CN116144314B - Sealant for single-component rapid deep curing photovoltaic module and preparation method thereof - Google Patents
Sealant for single-component rapid deep curing photovoltaic module and preparation method thereof Download PDFInfo
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- CN116144314B CN116144314B CN202211549025.8A CN202211549025A CN116144314B CN 116144314 B CN116144314 B CN 116144314B CN 202211549025 A CN202211549025 A CN 202211549025A CN 116144314 B CN116144314 B CN 116144314B
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- 239000000565 sealant Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003094 microcapsule Substances 0.000 claims abstract description 31
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000077 silane Inorganic materials 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012188 paraffin wax Substances 0.000 claims abstract description 20
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 19
- 239000011257 shell material Substances 0.000 claims abstract description 19
- 229940099259 vaseline Drugs 0.000 claims abstract description 18
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011162 core material Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 39
- 238000002156 mixing Methods 0.000 claims description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000002736 nonionic surfactant Substances 0.000 claims description 11
- 229920002554 vinyl polymer Polymers 0.000 claims description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- 230000001737 promoting effect Effects 0.000 claims description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 8
- 230000001804 emulsifying effect Effects 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 150000002923 oximes Chemical class 0.000 claims 3
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 229920002545 silicone oil Polymers 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000000741 silica gel Substances 0.000 abstract 1
- 229910002027 silica gel Inorganic materials 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 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 description 7
- 230000008569 process Effects 0.000 description 7
- 229940083037 simethicone Drugs 0.000 description 7
- 230000032683 aging Effects 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 239000004590 silicone sealant Substances 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000007963 capsule composition Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000004513 sizing Methods 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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 sealant for a single-component rapid deep curing photovoltaic module and a preparation method thereof, wherein the sealant comprises the following raw materials in parts by weight: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane; 70-100 parts of reinforcing filler; 10-20 parts of ketoximino silane cross-linking agent; 0-10 parts of plasticizer; 1-5 parts of curing accelerating microcapsules; 0.5-1.5 parts of silane coupling agent and 0.06-0.1 part of catalyst; wherein the curing accelerating microcapsule is prepared by taking deionized water as a core material and taking a mixture of paraffin and vaseline as a shell material, and the particle size of the microcapsule is 0.5-50 mu m. The single-component rapid deep curing ketoxime-removing room temperature vulcanized silica gel has the characteristic of rapid deep curing, simultaneously keeps good adhesion performance on glass, metal and other base materials, is very suitable for the production of photovoltaic modules, and is very suitable for rapid flowing water beats of piece production.
Description
Technical Field
The invention belongs to the technical field of silicon rubber, and particularly relates to a sealant for a single-component rapid deep curing photovoltaic module and a preparation method thereof.
Background
The room temperature vulcanized silicone sealant can be crosslinked and cured at room temperature to generate an elastomer, and has excellent performances of high and low temperature resistance, weather aging resistance, ozone resistance and the like, so that the room temperature vulcanized silicone sealant becomes a first-choice glue for producing photovoltaic modules. At present, a single-component type room temperature vulcanized silicone sealant for photovoltaic module production is mainly adopted. In order to maintain storage stability, a cross-linking agent, a coupling agent and a catalyst are added after deep dehydration during the production of the single component, so that the single component type curing mechanism is that the sealant is cured by utilizing water vapor in air, the curing process is from the surface to the inside, natural deep curing is slow, and the requirement of faster running water beats of component production enterprises cannot be met.
At present, in order to accelerate the deep curing speed and efficiency of silicone sealant for photovoltaic modules, a solution is generally provided, wherein the solution is a two-component solution, such as CN101717582A, CN101768421A, CN102167965A, CN102181264A and the like, the base material and the curing components are respectively packaged, the base material and the curing components are fully and uniformly mixed when in use, and the curing process is performed by using a small amount of moisture in the base material, and the curing process is performed simultaneously inside and outside. These two-component curing schemes tend to require the component manufacturers to replace large batches of dispensing equipment with less economical results.
