion liquid, and then removing the dispersion liquid after blending to form the compound intermediate. The cubic mesoporous silica, the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin are dispersed in the dispersion liquid, the phenyl silicone resin can increase the compatibility of the cubic mesoporous silica and the alpha, omega-dihydroxypolydimethylsiloxane, and the blending of the cubic mesoporous silica, the main resin of the silicone structural sealant, namely the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin is realized in a proper solution environment, so that the three are mixed more uniformly.
For example, the compounding intermediate may include, by weight: 9.9 parts, or 10.0 parts, or 11.2 parts, or 12.3 parts, or 13.1 parts, or 14.0 parts, or 14.7 parts, or 14.8 parts, or 15.6 parts, or 17.7 parts, or 18.1 parts, or 19.6 parts of cubic mesoporous silica, 98.7 parts, or 98.9 parts, or 98.92 parts, or 98.99 parts, or 99.0 parts, or 99.03 parts, or 99.09 parts, or 99.1 parts of alpha, omega-dihydroxy polydimethylsiloxane, 10.4 parts, or 10.9 parts, or 11.0 parts, or 12.2 parts, or 12.25 parts, or 12.3 parts, or 13.1 parts, or 13.4 parts, or 14.1 parts of phenyl silicone resin. Specifically, according to pore size, porous materials can be classified into: the pore diameter of the inorganic microporous material is generally smaller than 2nm (nanometers), and the inorganic microporous material can comprise tobermorite, active carbon, zeolite molecular sieve and the like, wherein the zeolite molecular sieve is most representative, and the zeolite molecular sieve is characterized by a regular pore channel structure, but the pore diameter is small, so that the adsorption effect of the zeolite molecular sieve on macromolecules is limited. The macroporous material has a pore size of more than 50nm, and can comprise porous ceramics, cement, aerogel and the like, and is characterized in that the pore size is large, but the porous material is non-uniformly combined with main resin polydimethylsiloxane such as silicone structural sealant, and points of stress concentration and stress relaxation are easy to occur. The porous material between micropores and macropores is a mesoporous material, the pore diameter of which ranges from 2nm to 50nm, such as some aerogels, microcrystalline glass and the like, and the mesoporous material has a pore size which is much larger than that of the microporous material.
The mesoporous silica material has the characteristics of uniform pore size, ordered pore shape, continuously adjustable pore diameter range, high specific surface area, good thermal stability and good hydrothermal stability. The mesoporous silicon oxide material can be divided into six types of hexagonal MCM-41 according to different structures, wherein the space group is P6m, cubic MCM-48, the space group is Ia3d, layered unstable MCM-50 and hexagonal SBA-1, the space group is Pm3n, three-dimensional hexagonal SBA-2, the space group is P63/mmc, unordered hexagonal MSU-n and the space group is P6m.
The cubic mesoporous silica has uniform pore size, ordered pore shape, continuously adjustable pore diameter range, high specific surface area, better thermal stability and hydrothermal stability, independent pore diameters, open structure and special cubic three-dimensional double-spiral pore structure, is easy for diffusion, adsorption and penetration of polymer molecular chain segments such as main resin alpha, omega-dihydroxypolydimethylsiloxane of silicone structural sealant, and the pore size or pore diameter of the cubic mesoporous silica can be adjusted between 1.5nm and 50nm. For example, the pore size or pore channel size of the cubic mesoporous silica is 2nm to 50nm. In the first aspect, since the pore morphology structure of the cubic mesoporous silica is a regular cubic three-dimensional pore structure, the main resin alpha, omega-dihydroxy polydimethylsiloxane molecules of the silicone structural sealant are easier to diffuse, adsorb and penetrate in the dispersing and crosslinking curing process, the molecular size of the phenyl silicone resin is larger than the pore diameter of the pore structure of the mesoporous silica, the phenyl silicone resin basically does not occupy the pore structure of the mesoporous silica, the size of the alpha, omega-dihydroxy polydimethylsiloxane molecules is smaller than or equal to the pore diameter of the pore structure of the cubic mesoporous silica, so that part of alpha, omega-dihydroxy polydimethylsiloxane molecular chains can penetrate through the pore structure of the cubic mesoporous silica to form a meshed structure of the cubic mesoporous silica and alpha, omega-dihydroxy polydimethylsiloxane molecular chain hybridization interpenetrating, entangled and interlocked, the strong interface bonding energy is formed, the free movement of the main resin alpha, omega-dihydroxyl polydimethylsiloxane molecular chain segments of the silicone structural sealant is limited and blocked, and the stress transmission is facilitated, when the silicone structural sealant is acted by external force, the cubic mesoporous silica can induce the microcracks of the surrounding organosilicon polymers such as alpha, omega-dihydroxyl polydimethylsiloxane and can block the expansion of the cracks, meanwhile, the existence of the mesopores can also effectively promote the crack to terminate or further expand, absorb more energy and finally block destructive cracking, so that the creep resistance of the silicone structural sealant is greatly improved, the tensile strength, the elongation and the strength retention rate are also obviously increased, therefore, the mechanical strength of the silicone structural sealant is greatly improved, improving creep resistance. In the second aspect, the cubic mesoporous silica has a good reinforcing effect, so that the mechanical property of the silicone structural sealant can be improved, and the contact area between the molecular chain of the main resin alpha, omega-dihydroxy polydimethylsiloxane of the silicone structural sealant and the mesoporous silica is greatly improved due to the higher specific surface area of the cubic mesoporous silica, so that the strength of the cured colloid is improved. In the third aspect, the added phenyl silicone resin can introduce a rigid functional group, so that the sliding of a molecular chain of the silicone structural sealant under the condition of external force is limited, and the creep process of the silicone structural sealant can be slowed down by cooperating with the cubic mesoporous silica. In conclusion, the silicone structural sealant disclosed by the invention has the advantages of excellent creep resistance, better mechanical property, excellent strength and elongation, excellent strength retention rate and higher safety coefficient in long-term use and aging processes.
