CN109181623B - Silicone sealant for fast curing photovoltaic module and preparation method thereof - Google Patents
Silicone sealant for fast curing photovoltaic module and preparation method thereof Download PDFInfo
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- 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
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- 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
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- 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
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- 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
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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to a silicone sealant for a fast curing photovoltaic module and a preparation method thereof, wherein the silicone sealant is prepared from the following components: the alkoxy-terminated polydimethylsiloxane, the reinforcing agent, the flame retardant, the thixotropic agent, the crosslinking agent, the coupling agent and the first catalyst, wherein the crosslinking agent is multifunctional polysiloxane, the coupling agent is a secondary amine silane coupling agent in the structural formula, and the first catalyst is a chelate titanate catalyst. According to the invention, the multifunctional polysiloxane is used as a cross-linking agent, and is compounded with the secondary amine silane coupling agent, the chelate titanate catalyst and the flame retardant, so that the silicone sealant for the rapidly cured photovoltaic module, which is suitable for various bonding materials, has excellent bonding strength, is rapidly cured and is not easy to yellow, can be obtained.
Description
Technical Field
The invention relates to a silicone sealant for a fast curing photovoltaic module and a preparation method thereof, belonging to the field of silicone sealants for photovoltaic modules.
Background
The solar photovoltaic adhesive is a sealant which absorbs moisture in air at room temperature and is cured, and can be used for bonding and sealing various back plates, aluminum alloy frames, junction boxes and the like, so that photovoltaic modules under various severe conditions are protected. The main raw material of the silicone sealant is 107 glue and other linear polysiloxanes, the main chain of the silicone sealant mainly comprises Si-O-Si bonds, the Si-O-Si bonds are higher than the ultraviolet bond energy, and a cross-linking agent and a basic polymer react to form a net-shaped structure in the curing process, so that the silicone sealant has excellent cohesiveness, weather resistance and ultraviolet resistance compared with other types of sealants, and is also often applied to sealing of solar photovoltaic components. The silicone sealant is divided into a single-component silicone sealant and a two-component silicone sealant, the single-component silicone sealant does not need to be added with an additional curing agent, the curing is realized by contacting moisture in the air to generate the change of physical properties, and the single-component silicone sealant with a structure can be divided into a deacetylation type, a ketoxime type, a dealcoholization type and a deamidation type according to released substances in the curing process; the two-component silicone sealant is divided into two components, and the two components are cured after the two groups of mucilage are mixed.
Because the photovoltaic module is placed outdoors for a long time, the silicone sealant for the solar photovoltaic module is required to have good ultraviolet resistance, high and low temperature resistance, moisture resistance, electrical insulation and good cohesiveness to different materials. Most of silicone sealants commonly used for solar photovoltaic modules on the market at present are deoximated silicone sealants and dealcoholized silicone sealants, wherein ketoxime released by the deoximated silicone sealants during vulcanization is corrosive to copper, lead, zinc and polycarbonate, and the application of the deoximated silicone sealants in the electronic industry is limited; the dealcoholized silicone sealant has no corrosiveness to any material and does not affect the health of workers. However, the curing speed of the dealcoholized silicone sealant is relatively slow, which is not favorable for the continuous operation of photovoltaic plants. Meanwhile, different bonding materials can be involved in the production process of the solar photovoltaic module, and the silicone sealant of the solar photovoltaic module, which has excellent bonding property to various materials, is less in the market at present, so that the dealcoholized silicone sealant which has excellent performance and high curing speed and is used for the solar photovoltaic module is developed, and the trend is great.
The Chinese invention patent application publication CN108059945A discloses an organosilicon sealant for photovoltaic glass components and a preparation method thereof, wherein the organosilicon sealant comprises alkoxy-terminated polydimethylsiloxane, active nano calcium carbonate, modified fumed silica, a silicone oil plasticizer, a cross-linking agent, a catalyst and an adhesion promoter. The organic silicon sealant disclosed by the invention is high in strength, good in elasticity, excellent in bonding performance to a base material, and excellent in weather resistance, has a performance retention rate of over 80% in a long-term environment of smoke, ultraviolet rays, high temperature and high humidity, and is suitable for structural bonding and sealing of a photovoltaic dual-glass assembly.