Disclosure of Invention
The invention provides a sealant for a single-component rapid deep-curing photovoltaic module and a preparation method thereof, wherein the sealant is prepared by introducing deep-curing accelerating microcapsules which take deionized water as a core material and paraffin and Vaseline composition shell materials, so that the single-component sealant has the same high-efficiency curing performance as double components, the curing temperature is low, the curing time is controllable, and the cured sealant has excellent ageing resistance and no degradation.
The sealant for the single-component rapid deep curing photovoltaic module comprises the following raw materials in parts by weight:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane; 70-100 parts of reinforcing filler; 10-20 parts of ketoximino silane cross-linking agent; 0-10 parts of plasticizer; 1-5 parts of curing accelerating microcapsules; 0.5-1.5 parts of silane coupling agent and 0.06-0.1 part of catalyst;
further, the curing accelerating microcapsule is prepared by taking deionized water as a core material and taking a mixture of paraffin and vaseline as a shell material, and the particle size of the microcapsule is 0.5-50 mu m.
Further, the alpha, omega-dihydroxy polydimethylsiloxane has a viscosity of 200 to 80000mpa.s or a mixture of viscosities.
Further, the reinforcing filler is at least one or two mixtures of precipitated white carbon black, gas phase white carbon black and nano calcium carbonate.
Further, the ketoxime silane cross-linking agent is one or a mixture of more of tetrabutyl ketoxime silane, methyl vinyl dibutyl ketoxime silane, methyl tributyl ketoxime silane, methyl tri-acetoxime silane, phenyl tri-butanone oxime silane, vinyl tri-acetoxime silane and vinyl tri-butanone oxime silane.
Further, the plasticizer is simethicone, and the viscosity is 100-500cp; the silane coupling agent is one or two of gamma-aminopropyl triethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane and gamma- (2, 3-glycidoxy) propyl trimethoxysilane; the catalyst is dibutyl tin dilaurate.
Further, when the curing acceleration microcapsule is prepared, the proportion of paraffin, vaseline and water is 40-70 parts by weight: 5-15:30-40 parts; also comprises 0.5-1.0 nonionic surfactant which is added during the preparation of the shell material.
Further, the nonionic surfactant is one or a mixture of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester.
Further, when preparing the curing acceleration microcapsule, firstly heating the shell material paraffin and vaseline to 50-60 ℃ for melting, then adding a nonionic surfactant and uniformly mixing; adding deionized water, maintaining at 50-60deg.C, shearing and emulsifying at 1.2-2.0 RPM for 30-120 min, and granulating by spray congealing method.
The invention also relates to a preparation method of the sealant, which comprises the following steps:
s1, firstly adding alpha, omega-dihydroxyl polydimethylsiloxane and a plasticizer, uniformly mixing in a planetary machine, then adding a reinforcing filler, heating to 100-120 ℃ after completely eating powder, vacuumizing, uniformly mixing, stirring for 1-5 hours, and cooling;
s2, adding a ketoxime silane cross-linking agent, a silane coupling agent and a catalyst into the cooled material of the S1, and uniformly mixing for 20-50 minutes by vacuumizing; adding curing accelerator microcapsule, and mixing at 20-30deg.C under vacuum for 20-50min to obtain single-component sealant for rapidly deep-layer curing photovoltaic module
Further, in the steps S1 and S2, the vacuum degree is controlled below-0.8 MPa.
The invention has the following beneficial effects:
1. according to the sealant for the single-component rapid deep curing photovoltaic module, water molecules are introduced into the single-component sealant by utilizing the microcapsules, so that the same high-efficiency curing performance as that of the double components is obtained, and meanwhile, the selected shell material can be melted at a lower temperature, so that the damage to the sealant caused by high-temperature melting is avoided; the performances of the traditional single-component photovoltaic module sealant, such as workability, mechanical property, ageing resistance, storage performance and the like, are not affected.