For example, in silicone structural sealants, the a-component may include, by weight: 80 parts, or 82 parts, or 85 parts, or 89 parts, or 90 parts, or 93 parts, or 100 parts of base polymer, 3 parts, 3.2 parts, or 3.7 parts, or 4 parts, or 4.5 parts, or 4.8 parts, or 5 parts of plasticizer, 80 parts, or 83 parts, or 84 parts, or 86 parts, or 90 parts, or 92.5 parts, or 97 parts, or 100 parts of compounded intermediate, 180 parts, or 185 parts, or 187 parts, or 190 parts, or 194 parts, or 195.3 parts, or 200 parts, or 209 parts, or 220 parts of filler. The B component may include, by weight: 105 parts, 108 parts, 110 parts, 117 parts, 120 parts, 128 parts, 130 parts, 135 parts of cross-linking agent 35 parts, 37 parts, 40 parts, 42 parts, 43 parts, 47 parts, or 50 parts of coupling agent 25 parts, 26 parts, 30 parts, 32 parts, 35 parts, 38 parts, 40 parts, 42.2 parts, 43 parts, 45 parts of catalyst 1 parts, 1.06 parts, 1.2 parts, 1.5 parts, 1.8 parts, 1.9 parts, or 2 parts.
Optionally, the mass ratio of the component A to the component B is as follows: (8.5 to 11.5): the mass ratio of the component A to the component B is proper, and the obtained silicone structural sealant has good mechanical properties. For example, in a silicone structural sealant, the mass ratio of the a component to the B component is: 8.5:1, or 8.8:1, or 8.9:1, or 9.3:1, or 9.5:1, or 9.9:1, or 10:1, or 10.3:1, or 10.8:1, or 11:1, or 11.5:1.
Optionally, stand upFang Xiangjie pore silica has a specific surface area of 800g/m 2 (g/square meter) to 1000g/m 2 The cubic phase mesoporous silica has a proper specific surface area, the porosity is 95-97%, the aperture is 2.5-5 nm, and the contact area of the main resin alpha, omega-dihydroxy polydimethylsiloxane molecular chain of the silicone structural sealant and the mesoporous silica is greatly increased, so that the strength of the gel after solidification is improved. In addition, the aperture and the porosity of the cubic phase mesoporous silica are proper, in the dispersing and crosslinking curing process, the main resin alpha, omega-dihydroxypolydimethylsiloxane molecules of the silicone structure sealant are easier to diffuse, adsorb and penetrate, the molecular size of the phenyl silicone resin is larger than the aperture of the pore structure of the mesoporous silica, the phenyl silicone resin basically does not occupy the pore structure of the mesoporous silica, and the size of the alpha, omega-dihydroxypolydimethylsiloxane molecules is smaller than or equal to the aperture of the pore structure of the cubic phase mesoporous silica, so that more alpha, omega-dihydroxypolydimethylsiloxane molecular chains can penetrate through the pore structure of the mesoporous silica to form a network structure of the cubic phase mesoporous silica and alpha, omega-dihydroxypolydimethylsiloxane molecular chains which are hybridized and interpenetrating, entangled and interlocked, thereby greatly improving the mechanical strength of the silicone structure sealant and improving the creep resistance.
For example, the specific surface area of the cubic mesoporous silica may be 800g/m 2 Or 820g/m 2 Or 840g/m 2 Or 850g/m 2 Or 860g/m 2 Or 900g/m 2 Or 920g/m 2 Or 970g/m 2 Or 980g/m 2 Or 1000g/m 2 The porosity is 95%, or 95.4%, or 95.9%, or 96%, or 96.2%, or 96.4%, or 96.8%, or 97%, the pore size is 2.5nm, or 2.7nm, or 2.9nm, or 3.0nm, or 3.3nm, or 3.7nm, or 4.0nm, or 4.2nm, or 4.7nm, or 5nm.
Alternatively, the aforementioned phenyl silicone may include: at least one of methyl phenyl silicone resin and vinyl phenyl silicone resin. The phenyl silicone resin can further increase the compatibility of the cubic phase mesoporous silica and the alpha, omega-dihydroxyl polydimethylsiloxane, realizes the blending of the cubic phase mesoporous silica, the main resin alpha, omega-dihydroxyl polydimethylsiloxane of the silicone structural sealant and the phenyl silicone resin in a more proper solution environment, and has better mixing effect. The size of the molecules of the phenyl silicone resin is larger than the pore diameter of the pore structure of mesoporous silica, the phenyl silicone resin basically does not occupy the pore structure of the mesoporous silica, and the size of the alpha, omega-dihydroxy polydimethylsiloxane molecules is smaller than or equal to the pore diameter of the pore structure of cubic phase mesoporous silica, so that more alpha, omega-dihydroxy polydimethylsiloxane molecular chains can penetrate through the pore structure of the mesoporous silica to form a network structure of cubic phase mesoporous silica and alpha, omega-dihydroxy polydimethylsiloxane molecular chains for hybridization interpenetrating, entanglement and interlocking, thereby greatly improving the mechanical strength of the silicone structure sealant and improving the creep resistance. And the added phenyl silicone resin can introduce a rigid functional group, so that the sliding of a molecular chain of the silicone structural sealant under the condition of external force is limited, and the creep process of the silicone structural sealant can be slowed down by cooperating with the cubic phase mesoporous silica.