Chinese patent application publication No. CN101805585A discloses a single-component flame-retardant solar photovoltaic module sealant and a preparation method thereof, wherein the sealant comprises end-capped polydimethylsiloxane, a plasticizer, a filler, a flame retardant, a cross-linking agent, a hydroxyl scavenging agent, a tackifier and a catalyst. The flame retardant property of the sealant reaches V0 level, the adhesive force to the photovoltaic cell glass is good, and the sealant has no corrosion to an EVA adhesive film and a cell circuit.
Comparative analysis the above patents do not describe the curing speed of the gel. In order to meet the market demand, the inventor researches a solar photovoltaic adhesive which is suitable for various bonding materials, excellent in various performances and high in curing speed.
Disclosure of Invention
The invention aims at overcoming the defects of relatively slow curing speed and wide bonding in the prior art, namely the invention provides the silicone sealant for the fast curing photovoltaic module and the preparation method thereof. .
In order to solve the technical problems, the technical scheme adopted by the invention is to provide a silicone sealant for a fast curing photovoltaic module and a preparation method thereof, wherein the silicone sealant comprises the following components: alkoxy-terminated polydimethylsiloxane, reinforcing agent, flame retardant, thixotropic agent, crosslinking agent, coupling agent and first catalyst, wherein the crosslinking agent is multifunctional polysiloxane, and the structural formula of the multifunctional polysiloxane is shown in the specification
Wherein R is selected from-Si (OCH)3)3、-Si(OC2H5)3、-CH2-Si(OCH3)3、-CH2-Si(OC2H5)3N is an integer of 0 to 10, the coupling agent is a secondary amine silane coupling agent, and the first catalyst is a chelate titanate catalyst. The multifunctional polysiloxane is dendritic in structure, is easy to be uniformly mixed with other components, and is beneficial to the passing of water vapor. The secondary amine silane coupling agent can improve the adhesive property of the sealant, and the chelate titanate catalyst can reduce the yellowing of the sealant.
Preferably, the component for preparing the multifunctional polysiloxane comprises siloxane containing terminal vinyl, siloxane containing terminal hydrogen and a second catalyst, wherein the siloxane containing terminal vinyl is
Or R-CH ═ CH2At least one of, the terminal hydrogen group-containing siloxane is
Or at least one of R-H, the second catalyst is a platinum catalyst, and the second catalyst is a Karster catalyst, namely platinum (0) -1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane with the CAS number of 68478-92-2.
Preferably, in the process of preparing the multifunctional polysiloxane, the siloxane containing the terminal hydrogen group is dropwise added into the siloxane containing the terminal vinyl group and the second catalyst under the condition of introducing nitrogen at the temperature of 60-80 ℃ while stirring, after the dropwise addition is completed, stirring reaction is carried out for 1-3 hours, then activated carbon is added, stirring is continued for 1 hour, and then filtering and vacuumizing are carried out, so as to obtain the multifunctional polysiloxane.
The mass ratio of the terminal hydrogen group-containing siloxane to the terminal vinyl group-containing siloxane is 0.05-4: 1.
Preferably, the alkoxy-terminated polydimethylsiloxane has a viscosity of 5 pas to 50 pas at 25 ℃.
Preferably, the polydimethylsiloxane has a viscosity of 0.1 pas-10 pas at 25 ℃.
Preferably, the coupling agent is at least one of bis- [3- (triethoxysilyl) -propyl ] -amine and bis- [3- (trimethoxy-silyl) -propyl ] -amine.
Preferably, the first catalyst is at least one of an ethyl acetoacetate chelate of isopropyl titanate, an acetylacetone chelate of isopropyl titanate, an ethyl acetoacetate chelate of t-butyl titanate, and an acetylacetone chelate of t-butyl titanate.
Preferably, the reinforcing agent is nano calcium carbonate treated by fatty acid or resin acid, the particle size of the nano calcium carbonate is 10-100nm, the thixotropic agent is fumed silica treated by hexamethyldisilazane, and the specific surface area is 100-200 m-2(ii) in terms of/g. The nano calcium carbonate and the fumed silica which are subjected to surface treatment are selected to improve the bonding strength and the weather resistance of the sealant.
Preferably, the flame retardant is an inorganic non-halogen flame retardant, and the flame retardant is at least one of borate, hydroxide, inorganic phosphorus compounds and inorganic nitrogen compounds.
Preferably, the flame retardant is one or a combination of more of aluminum hydroxide, magnesium hydroxide, zinc borate, melamine cyanurate and ammonium polyphosphate.