2. The shell material is selected from paraffin, vaseline and surfactant, and the shell material can be softened and destroyed at a reasonable temperature through reasonable combination of the paraffin and the vaseline, so that active substances are released; when the proportion of paraffin is too high, the softening and breaking temperature of the shell material is too high, so that the shell material is not suitable for a single-component formula; when the proportion of vaseline is too high, the softening point of the shell material is too low, and the capsule is damaged in the process of making the gel. The action of the surfactant causes the shell material to form a shell and encapsulate the active material to form a shell/core structure.
3. When the photovoltaic module is produced, the single-component sealant provided by the invention can be used without replacing the existing single-component sealant device, and meanwhile, the efficient running water beat is realized.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
preparation of cure promoting microcapsules:
step 1, adding 65 parts by mass of paraffin and 5 parts by mass of vaseline into a stirring kettle, heating to 50-60 ℃ to be in a molten state, and uniformly stirring;
step 2, adding 0.8 part by mass of nonionic surfactant OP-10 into a stirring kettle, and uniformly stirring;
and step 3, slowly adding 35 parts by mass of deionized water, shearing and emulsifying for 60 minutes at the rotating speed of 1.8 ten thousand RPM under the condition of keeping the temperature of 55 ℃, and granulating and forming by a spray congealing method.
Preparation of sealant for single-component rapid deep curing photovoltaic module:
step 1: at room temperature, firstly adding 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane and 5 parts by mass of simethicone into a planetary machine for mixing, vacuumizing, and uniformly stirring for 10 minutes under the vacuum degree of-0.8 Mpa;
step 2: adding 80 parts by mass of nano calcium carbonate, adding for multiple times, mixing until powder is completely eaten, heating to 120 ℃ for surface display, vacuumizing, and uniformly stirring for 3 hours under the vacuum degree of-0.8 Mpa;
step 3: after cooling, 10 parts of methyl tributyl ketoxime group silane cross-linking agent, 5 parts of vinyl tributyl ketoxime group silane, 0.8 part of gamma-aminopropyl triethoxysilane, 0.2 part of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 0.07 part of dibutyl tin dilaurate are added, and the mixture is vacuumized, and the vacuum degree is kept below-0.8 Mpa and stirred for 20 minutes at a constant speed;
step 4: adding 2 parts of curing accelerator microcapsule, maintaining vacuum degree below-0.8 Mpa, stirring at 20-30deg.C for 20 min, discharging, packaging, sealing, and storing.
Example 2:
preparation of cure promoting microcapsules:
step 1, 70 parts by mass of paraffin and 5 parts by mass of vaseline are added into a stirring kettle, heated to 50-60 ℃ to be in a molten state and stirred uniformly;
step 2, adding 0.8 part by mass of nonionic surfactant OP-10 into a stirring kettle, and uniformly stirring;
and step 3, slowly adding 30 parts by mass of deionized water, shearing and emulsifying for 60 minutes at the rotating speed of 1.8 ten thousand RPM under the condition of keeping the temperature of 55 ℃, and granulating and forming by a spray congealing method.
Preparation of sealant for single-component rapid deep curing photovoltaic module:
step 1: at room temperature, firstly adding 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane and 5 parts by mass of simethicone into a planetary machine for mixing, vacuumizing, and uniformly stirring for 10 minutes under the vacuum degree of-0.8 Mpa;
step 2: adding 100 parts by mass of nano calcium carbonate, adding for multiple times, mixing until powder is completely eaten, heating to 120 ℃ for surface display, vacuumizing, and uniformly stirring for 3 hours under the vacuum degree of-0.8 Mpa;
step 3: after cooling, 15 parts of methyl tributyl ketoxime group silane cross-linking agent, 5 parts of vinyl tributyl ketoxime group silane, 0.8 part of gamma-aminopropyl triethoxysilane, 0.2 part of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 0.07 part of dibutyl tin dilaurate are added, and the mixture is vacuumized, and the vacuum degree is kept below-0.8 Mpa and stirred for 20 minutes at a constant speed;
step 4: adding 2 parts of curing accelerator microcapsule, maintaining vacuum degree below-0.8 Mpa, stirring at 20-30deg.C for 20 min, discharging, packaging, sealing, and storing.