Optionally, the aforementioned base polymer comprises: polydimethylsiloxane with viscosity of 10000mpa.s to 20000mpa.s, and the base polymer with viscosity is excellent in mechanical properties and easy to obtain after being matched with the compound intermediate.
For example, the base polymer may be polydimethylsiloxane having a viscosity of 10000mpa.s, or a viscosity of 11000mpa.s, or a viscosity of 12000mpa.s, or a viscosity of 14600mpa.s, or a viscosity of 15000mpa.s, or a viscosity of 16000mpa.s, or a viscosity of 18000mpa.s, or a viscosity of 20000 mpa.s.
Optionally, the aforementioned plasticizer comprises: at least one of dimethyl silicone oil with the viscosity of 100-350 mpa.s and branched silicone oil with the viscosity of 100-350 mpa.s, and the plasticizer with the viscosity is matched with other components, so that the plasticizer has excellent mechanical properties and is easy to obtain.
For example, the plasticizer is a polydimethyl silicone oil having a viscosity of 100mpa.s, 110mpa.s, 180mpa.s, 200mpa.s, 220mpa.s, 225mpa.s, 260mpa.s, 300mpa.s, or 350 mpa.s. Alternatively, the plasticizer may be a branched silicone oil having a viscosity of 100mpa.s, 110mpa.s, 180mpa.s, 200mpa.s, 220mpa.s, 225mpa.s, 260mpa.s, 300mpa.s, or 350 mpa.s.
Alternatively, the foregoing filler may include: at least one of nano active calcium carbonate, heavy calcium carbonate, precipitated white carbon black and gas phase white carbon black, the filler has excellent reinforcing effect, good weight increasing effect, low cost and easy obtainment. Optionally, the particle size of the nano active calcium carbonate is 40nm to 80nm, and the nano active calcium carbonate has proper particle size, better reinforcing and weight increasing effects, lower cost and easy acquisition.
For example, the particle size of the nano-active calcium carbonate is 40nm, or 50nm, or 58nm, or 60nm, or 62nm, or 70nm, or 77nm, or 80nm.
Optionally, the color paste can be prepared by stirring and defoaming carbon black and dimethyl silicone oil according to the mass ratio of 1 (2 to 3) in a high-speed dispersing machine to 140 ℃ with the vacuum degree of more than or equal to-0.095 MPa (megapascal) for 2.5 to 3.5 hours. The color paste has good color mixing effect, and the color paste used as an adsorption auxiliary agent in the component B has good adjusting effect on the viscosity of the component B and is easy to obtain. Optionally, the oil absorption value of the carbon black in the color paste is greater than or equal to 120ml/100g, the viscosity of the dimethyl silicone oil in the color paste is 12000mpa.s to 13000mpa.s, and the color mixing effect and the adjusting effect on the viscosity are better after the two are matched with each other.
For example, the color paste can be prepared by heating carbon black and simethicone according to a mass ratio of 1:2, or 1:2.2, or 1:2.4, or 1:2.5, or 1:2.7, or 1:2.9, or 1:3 in a high-speed dispersing machine to 140 ℃, wherein the vacuum degree is-0.095 MPa, or-0.093 MPa, or-0.090 MPa, or-0.087 MPa, or-0.082 MPa, -0.080MPa, and the stirring is carried out for 2.5 hours, or 2.6 hours, or 2.8 hours, or 2.9 hours, or 3 hours, or 3.1 hours, or 3.3 hours, or 3.5 hours. For example, the oil absorption value of the carbon black in the color paste can be 120ml/100g, 130ml/100g, 140ml/100g, 150ml/100g, 170ml/100g, or 180ml/100g, and the viscosity of the simethicone is 12000mpa.s, 12100mpa.s, 12400mpa.s, 12500mpa.s, 12600mpa.s, 12700mpa.s, 13000mpa.s.
Optionally, the cross-linking agent is at least one of methyltrimethoxysilane, tetraethoxysilane, an oligomer of polymethyl triethoxysilane and propyl trimethoxysilane, and has good cross-linking effect and is easy to obtain.
Optionally, the coupling agent is at least one of gamma-aminopropyl triethoxysilane, 3- (2-aminoethyl) aminopropyl triethoxysilane, gamma-glycidol ether oxypropyl triethoxysilane and beta- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane, and the coupling effect of the coupling agent is good and the coupling agent is easy to obtain.
Optionally, the catalyst is at least one of dibutyl tin diacetate, dibutyl tin dilaurate and stannous octoate. The catalyst has good catalytic effect and is easy to obtain.
The invention also provides a preparation method of any one of the silicone structural sealants. Fig. 1 shows a flowchart of steps of a method for preparing a silicone structural sealant according to an embodiment of the present invention. Referring to fig. 1, the method includes the following steps.