Preferably, the alkoxy-terminated polydimethylsiloxane is selected from the group consisting of those produced by Jiangsu Konghe New Material Co., Ltd
One or more of F-10A, F-40A and J-200, wherein the polydimethylsiloxane is selected from XHG-201 produced by New chemical group of GmbH, Zhejiang, the reinforcing agent is selected from nano calcium carbonate produced by New Material science and technology, Guangxi Huana, and the flame retardant is selected from AH-108, AH-1011 and AH1015 produced by Shandong Shipo chemical science and technologyAnd at least one of AH-1020, the thixotropic agent is fumed silica produced by Synsheng silicon industries, Inc., the coupling agent is at least one of JH-A117, JH-A1171 and JH-A118 produced by Jianghan Fine chemical industries, Inc., Jingzhou, the first catalyst is TYZOR produced by Doffkat chemical company@726、TYZOR@IBAY、TYZOR@PITA and TYZOR@AA, and the second catalyst is selected from platinum catalysts produced by Shanghai silicon Bao high-tech materials, Inc.
The invention also provides a preparation method of the silicone sealant for the fast curing photovoltaic module, which is characterized by comprising the following steps:
(1) adding alkoxy-terminated polydimethylsiloxane, reinforcing agent and flame retardant into a stirring kettle, and blending and kneading for 2-4 hours at the temperature of 110-130 ℃ and the vacuum degree of-0.085-0.099 MPa;
(2) cooling to below 50 deg.C, adding thixotropic agent, and stirring for 60-100 min;
(3) adding coupling agent, stirring for 15 min;
(4) and (2) mixing the multifunctional siloxane and the first catalyst, adding the mixture and polydimethylsiloxane into the reaction kettle, and stirring for 30min under the vacuum degree of-0.085-0.099 MPa to obtain the silicone sealant for the fast curing photovoltaic module.
In a word, by adopting the silicone sealant for the fast curing photovoltaic module and the preparation method thereof, disclosed by the invention, the silicone sealant for the fast curing photovoltaic module, which is suitable for various bonding materials, has excellent bonding strength, is fast cured and is not easy to yellow, can be obtained by compounding the multifunctional polysiloxane serving as a cross-linking agent, a secondary amine silane coupling agent, a chelating type titanate catalyst and a flame retardant.
Detailed Description
The following detailed description of embodiments of the present invention is not intended to limit the scope of the invention.
Example 1
The invention provides a silicone sealant for a fast curing photovoltaic module, which comprises alkoxy-terminated polydimethylsiloxane100 parts of siloxane, 5 parts of polydimethylsiloxane, 80 parts of reinforcing agent, 30 parts of flame retardant, 2 parts of thixotropic agent, 10 parts of cross-linking agent, 2 parts of coupling agent and 3 parts of first catalyst, wherein the cross-linking agent is multifunctional polysiloxane. The multifunctional polysiloxane has a structural formula of
Wherein R is selected from-Si (OCH)3)3And n is selected from 8.
The component for preparing the multifunctional polysiloxane comprises siloxane containing terminal vinyl, siloxane containing terminal hydrogen and a second catalyst
The siloxane containing the end hydrogen group is R-H, the mass ratio of the siloxane containing the end hydrogen group to the siloxane containing the end vinyl group is 0.6:1, and the second catalyst is selected from platinum catalysts produced by Shanghai Silibao high-tech materials Co. In the process of preparing the multifunctional polysiloxane, the siloxane containing the terminal hydrogen group is dropwise added into the mixture of the siloxane containing the terminal vinyl group and the second catalyst under the condition of introducing nitrogen at the temperature of 60 ℃, stirring and reacting for 1 hour after the dropwise addition is finished, then adding activated carbon, continuously stirring for 1 hour, and then filtering and vacuumizing to obtain the multifunctional polysiloxane.
The viscosity of the alkoxy-terminated polydimethylsiloxane at 25 ℃ is 5 pas.
The polydimethylsiloxane is selected from XHG-201 produced by Xinan chemical group of Zhejiang, and has a viscosity of 5 pas at 25 ℃.
The reinforcing agent is selected from nano calcium carbonate produced by Guangxi Huana new material science and technology limited company, and the particle size is 80 nm.
The flame retardant is AH-1011 produced by Shandong lion nation chemical technology Co.
The thixotropic agent is fumed silica produced by Hesheng silicon industry Co., Ltd, and has a specific surface area of 150m2/g。
The coupling agent is selected from JH-A1171 produced by Jianghan Fine chemical Co., Ltd.