Example 3
Preparation of cure promoting microcapsules:
step 1, adding 60 parts by mass of paraffin and 5 parts by mass of vaseline into a stirring kettle, heating to 50-60 ℃ to be in a molten state, and uniformly stirring;
step 2, adding 0.8 part by mass of nonionic surfactant OP-10 into a stirring kettle, and uniformly stirring;
and step 3, slowly adding 40 parts by mass of deionized water, shearing and emulsifying for 60 minutes at the rotating speed of 1.8 ten thousand RPM under the condition of keeping the temperature of 55 ℃, and granulating and forming by a spray congealing method.
Preparation of sealant for single-component rapid deep curing photovoltaic module:
step 1: at room temperature, firstly adding 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane and 5 parts by mass of simethicone into a planetary machine for mixing, vacuumizing, and uniformly stirring for 10 minutes under the vacuum degree of-0.8 Mpa;
step 2: adding 80 parts by mass of nano calcium carbonate, adding for multiple times, mixing until powder is completely eaten, heating to 120 ℃ for surface display, vacuumizing, and uniformly stirring for 3 hours under the vacuum degree of-0.8 Mpa;
step 3: after cooling, 10 parts of methyl tributyl ketoxime group silane cross-linking agent, 5 parts of vinyl tributyl ketoxime group silane, 0.8 part of gamma-aminopropyl triethoxysilane, 0.2 part of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 0.07 part of dibutyl tin dilaurate are added, and the mixture is vacuumized, and the vacuum degree is kept below-0.8 Mpa and stirred for 20 minutes at a constant speed;
step 4: adding 2 parts of curing accelerator microcapsule, maintaining vacuum degree below-0.8 Mpa, stirring at 20-30deg.C for 20 min, discharging, packaging, sealing, and storing.
Example 4
Preparation of cure promoting microcapsules:
step 1, adding 65 parts by mass of paraffin and 5 parts by mass of vaseline into a stirring kettle, heating to 50-60 ℃ to be in a molten state, and uniformly stirring;
step 2, adding 0.8 part by mass of nonionic surfactant OP-10 into a stirring kettle, and uniformly stirring;
and step 3, slowly adding 35 parts by mass of deionized water, shearing and emulsifying for 60 minutes at the rotating speed of 1.8 ten thousand RPM under the condition of keeping the temperature of 55 ℃, and granulating and forming by a spray congealing method.
Preparation of sealant for single-component rapid deep curing photovoltaic module:
step 1: at room temperature, firstly adding 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane and 5 parts by mass of simethicone into a planetary machine for mixing, vacuumizing, and uniformly stirring for 10 minutes under the vacuum degree of-0.8 Mpa;
step 2: adding 100 parts by mass of nano calcium carbonate, adding for multiple times, mixing until powder is completely eaten, heating to 120 ℃ for surface display, vacuumizing, and uniformly stirring for 3 hours under the vacuum degree of-0.8 Mpa;
step 3: after cooling, 10 parts of methyl tributyl ketoxime group silane cross-linking agent, 5 parts of vinyl tributyl ketoxime group silane, 0.8 part of gamma-aminopropyl triethoxysilane, 0.2 part of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 0.07 part of dibutyl tin dilaurate are added, and the mixture is vacuumized, and the vacuum degree is kept below-0.8 Mpa and stirred for 20 minutes at a constant speed;
step 4: adding 5 parts of curing accelerator microcapsule, maintaining vacuum degree below-0.8 Mpa, stirring at 20-30deg.C for 20 min, discharging, packaging, sealing, and storing.
Comparative example 1
Preparation of cure promoting microcapsules:
step 1, adding 65 parts by mass of paraffin and 5 parts by mass of vaseline into a stirring kettle, heating to 50-60 ℃ to be in a molten state, and uniformly stirring;
step 2, adding 0.8 part by mass of nonionic surfactant OP-10 into a stirring kettle, and uniformly stirring;
and step 3, slowly adding 35 parts by mass of deionized water, shearing and emulsifying for 60 minutes at the rotating speed of 1.8 ten thousand RPM under the condition of keeping the temperature of 55 ℃, and granulating and forming by a spray congealing method.