In the dispersing in step 101, cubic mesoporous silica, alpha, omega-dihydroxypolydimethylsiloxane and phenyl silicone resin can be respectively dispersed into corresponding dispersion liquid, and then the three liquids dispersed in the dispersion liquid are mixed. Alternatively, in step 101, cubic mesoporous silica may be dispersed alone, and α, ω -dihydroxypolydimethylsiloxane and phenyl silicone may be dispersed together and then mixed. In the embodiment of the present invention, this is not particularly limited.
102, preparing a component A; 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler are uniformly mixed by weight.
It should be noted that the order of steps 102 and 103 may be changed.
Optionally, the foregoing step 101 may include: substep 1011 to substep 1013.
Sub-step 1011, dispersing 10 to 20 parts by weight of cubic phase mesoporous silica in 1000 parts of the first dispersion, and obtaining the cubic phase mesoporous silica dispersion after ultrasonic treatment. The ultrasonic dispersion has larger energy, and the cubic mesoporous silica can be uniformly dispersed in the first dispersion liquid.
For example, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 14.9 parts, 15 parts, 15.2 parts, 16 parts, 17 parts, 18 parts, or 20 parts of cubic mesoporous silica is dispersed in 1000 parts of the first dispersion by weight, and the cubic mesoporous silica dispersion is obtained after ultrasonic treatment.
Optionally, this substep 1011 may include: 10 to 20 parts by weight of cubic mesoporous silica is added to 1000 parts of the first dispersion liquid, stirred in a dispersing machine, and the rotating speed of the dispersing machine is 800r/min to 1000r/min, and the cubic mesoporous silica dispersion liquid is obtained after ultrasonic power is 120W to 150W and ultrasonic power is carried out for 1.5 to 2.5 hours.
The stirring and dispersing process can be performed in a high-speed dispersing machine. Sub-step 1011 serves primarily to disperse the cubic phase mesoporous silica well in a liquid environment.
For example, 10 parts, or 12 parts, or 14 parts, or 15 parts, or 15.2 parts, or 17 parts, or 19 parts, or 20 parts of the cubic phase mesoporous silica is dispersed in 1000 parts of the first dispersion by stirring at a rotation speed of 800r/min (revolutions/min), or 800r/min, or 840r/min, or 890r/min, or 900r/min, or 920r/min, or 950r/min, or 1000r/min, and the cubic phase mesoporous silica dispersion is obtained after ultrasonic power of 120W (watts), or 128W, or 130W, or 135W, or 136W, or 140W, or 147W, 150W for 1.5 hours, or 1.6 hours, or 1.8 hours, or 1.9 hours, or 2.0 hours, or 2.1 hours, or 2.2 hours, or 2.3 hours, or 2.5 hours.
Sub-step 1012, adding 1000 parts by weight of the cubic mesoporous silica dispersion liquid into 1100 parts of mixed dispersion solution, and stirring to obtain mixed solution; the mixed dispersion solution includes: alpha, omega-dihydroxy polydimethylsiloxane, phenyl silicone and a second dispersion; in the mixed dispersion solution, the mass ratio of the alpha, omega-dihydroxypolydimethylsiloxane, the phenyl silicone resin and the second dispersion liquid is (95 to 105): 10 to 15): 950 to 1050. The dispersion of the alpha, omega-dihydroxy polydimethylsiloxane and the phenyl silicone resin can be carried out by mechanical stirring and dispersion without ultrasound, so that the molecular chains of the alpha, omega-dihydroxy polydimethylsiloxane and the phenyl silicone resin can not be lost due to strong energy of ultrasound, and the integrity of the molecular chains of the alpha, omega-dihydroxy polydimethylsiloxane and the phenyl silicone resin can be maintained to a large extent by mechanical stirring and dispersion. In addition, the alpha, omega-dihydroxy polydimethylsiloxane and the phenyl silicone resin can obtain good dispersing effect under the condition of mechanical stirring and dispersing, and the process can be reduced compared with the process of dispersing the alpha, omega-dihydroxy polydimethylsiloxane and the phenyl silicone resin respectively, so that the production efficiency is improved.
For example, the mass ratio of the alpha, omega-dihydroxy polydimethylsiloxane, the phenyl silicone, and the second dispersion in the mixed dispersion solution is 95:10:950, or 95:12:950, or 100:10:1000, or 100:11:1000, or 100:12:1000, or 100:13:990, or 99:14:1000, or 100:15:1000, or 95:10:980, or 95:12:990, or 97:12:999, or 100:10:1010, or 100:15:1050.
Optionally, sub-step 1012 may include: adding 1000 parts by weight of the cubic mesoporous silica dispersion liquid into 1100 parts by weight of the mixed dispersion solution, stirring in a dispersing machine, wherein the rotating speed of the dispersing machine is 200r/min to 300r/min, and continuously stirring at the rotating speed of 800r/min to 1000r/min for 55min to 65min to obtain the mixed solution.
The effect of sub-step 1012 is mainly to promote the compatibility of the alpha, omega-dihydroxyl polydimethylsiloxane and the cubic phase mesoporous silica, and the molecular size of the phenyl silicone resin is larger than the pore diameter of the pore structure of the mesoporous silica, the phenyl silicone resin basically does not occupy the pore structure of the mesoporous silica, and the size of the alpha, omega-dihydroxyl polydimethylsiloxane molecular is smaller than or equal to the pore diameter of the pore structure of the cubic phase mesoporous silica, so that part of alpha, omega-dihydroxyl polydimethylsiloxane molecular chains can penetrate through the pore structure of the mesoporous silica to form a network structure of hybridization interpenetrating, entanglement and interlocking of the cubic phase mesoporous silica and the alpha, omega-dihydroxyl polydimethylsiloxane molecular chains, thereby greatly improving the mechanical strength of the silicone structure sealant and improving the creep resistance. And the added phenyl silicone resin can introduce a rigid functional group, so that the sliding of a molecular chain of the silicone structural sealant under the condition of external force is limited, and the creep process of the silicone structural sealant can be slowed down by cooperating with the cubic phase mesoporous silica.