The first catalyst is selected from TYZOR manufactured by Doffkat chemical company@IBAY。
The preparation method of the silicone sealant for the fast curing photovoltaic module of the embodiment 1 comprises the following steps:
(1) adding alkoxy end-capped polydimethylsiloxane, a reinforcing agent and a flame retardant into a stirring kettle, and blending and kneading for 2 hours at the temperature of 130 ℃ and the vacuum degree of-0.085 MPa;
(2) cooling to below 50 deg.C, adding thixotropic agent, and stirring for 60 min;
(3) adding coupling agent, stirring for 15 min;
(4) and mixing the multifunctional siloxane and the first catalyst, adding the mixture and polydimethylsiloxane into the reaction kettle, and stirring for 30min under the vacuum degree of-0.085 MPa to obtain the silicone sealant for the rapidly cured photovoltaic module.
Example 2
The fast curing photovoltaic module of example 2 was distinguished by the silicone encapsulant and example 1: 10 parts of polydimethylsiloxane, 100 parts of reinforcing agent, 20 parts of flame retardant, 4 parts of thixotropic agent, 6 parts of cross-linking agent, 4 parts of coupling agent and 4 parts of first catalyst, wherein the cross-linking agent is polyfunctional polysiloxane. The multifunctional polysiloxane has a structural formula of
Wherein R is selected from-CH2-Si(OCH3)3And n is selected from 10.
The component for preparing the multifunctional polysiloxane comprises siloxane containing terminal vinyl, siloxane containing terminal hydrogen and a second catalyst, wherein the siloxane containing terminal vinyl is R-CH ═ CH2The terminal hydrogen group-containing siloxane is
The mass between the terminal hydrogen group-containing siloxane and the terminal vinyl group-containing siloxaneThe ratio is 0.5:1, and the second catalyst is selected from platinum catalysts produced by Shanghai Silibao advanced materials Co. In the process of preparing the multifunctional polysiloxane, the siloxane containing the terminal hydrogen group is dropwise added into the mixture of the siloxane containing the terminal vinyl group and the second catalyst under the condition of introducing nitrogen at the temperature of 80 ℃, stirring and reacting are carried out for 3 hours after the dropwise addition is finished, then activated carbon is added, stirring is continuously carried out for 1 hour, and then filtering and vacuumizing are carried out, so that the multifunctional polysiloxane is obtained.
The viscosity of the alkoxy-terminated polydimethylsiloxane at 25 ℃ is 50 pas.
The polydimethylsiloxane had a viscosity of 3.5 pas at 25 ℃.
The reinforcing agent is selected from nano calcium carbonate produced by Guangxi Huana new material science and technology limited company, and the particle size is 100 nm.
The flame retardant is AH-1015 produced by Shandong lion chemical technology Co.
The thixotropic agent is fumed silica produced by Hesheng silicon industry Co., Ltd, and has a specific surface area of 200m2/g。
The coupling agent is selected from JH-A118 produced by Jianghan Fine chemical Co., Ltd.
The first catalyst is selected from TYZOR manufactured by Doffkat chemical company@PITA。
The preparation method of the silicone sealant for the fast curing photovoltaic module in the embodiment 2 is different from that in the embodiment 1 in that:
(1) adding alkoxy end-capped polydimethylsiloxane, a reinforcing agent and a flame retardant into a stirring kettle, and blending and kneading for 3 hours at the temperature of 120 ℃ and the vacuum degree of-0.092 MPa;
(2) cooling to below 50 deg.C, adding thixotropic agent, and stirring for 80 min;
(3) adding coupling agent, stirring for 15 min;
(4) and firstly mixing the multifunctional siloxane and the first catalyst, then adding the mixture and polydimethylsiloxane into the reaction kettle, and stirring for 30min under the vacuum degree of-0.095 MPa to obtain the silicone sealant for the fast curing photovoltaic module.
Example 3
The fast curing photovoltaic module of example 3 was distinguished by silicone encapsulant and example 1 by: 3 parts of polydimethylsiloxane, 90 parts of reinforcing agent, 10 parts of flame retardant, 10 parts of thixotropic agent, 8 parts of cross-linking agent, 3 parts of coupling agent and 5 parts of first catalyst, wherein the cross-linking agent is polyfunctional polysiloxane. The multifunctional polysiloxane has a structural formula of
Wherein R is selected from-CH2-Si(OC2H5)3And n is selected from 3.