Preparation of sealant for single-component rapid deep curing photovoltaic module:
step 1: at room temperature, firstly adding 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane and 5 parts by mass of simethicone into a planetary machine for mixing, vacuumizing, and uniformly stirring for 10 minutes under the vacuum degree of-0.8 Mpa;
step 2: adding 100 parts by mass of nano calcium carbonate, adding for multiple times, mixing until powder is completely eaten, heating to 120 ℃ for surface display, vacuumizing, and uniformly stirring for 3 hours under the vacuum degree of-0.8 Mpa;
step 3: after cooling, 10 parts of methyl tributylketoxime silane cross-linking agent, 5 parts of vinyl tributylketoxime silane, 0.8 part of gamma-aminopropyl triethoxysilane, 0.2 part of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 0.07 part of dibutyl tin dilaurate are added, and the mixture is vacuumized, and the vacuum degree is kept below-0.8 Mpa and stirred at a constant speed for 20 minutes;
step 4: adding 6 parts of curing accelerator microcapsule, maintaining vacuum degree below-0.8 Mpa, stirring at 20-30deg.C for 20 min, discharging, packaging, sealing, and storing.
Comparative example 2
Preparation of sealant for single-component rapid deep curing photovoltaic module:
step 1: at room temperature, firstly adding 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane and 5 parts by mass of simethicone into a planetary machine for mixing, vacuumizing, and uniformly stirring for 10 minutes under the vacuum degree of-0.8 Mpa;
step 2: adding 100 parts by mass of nano calcium carbonate, adding for multiple times, mixing until powder is completely eaten, heating to 120 ℃ for surface display, vacuumizing, and uniformly stirring for 3 hours under the vacuum degree of-0.8 Mpa;
step 3: after cooling, 10 parts of methyl tributyl ketoxime group silane cross-linking agent, 5 parts of vinyl tributyl ketoxime group silane, 0.8 part by mass of gamma-aminopropyl triethoxy silane, 0.2 part by mass of gamma- (2, 3-glycidoxy) propyl trimethoxy silane and 0.07 part by mass of dibutyl tin dilaurate are added, the vacuum is pumped, the vacuum degree is kept below-0.8 Mpa, the uniform stirring is carried out for 20 minutes, and the materials are discharged, packaged and stored in a sealing mode.
Table 1 below summarizes the compositions of the curing-promoting microcapsules used in the above examples and comparative examples, and table 2 below summarizes the compositions and water contents of the sealants for the one-component rapid deep-cure photovoltaic modules in the above examples and comparative examples.
Comparative example 3
Based on example 1, the only difference is that the ratio of paraffin wax to vaseline used in the cure promoting microcapsules is 80:5.
comparative example 4
Based on example 1, the only difference is that the ratio of paraffin wax to vaseline used in the cure promoting microcapsules is 50:20.
table 1 cure accelerator microcapsule compositions in examples and comparative examples
TABLE 2 composition and moisture content of sealant for fast deep curing photovoltaic modules
And (3) performance detection: the curing depth is carried out according to the specification of 5.8 in national standard GB/T29595-2013; tensile strength is tested according to the shape of II type dumbbell sheet in national standard GB/T528-2009; shear strength, according to the requirement of 5.10 in GB/T29595-2013; ageing by wet heat circulation according to the requirement of 5.19 in GB/T29595-2013.
Table 3 summarizes the performance test results for the examples and comparative examples.