And step 1013, adding the mixed solution into an extractant, washing and separating the mixed solution, and performing reduced pressure distillation to obtain the compound intermediate. The purpose of the separation is mainly to remove the first dispersion and the second dispersion in the mixed solution. The reduced pressure distillation mainly aims at removing the extractant in the mixed liquor.
Optionally, this substep 1013 may include: pouring the mixed solution into an extractant, separating the solution after stirring, and distilling under reduced pressure at the temperature of 60-80 ℃ and the vacuum degree of-0.05 Mpa to-0.095 Mpa; the volume ratio of the mixed solution to the extractant is as follows: 1 (2) to 4).
For example, the mixture is poured into an extractant, stirred and separated, and distilled under reduced pressure at a temperature of 60℃or 62℃or 65℃or 68℃or 70℃or 71.2℃or 77℃or 80℃under vacuum of-0.05 MPa or-0.057 MPa or-0.06 MPa or-0.07 MPa or-0.0725 MPa or-0.08 MPa or-0.087 MPa or-0.09 MPa or-0.095 MPa. The volume ratio of the mixed solution to the extractant is as follows: 1:2, or 1:2.3, or 1:2.9, or 1:3, or 1:3.1, or 1:3.6, or 1:3.7, or 1:3.9, or 1:4.
Alternatively, the aforementioned first dispersion may include: at least one of toluene and tetrahydrofuran, the first dispersion liquid can sufficiently disperse the cubic mesoporous silica, and the dispersing effect of the cubic mesoporous silica on Fang Xiangjie pore silica is good.
Alternatively, the aforementioned second dispersion may include: at least one of toluene and tetrahydrofuran, the second dispersion liquid can fully disperse the cubic phase mesoporous silica, the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin, and has good dispersing and mixing effects on the cubic phase mesoporous silica, the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin.
Alternatively, the aforementioned extractant may include: at least one of ethanol and isopropanol, the extractant is more thorough in removal of the first dispersion liquid and the second dispersion liquid, and is easy to obtain.
Optionally, the foregoing step 102 may include: 80 to 100 parts by weight of base polymer, 3 to 5 parts by weight of plasticizer and 80 to 100 parts by weight of the compound intermediate are stirred for 20 to 30 minutes under the vacuum degree of more than or equal to minus 0.095MPa, 180 to 220 parts by weight of filler are added in portions, and the mixture is dispersed and stirred for 55 to 65 minutes under the vacuum degree of more than or equal to minus 0.095 MPa.
For example, the foregoing step 102 may be: 80 parts, or 82 parts, or 85 parts, or 89 parts, or 90 parts, or 92 parts, or 97 parts, or 100 parts of the base polymer, 3 parts, or 3.2 parts, or 3.4 parts, or 3.7 parts, or 4.0 parts, or 4.2 parts, or 4.6 parts, or 4.7 parts, or 4.9 parts, or 5 parts of plasticizer, 80 parts, or 82 parts, or 85 parts, or 87 parts, or 89 parts, or 90 parts, or 90.1 parts, or 94 parts, or 97 parts, or 100 parts of the foregoing compounded intermediate, and the filler is dispersed at a vacuum level of-0.095 MPa, or-0.092 MPa, or-0.091 MPa, or-0.090 MPa, or-0.089 MPa, or-0.085 MPa, or-0.080 MPa for 20min, or 22min, or 24min, or 25min, or 25.2min, or 26min, 28, 29min, or 180 to 55min, or more, and the filler is stirred at a vacuum level of-0.092 MPa, or-0.091 MPa, or-0.090 MPa, or-0.089 min.
Optionally, the foregoing step 103 may include: 105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst are stirred and defoamed for 55 to 65 minutes under the vacuum degree of more than or equal to-0.095 MPa, and the step of forming the component B is simple and easy to implement.
The invention also provides application of any one of the silicone structural sealant in a photovoltaic product. For example, the silicone structural sealant of any of the foregoing embodiments of the present invention is applied to back hook bonding of a dual-glass assembly for structural bonding and sealing. For another example, the silicone structural sealant of any of the present invention is applied to BIPV (Building Integrated Photovoltaic, photovoltaic building integration) for structural bonding and sealing. The silicone structural sealant of any of the foregoing embodiments of the present invention was applied to BAPV (Building Attached Photovoltaic) for structural bonding and sealing. BAPV is defined differently from BIPV and mainly refers to solar photovoltaic power generation systems installed on existing buildings.
The application of any of the silicone structural sealants to photovoltaic products is not limited to the above examples, and any silicone structural sealant is within the scope of protection thereof.
According to the invention, the silicone structural sealant can bear larger dynamic load and static load, such as gravity, wind load, snow load and the like, and has the advantages of excellent heat resistance, ultraviolet resistance, damp heat resistance, acid and alkali resistance, creep resistance, lasting high strength retention rate and the like due to complex and changeable application environments in the photovoltaic product, and can improve the safety performance and the service life of the photovoltaic device.