The component for preparing the multifunctional polysiloxane comprises siloxane containing terminal vinyl, siloxane containing terminal hydrogen and a second catalyst, wherein the siloxane containing terminal vinyl is R-CH ═ CH2The terminal hydrogen group-containing siloxane is
The mass ratio of the siloxane containing the terminal hydrogen group to the siloxane containing the terminal vinyl group is 2:1, and the second catalyst is selected from platinum catalysts produced by Shanghai Silibao advanced materials Co. In the process of preparing the multifunctional polysiloxane, the siloxane containing the terminal hydrogen group is dropwise added into the mixture of the siloxane containing the terminal vinyl group and the second catalyst under the condition of introducing nitrogen at 78 ℃, stirring and reacting for 3 hours after the dropwise addition is finished, then activated carbon is added, stirring is continued for 1 hour, and then filtering and vacuumizing are carried out, so that the multifunctional polysiloxane is obtained.
The viscosity of the alkoxy-terminated polydimethylsiloxane at 25 ℃ is 40 Pa.s.
The polydimethylsiloxane is selected from XHG-201 produced by Xinan chemical group of Zhejiang, and has a viscosity of 8 pas at 25 ℃.
The reinforcing agent is selected from nano calcium carbonate produced by Guangxi Huana new material science and technology limited company, and the particle size is 40 nm.
The flame retardant is AH-1015 produced by Shandong lion chemical technology Co.
The thixotropic agent is selected from fumed silica produced by Hesheng silicon industries, Ltd, and has a specific surface area of 180m2/g。
The coupling agent is selected from JH-A118 produced by Jianghan Fine chemical Co., Ltd.
The first catalyst is selected from TYZOR manufactured by Doffkat chemical company@AA。
The preparation method of the silicone sealant for the fast curing photovoltaic module in the embodiment 3 is different from that in the embodiment 1 in that:
(1) adding alkoxy end-capped polydimethylsiloxane, a reinforcing agent and a flame retardant into a stirring kettle, and blending and kneading for 4 hours at the temperature of 110 ℃ and the vacuum degree of-0.099 MPa;
(2) after cooling to below 50 ℃, adding a thixotropic agent, and stirring for 100 min;
(3) adding coupling agent, stirring for 15 min;
(4) and firstly mixing the multifunctional siloxane and the first catalyst, then adding the mixture and polydimethylsiloxane into the reaction kettle, and stirring for 30min under the vacuum degree of-0.099 MPa to obtain the silicone sealant for the fast curing photovoltaic module.
Example 4
The fast curing photovoltaic module of example 4 was distinguished by silicone encapsulant and example 1 by: 1 part of polydimethylsiloxane, 10 parts of flame retardant, 6 parts of thixotropic agent, 5 parts of cross-linking agent, 4 parts of coupling agent and 2 parts of first catalyst, wherein the cross-linking agent is multifunctional polysiloxane. The multifunctional polysiloxane has a structural formula of
Wherein R is selected from-CH2-Si(OC2H5)3And n is selected from 1.
The component for preparing the multifunctional polysiloxane comprises siloxane containing terminal vinyl, siloxane containing terminal hydrogen and a second catalyst, wherein the siloxane containing terminal vinyl is R-CH ═ CH2The terminal hydrogen group-containing siloxaneIs composed of
The mass ratio of the siloxane containing the terminal hydrogen group to the siloxane containing the terminal vinyl group is 4:1, and the second catalyst is selected from platinum catalysts produced by Shanghai Silibao advanced materials Co. In the process of preparing the multifunctional polysiloxane, the siloxane containing the terminal hydrogen group is dropwise added into the mixture of the siloxane containing the terminal vinyl group and the second catalyst under the condition of introducing nitrogen at 78 ℃, stirring and reacting for 3 hours after the dropwise addition is finished, then activated carbon is added, stirring is continued for 1 hour, and then filtering and vacuumizing are carried out, so that the multifunctional polysiloxane is obtained.
The viscosity of the alkoxy-terminated polydimethylsiloxane at 25 ℃ is 30 pas.
The polydimethylsiloxane is selected from XHG-201 produced by Xinan chemical group of Zhejiang, and has a viscosity of 10 pas at 25 ℃.
The reinforcing agent is selected from nano calcium carbonate produced by Guangxi Huana new material science and technology limited company, and the particle size is 10 nm.