Table 3 summary of performance test fruits
From the results in Table 2 and Table 3, it can be seen that when the water content introduced in the formulation is below 0.8%, the tensile strength and shear strength before and after aging are equivalent to those of the conventional deep dehydration type single component (comparative example 2), almost no difference exists, and all the requirements of GB/T29595-2013 standard can be met; when the amount of water introduced in the formulation is too large (comparative example 1), the colloid will have pores, and the properties before and after aging are inferior to those of the conventional single component, and the requirements of GB/T29595-2013 cannot be satisfied. When the proportion of paraffin in the capsule formula is too high, the shell layer is not easy to soften in the sizing process and the shell layer materials are uniformly mixed in the process of dosing, so that the finally formed rubber is poor in performance due to uneven constitution; when the paraffin proportion in the capsule formulation is too low, the resulting capsule is destroyed during the gum making process, such that a sample that can be tested is ultimately not available.
The foregoing embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without collision. The protection scope of the present invention is defined by the claims, and the protection scope includes equivalent alternatives to the technical features of the claims. I.e., equivalent replacement modifications within the scope of this invention are also within the scope of the invention.
Claims (10)
1. The sealant for the single-component rapid deep curing photovoltaic module is characterized by comprising the following raw materials in parts by weight:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane; 70-100 parts of reinforcing filler; 10-20 parts of ketoximino silane cross-linking agent; 0-10 parts of plasticizer; 1-5 parts of curing accelerating microcapsules; 0.5-1.5 parts of silane coupling agent and 0.06-0.1 part of catalyst;
wherein the curing accelerating microcapsule is prepared by taking deionized water as a core material and taking a mixture of paraffin and vaseline as a shell material, and the weight ratio of the paraffin to the vaseline to the water is 40-70:5-15:30-40 parts; the grain size of the microcapsule is 0.5-50 μm.
2. The sealant according to claim 1, wherein: the alpha, omega-dihydroxy polydimethylsiloxane has a viscosity of 200 to 80000mpa.s or a mixture of viscosities of more than one.
3. The sealant according to claim 1, wherein: the reinforcing filler is at least one or two of precipitated white carbon black, gas phase white carbon black and nano calcium carbonate.
4. The sealant according to claim 1, wherein: the ketoxime silane cross-linking agent is one or a mixture of more of tetrabutylketoxime silane, methyl vinyl diacetone oxime silane, methyl tributylketoxime silane, methyl triacetone oxime silane, phenyl tributylketoxime silane, vinyl triacetone oxime silane and vinyl tributylketoxime silane.
5. The sealant according to claim 1, wherein: the plasticizer is dimethyl silicone oil, and the viscosity is 100-500cp; the silane coupling agent is one or two of gamma-aminopropyl triethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane and gamma- (2, 3-glycidoxy) propyl trimethoxysilane; the catalyst is dibutyl tin dilaurate.
6. The sealant according to any one of claims 1 to 5, wherein: the curing promoting microcapsule also comprises 0.5-1.0 part of nonionic surfactant which is added during the preparation of the shell material.
7. The sealant according to claim 6, wherein: the nonionic surfactant is one or two of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester.
8. The sealant according to claim 6, wherein: when the curing promoting microcapsule is prepared, firstly, the shell material paraffin and vaseline are heated to 50-60 ℃ to be melted, and then, the nonionic surfactant is added and mixed uniformly; adding deionized water, maintaining at 50-60deg.C, shearing and emulsifying at 1.2-2.0 RPM for 30-120 min, and granulating by spray congealing method.
9. The method for preparing the sealant according to any one of claims 1 to 8, comprising the steps of:
s1, firstly adding alpha, omega-dihydroxyl polydimethylsiloxane and a plasticizer, uniformly mixing in a planetary machine, then adding a reinforcing filler, heating to 100-120 ℃ after completely eating powder, vacuumizing, uniformly mixing, stirring for 1-5 hours, and cooling;
s2, adding a ketoxime silane cross-linking agent, a silane coupling agent and a catalyst into the cooled material of the S1, and uniformly mixing for 20-50 minutes by vacuumizing; and adding the curing accelerator microcapsules, and uniformly mixing for 20-50min at the temperature of 20-30 ℃ under vacuum to obtain the sealant for the single-component rapid deep curing photovoltaic module.
10. The method for preparing the sealant according to claim 9, wherein: in the steps S1 and S2, the vacuum degree is controlled below-0.8 MPa.
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