In the invention, the silicone structural sealant, the preparation method of the silicone structural sealant, the application of the silicone structural sealant in the photovoltaic product, and the related parts of the silicone structural sealant, the silicone structural sealant and the photovoltaic product can be referred to each other for avoiding repetition, and the same or similar beneficial effects can be achieved.
The present application is further illustrated below in conjunction with specific examples.
Examples
(1) Preparing a compound intermediate. The high-speed dispersing machine is stirred at a high speed under the rotating speed of 800r/min to 1000r/min, and the specific surface area of 10g is 900g/m 2 Dispersing cubic phase MCM-48 mesoporous silica with the aperture of 5nm in 1000g of toluene, carrying out ultrasonic treatment for 2 hours at the ultrasonic power of 120W to 150W to obtain cubic phase mesoporous silica dispersion liquid, adding 1000g of the dispersion liquid into 1100g of mixed dispersion solution under the stirring condition with the rotating speed of 200r/min to 300r/min, and adding the mixture into 1100g of mixed dispersion solution, wherein the mass ratio of alpha, omega-dihydroxy polydimethylsiloxane to methyl phenyl silicone resin to toluene is 100:10:1000. The viscosity of the alpha, omega-dihydroxy polydimethylsiloxane was 12000mpa.s. Continuously stirring at a high speed for 60min at a rotating speed of 800r/min to 1000r/min to obtain a mixed solution. Pouring the mixed solution into absolute ethyl alcohol according to the volume ratio of 1:2, stirring, separating the solution, repeatedly washing the separated solution with absolute ethyl alcohol for three times, obtaining a dispersion of mesoporous silicon dioxide, alpha, omega-dihydroxypolydimethylsiloxane and methylbenzyl silicone resin containing a small amount of absolute ethyl alcohol, and carrying out reduced pressure distillation on the dispersion at the temperature of 70 ℃ and the vacuum degree of-0.09 Mpa, and separating to obtain a compound intermediate.
(2) Preparing the component A. Weighing 100 parts by mass of polydimethylsiloxane with viscosity of 10000mpa.s, 3 parts by mass of simethicone with viscosity of 350mpa.s and 100 parts by mass of compound intermediate, stirring in a planetary stirrer for 25min under vacuum degree of more than or equal to-0.095 MPa, adding 180 parts by mass of nano calcium carbonate three times, and dispersing and stirring for 60min under vacuum degree of more than or equal to-0.095 MPa to obtain the component A.
(3) Preparing a component B. 105 parts by mass of color paste, 20 parts by mass of methyltrimethoxysilane, 24 parts by mass of propyltrimethoxysilane, 25 parts by mass of gamma-aminopropyltriethoxysilane, 15 parts by mass of gamma-glycidol ether oxypropyl triethoxysilane and 1.2 parts by mass of dibutyltin dilaurate are weighed, stirred and defoamed for 60 minutes under the vacuum degree of more than or equal to-0.095 MPa, and the component B is prepared.
(4) Mixing the prepared A component and B component according to the mass ratio of 10:1, and preparing samples.
Comparative example 1
In the process of preparing the compound intermediate in comparative example 1, fumed silica was used instead of cubic MCM-48 mesoporous silica in examples, and the remainder was the same as in examples.
Comparative example 2
In the process of preparing the compound intermediate in comparative example 2, hexagonal phase mesoporous silica was used instead of cubic phase MCM-48 mesoporous silica in examples, and the rest were the same as in examples.
Comparative example 3
In the process of preparing the compound intermediate in comparative example 3, the methylphenyl silicone resin in the example was replaced with a silane coupling agent, and the rest was the same as the corresponding example.
Comparative example 4
In the preparation of the compounded intermediate in comparative example 4, a high-speed disperser was used to prepare a compound intermediate having a specific surface area of 900g/m, 10g 2 The preparation method comprises the steps of stirring cubic MCM-48 mesoporous silica with the aperture of 5nm, 99.1g of alpha, omega-dihydroxypolydimethylsiloxane with the viscosity of 12000mpa.s and 9.91g of methylphenyl silicone resin at a high speed at a rotating speed of 800r/min to 1000r/min to obtain a compound intermediate, wherein the rest components are the same as those in the embodiment.
Comparative example 5
Comparative example 5 differs from example only in that no methylphenyl silicone resin was added during the preparation of the compounded intermediate, and the remainder was the same as in example.
The tensile strength, elongation and strength retention under the corresponding conditions were all examined for examples and comparative examples 1 to 5 using the method of T/CPIA0008-2019 Silicone structural adhesive for photovoltaic modules. Creep displacement was measured for examples and comparative examples 1 to 5 by the method described in appendix C of JG/T475-2015, silicone structural sealant for building curtain wall. The results of the measurements are shown in the following table.
Comparative examples and comparative examples 1 to 5 test results comparison table
DH1500 refers to placing the test piece in a humid heat aging chamber according to the specification of 10.13 in GB/T9535-1998, and a constant humid heat test chamber at 85 DEG C.+ -. 2 ℃ and a relative humidity of 85% RH.+ -. 5% RH for 1500 hours.
HF20 means that the sample is put into a high-low temperature test box according to the specification of 10.12 in GB/T9535-1998, 20 cycles are completed between-40+/-2 ℃ and 85+/-2 ℃, and the relative humidity is kept within 85%RH+/-5%RH of a set value. The rate of temperature change above 0 ℃ should not exceed 100 ℃/h, the rate of temperature change below 0 ℃ should not exceed 200 ℃/h, and should remain stable for a minimum of 20 hours at the highest temperature and for a minimum of 4 hours at the lowest temperature, and for a minimum of 0.5 hours in one cycle.