The flame retardant is AH-108 produced by Shandong lion chemical technology Co.
The thixotropic agent is selected from fumed silica produced by Hesheng silicon industries, Ltd, and has a specific surface area of 100m2/g。
The coupling agent is selected from JH-A117 produced by Jianghan Fine chemical Co., Ltd.
The first catalyst is selected from TYZOR manufactured by Doffkat chemical company@PITA。
Preferred embodiment(s) of the invention
The difference between the silicone sealant for the fast curing photovoltaic module of the preferred embodiment and the silicone sealant of embodiment 1 is that: 10 parts of polydimethylsiloxane, 100 parts of reinforcing agent, 20 parts of flame retardant, 4 parts of thixotropic agent, 6 parts of cross-linking agent and 3.5 parts of first catalyst, wherein the cross-linking agent is multifunctional polysiloxane. The multifunctional polysiloxane has a structural formula of
Wherein R is selected from-Si (OC)2H5)3And n is selected from 10.
The component for preparing the multifunctional polysiloxane comprises siloxane containing terminal vinyl, siloxane containing terminal hydrogen and a second catalyst
The siloxane containing the end hydrogen group is R-H, the mass ratio of the siloxane containing the end hydrogen group to the siloxane containing the end vinyl group is 0.5:1, and the second catalyst is selected from platinum catalysts produced by Shanghai Silibao high-tech materials Co. In the process of preparing the multifunctional polysiloxane, the siloxane containing the terminal hydrogen group is dropwise added into the mixture of the siloxane containing the terminal vinyl group and the second catalyst under the condition of introducing nitrogen at 78 ℃, stirring and reacting for 3 hours after the dropwise addition is finished, then activated carbon is added, stirring is continued for 1 hour, and then filtering and vacuumizing are carried out, so that the multifunctional polysiloxane is obtained.
The alkoxy-terminated polydimethylsiloxane is selected from the group consisting of those produced by Jiangsu Konghe New Material Ltd
J-200, viscosity at 25 ℃ of 20 pas.
The polydimethylsiloxane is selected from XHG-201 produced by Xinan chemical group of Zhejiang, and has a viscosity of 1 pas at 25 ℃.
The reinforcing agent is selected from nano calcium carbonate produced by Guangxi Huana new material science and technology limited company, and the particle size is 80 nm.
The flame retardant is AH-108 produced by Shandong lion chemical technology Co.
The thixotropic agent is fumed silica produced by Hesheng silicon industry Co., Ltd, and has a specific surface area of 200m2/g。
The coupling agent is selected from JH-A117 produced by Jianghan Fine chemical Co., Ltd.
The first catalyst is selected from TYZOR manufactured by Doffkat chemical company@726。
Comparative example 1
The silicone sealant of comparative example 1 and example 1 differed in that: the cross-linking agent is methyl trimethoxy silane.
Comparative example 2
The silicone sealant of comparative example 2 and example 1 differed in that: the cross-linking agent is methyl triethoxysilane, and the coupling agent is gamma-glycidoxypropyltrimethoxysilane.
Comparative example 3
Comparative example 3 was selected from commercially available silicone sealants also used in photovoltaic modules.
The relevant physicochemical properties and the test standards of the finished products obtained by the invention through the examples 1-4 and the preferred examples and the comparative examples 1-3 are shown in the following table:
in addition, the curing speed was determined by the method of Standard GB/T32369-2015 determination of the extent of curing of the sealants, i.e.the two-wedge trough method.
From the performance data in the table, it can be seen that the silicone sealant for photovoltaic modules prepared in examples 1 to 4 and the preferred examples has a faster curing rate and better expansion and contraction performance, is suitable for more bonding materials, and can be applied to various construction scenes. The elastic fabric can still keep better elasticity under the conditions of ultraviolet irradiation, thermal cycle, damp freezing and damp heat, and is suitable for outdoor use. By visual inspection, compared with comparative examples 1-3, examples 1-4 and the preferred examples, the silicone sealant for the photovoltaic module prepared by the method has no obvious yellowing phenomenon and almost no yellowing phenomenon after respectively undergoing an ultraviolet irradiation test, a thermal cycle test, a wet-freeze test and a wet-heat test.
The invention has the beneficial effects that: the multifunctional polysiloxane is used as a cross-linking agent, and is compounded with a secondary amine silane coupling agent, a chelate titanate catalyst and a flame retardant, so that the one-component dealcoholized fast curing silicone sealant for the photovoltaic module, which is suitable for various bonding materials, has excellent bonding strength, is fast cured and is not easy to yellow, can be obtained.
Claims (8)
1. The silicone sealant for the fast curing photovoltaic module is characterized by being prepared from the following components in parts by weight:
wherein the cross-linking agent is multifunctional polysiloxane, and the structural formula of the multifunctional polysiloxane is shown in the specification
Wherein R is selected from-Si (OCH)3)3or-Si (OC)2H5)3When n is selected from an integer of 3 to 10, R is selected from-CH2-Si(OCH3)3or-CH2-Si(OC2H5)3When n is an integer of 1 to 10, the viscosity of the alkoxy-terminated polydimethylsiloxane at 25 ℃ is 25 Pa.s to 50 Pa.s, the viscosity of the polydimethylsiloxane at 25 ℃ is 0.1 Pa.s to 10 Pa.s, the coupling agent is a secondary amine silane coupling agent, and the first catalyst is a chelate titanate catalyst.
2. The silicone sealant for fast curing photovoltaic modules according to claim 1, wherein the component for preparing said multifunctional polysiloxane comprises a vinyl-terminated siloxane, a hydrogen-terminated siloxane and a second catalyst, said vinyl-terminated siloxane being
Or R-CH ═ CH2At least one of, the terminal hydrogen group-containing siloxane is
Or R-H, and the second catalyst is a Karster catalyst.
3. The silicone sealant for fast curing photovoltaic modules according to claim 2, wherein the multifunctional polysiloxane is prepared by adding the siloxane containing terminal hydrogen groups dropwise to the mixture of the siloxane containing terminal vinyl groups and the second catalyst under nitrogen atmosphere at a temperature of 60-80 ℃ while stirring, stirring for 1-3 hours after the completion of the dropwise addition, adding activated carbon, stirring for 1 hour, filtering and vacuumizing.
4. The silicone sealant for fast curing photovoltaic modules according to claim 2, wherein the mass ratio between the terminal hydrogen group-containing siloxane and the terminal vinyl group-containing siloxane is 0.05-4: 1.
5. The silicone sealant for fast curing photovoltaic modules according to claim 1, wherein said first catalyst is at least one of ethyl acetoacetate chelate of isopropyl titanate, acetylacetone chelate of isopropyl titanate, ethyl acetoacetate chelate of t-butyl titanate, and acetylacetone chelate of t-butyl titanate.
6. The silicone sealant for fast curing photovoltaic module as claimed in claim 1, wherein the reinforcing agent is nano calcium carbonate treated with fatty acid or resin acid, the nano calcium carbonate has a particle size of 10-100nm, the thixotropic agent is fumed silica treated with hexamethyldisilazane, and the specific surface area is 100-200m2/g。
7. The silicone sealant for fast curing photovoltaic modules according to claim 1, wherein said coupling agent is at least one of bis- [3- (triethoxysilyl) -propyl ] -amine and bis- [3- (trimethoxy-silyl) -propyl ] -amine.
8. The preparation method of the silicone sealant for the fast curing photovoltaic module, based on the claim 1, is characterized by comprising the following steps:
(1) adding alkoxy-terminated polydimethylsiloxane, reinforcing agent and flame retardant into a stirring kettle, and blending and kneading for 2-4 hours at the temperature of 110-130 ℃ and the vacuum degree of-0.085-0.099 MPa;
(2) cooling to below 50 deg.C, adding thixotropic agent, and stirring for 60-100 min;
(3) adding a secondary amine silane coupling agent, and stirring for 15 min;
(4) and (2) mixing the multifunctional siloxane and the chelate titanate catalyst, adding the mixture and polydimethylsiloxane into the reaction kettle, and stirring for 30min under the vacuum degree of-0.085-0.099 MPa to obtain the silicone sealant for the fast curing photovoltaic module.
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| CN111320964A (en) * | 2020-03-20 | 2020-06-23 | 佛山市金云信硅材料制品有限公司 | Silicone sealant and preparation method thereof |
| CN111334186A (en) * | 2020-04-26 | 2020-06-26 | 浙江励德有机硅材料有限公司 | Room-temperature self-curing insulation coated silica gel and preparation method thereof |
| CN112143451A (en) * | 2020-10-13 | 2020-12-29 | 广州市高士实业有限公司 | Single-component dealcoholized room temperature vulcanized silicone sealant and preparation method thereof |
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