From the table, the embodiment adopts cube phase MCM-48 mesoporous silica and methyl phenyl silicone resin to cooperatively reinforce, the strength retention rate of the silicone structural sealant DH1500 and the strength retention rate of the silicone structural sealant HF20 after aging are both more than 75%, the creep displacement is 0.54mm, and the mechanical property is good. The reinforcing effect of the gas phase method silicon dioxide adopted in the comparative example 1 and the reinforcing effect of the hexagonal phase mesoporous silicon dioxide adopted in the comparative example 2 are inferior to those of the examples, mainly because the gas phase method silicon dioxide and the hexagonal phase mesoporous silicon dioxide have corresponding microstructures although the specific surface areas are large, but are inferior to the cubic three-dimensional silicon double-helix pore canal structure of the cubic phase mesoporous silicon dioxide, and the diffusion, the adsorption and the penetration of the alpha, omega-dihydroxypolydimethylsiloxane molecular chains are easy. In comparative example 3, the cubic mesoporous silica is subjected to surface treatment with a silane coupling agent and then reinforced, and the cubic mesoporous silica is subjected to surface treatment with the silane coupling agent, so that the dispersion of the cubic mesoporous silica can be improved, but the size of the silane coupling agent molecules is smaller than that of the pore channels of the cubic mesoporous silica, so that the silane coupling agent molecules occupy the pore channels of the cubic mesoporous silica, and the diffusion, adsorption and penetration of the cubic mesoporous silica to the alpha, omega-dihydroxy polydimethylsiloxane molecules are not facilitated, and the mechanical strength and creep resistance are not as good as those of the examples. In the process of forming the compound intermediate, the comparative example 4 only adopts a mechanical stirring mode to directly add mesoporous silica, does not add any dispersion liquid and the like, has the problems of agglomeration and nonuniform dispersion of cubic mesoporous silica, and is also unfavorable for adsorption of the cubic mesoporous pore canal on alpha, omega-dihydroxypolydimethylsiloxane molecules, so that the mechanical strength, creep resistance and strength retention rate after aging are poor. In the process of forming the compound intermediate, the comparative example 5 is not added with methyl phenyl silicone resin, so that the reinforcing effect of the methyl phenyl silicone resin is not required, and the compatibility of cubic mesoporous silica and alpha, omega-dihydroxypolydimethylsiloxane is poor, and the mixing effect is poor, so that the mechanical strength, the creep resistance and the strength retention after aging are poor.
It should be noted that, for simplicity of description, the method embodiments are shown as a series of acts, but it should be understood by those skilled in the art that the embodiments are not limited by the order of acts described, as some steps may occur in other orders or concurrently in accordance with the embodiments. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred, and that the acts referred to are not necessarily all required for the embodiments of the present application.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method article or apparatus that comprises the element.
From the above description of the embodiments, it will be clear to those skilled in the art that the above-described embodiment method may be implemented by means of software plus a necessary general hardware platform, but of course may also be implemented by means of hardware, but in many cases the former is a preferred embodiment. Based on such understanding, the technical solution of the present invention may be embodied essentially or in a part contributing to the prior art in the form of a software product stored in a storage medium (e.g. ROM/RAM, magnetic disk, optical disk) comprising instructions for causing a terminal (which may be a mobile phone, a computer, a server, an air conditioner, or a network device, etc.) to perform the method according to the embodiments of the present invention.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many forms may be made by those having ordinary skill in the art without departing from the spirit of the present invention and the scope of the claims, which are to be protected by the present invention.
Claims (13)
1. A silicone structural sealant, comprising:
a component A and a component B;
the A component comprises the following components in parts by weight: 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler; wherein, by weight, the compound intermediate comprises: 9.9 to 19.6 parts of cubic mesoporous silica, 98.7 to 99.1 parts of alpha, omega-dihydroxy polydimethylsiloxane and 10.4 to 14.1 parts of phenyl silicone resin; the cubic phase mesoporous silica, the alpha, omega-dihydroxypolydimethylsiloxane and the phenyl silicone resin are dispersed in a dispersion liquid, and then the dispersion liquid is removed after blending to form the compound intermediate;
the component B comprises the following components in parts by weight: 105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst.
2. The silicone structural sealant according to claim 1, wherein the mass ratio of the a component and the B component is: (8.5 to 11.5): 1.
3. the silicone structural sealant according to claim 1, wherein the cubic mesoporous silica has a specific surface area of 800g/m 2 To 1000g/m 2 The porosity is 95 to 97 percent, and the pore diameter is 2.5 to 5nm.
4. The silicone structural sealant according to claim 1, wherein the phenyl silicone resin comprises: at least one of methyl phenyl silicone resin and vinyl phenyl silicone resin.
5. The silicone structural sealant according to any one of claims 1 to 4, wherein the base polymer comprises: polydimethyl siloxane with viscosity of 10000mpa.s to 20000 mpa.s;
and/or, the plasticizer comprises: at least one of dimethyl silicone oil with viscosity of 100mpa.s to 350mpa.s and branched silicone oil with viscosity of 100mpa.s to 350 mpa.s;
and/or, the filler comprises: at least one of nano active calcium carbonate, heavy calcium carbonate, precipitated white carbon black and gas phase white carbon black;
and/or the color paste is prepared by stirring and defoaming carbon black and simethicone according to the mass ratio of 1 (2 to 3) in a high-speed dispersing machine to 140 ℃ with the vacuum degree being more than or equal to minus 0.095MPa for 2.5 to 3.5 hours;
and/or the cross-linking agent is at least one of methyltrimethoxysilane, tetraethoxysilane, an oligomer of polymethyl triethoxysilane and propyl trimethoxysilane;
And/or the coupling agent is at least one of gamma-aminopropyl triethoxysilane, 3- (2-aminoethyl) aminopropyl triethoxysilane, gamma-glycidoxypropyl triethoxysilane and beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane;
and/or the catalyst is at least one of dibutyl tin diacetate, dibutyl tin dilaurate and stannous octoate.
6. The silicone structural sealant according to claim 5, wherein the nano-activated calcium carbonate has a particle size of 40nm to 80nm;
and/or the oil absorption value of the carbon black in the color paste is greater than or equal to 120ml/100g, and the viscosity of the dimethyl silicone oil in the color paste is 12000mpa.s to 13000mpa.s.
7. A method of producing the silicone structural sealant according to any one of claims 1 to 6, comprising:
preparing a compound intermediate; 9.9 to 19.6 parts of cubic mesoporous silica, 98.7 to 99.1 parts of alpha, omega-dihydroxypolydimethylsiloxane and 10.4 to 14.1 parts of phenyl silicone resin are dispersed in a dispersion liquid by weight, and then the dispersion liquid is removed after blending to form the compound intermediate;
preparing a component A; uniformly mixing 80 to 100 parts of base polymer, 3 to 5 parts of plasticizer, 80 to 100 parts of compound intermediate and 180 to 220 parts of filler by weight;
Preparing a component B; uniformly mixing 105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst by weight;
and mixing the component A and the component B in proportion.
8. The method of preparing a silicone structural sealant according to claim 7, wherein the step of preparing a compounded intermediate comprises:
dispersing 10 to 20 parts by weight of cubic phase mesoporous silica in 1000 parts by weight of first dispersion liquid, and carrying out ultrasonic treatment to obtain cubic phase mesoporous silica dispersion liquid;
1000 parts by weight of the cubic mesoporous silica dispersion liquid is added into 1100 parts of mixed dispersion solution, and the mixed solution is obtained by stirring; the mixed dispersion solution includes: alpha, omega-dihydroxy polydimethylsiloxane, phenyl silicone and a second dispersion; in the mixed dispersion solution, the mass ratio of the alpha, omega-dihydroxy polydimethylsiloxane to the phenyl silicone to the second dispersion liquid is (95 to 105): 10 to 15): 950 to 1050;
and adding the mixed solution into an extractant, washing and separating the mixed solution, and performing reduced pressure distillation to obtain the compound intermediate.
9. The method of preparing a silicone structured sealant according to claim 8, wherein the step of preparing the cubic mesoporous silica dispersion comprises:
Adding 10 to 20 parts by weight of cubic phase mesoporous silica into 1000 parts by weight of first dispersion liquid, stirring in a dispersing machine, and carrying out ultrasonic treatment for 1.5 to 2.5 hours at ultrasonic power of 120 to 150W at the rotating speed of 800 to 1000r/min to obtain cubic phase mesoporous silica dispersion liquid;
the step of preparing the mixed liquor comprises the following steps:
adding 1000 parts by weight of the cubic mesoporous silica dispersion liquid into 1100 parts by weight of the mixed dispersion solution, stirring in a dispersing machine, wherein the rotating speed of the dispersing machine is 200r/min to 300r/min, and continuously stirring at the rotating speed of 800r/min to 1000r/min for 55min to 65min to obtain the mixed solution;
the mixed solution is added into an extractant to be washed and separated, and the compound intermediate is obtained after reduced pressure distillation, and the method comprises the following steps:
pouring the mixed solution into an extractant, separating the solution after stirring, and distilling under reduced pressure at the temperature of 60-80 ℃ and the vacuum degree of-0.05 Mpa to-0.095 Mpa; the volume ratio of the mixed solution to the extractant is as follows: 1 (2) to 4).
10. The method of preparing a silicone structural sealant according to claim 8 or 9, wherein the first dispersion liquid comprises: at least one of toluene and tetrahydrofuran;
The second dispersion liquid includes: at least one of toluene and tetrahydrofuran;
the extractant comprises: at least one of ethanol and isopropanol.
11. The method for producing a silicone structural sealant according to any one of claims 7 to 9, wherein the step of producing the a component comprises:
80 to 100 parts by weight of base polymer, 3 to 5 parts by weight of plasticizer and 80 to 100 parts by weight of the compound intermediate are stirred for 20 to 30 minutes under the vacuum degree of more than or equal to minus 0.095MPa, 180 to 220 parts by weight of filler are added in portions, and the mixture is dispersed and stirred for 55 to 65 minutes under the vacuum degree of more than or equal to minus 0.095 MPa.
12. The method for producing a silicone structural sealant according to any one of claims 7 to 9, wherein the step of producing a B component comprises:
105 to 135 parts of color paste, 35 to 50 parts of cross-linking agent, 25 to 45 parts of coupling agent and 1 to 2 parts of catalyst by weight are stirred and defoamed for 55 to 65 minutes under the vacuum degree of more than or equal to minus 0.095 MPa.
13. Use of the silicone structured sealant according to any of claims 1 to 6 in a photovoltaic product.
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