CN109135660B - Dealcoholized bi-component sealant and preparation method thereof - Google Patents
Dealcoholized bi-component sealant and preparation method thereof Download PDFInfo
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- CN109135660B CN109135660B CN201810971458.XA CN201810971458A CN109135660B CN 109135660 B CN109135660 B CN 109135660B CN 201810971458 A CN201810971458 A CN 201810971458A CN 109135660 B CN109135660 B CN 109135660B
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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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- 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
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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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention provides dealcoholized double-component sealant which comprises the following components in percentage by mass of 100: (2-20) a component A and a component B; the component A comprises: 100 parts by weight of hydroxyl-terminated polydimethylsiloxane; 5-150 parts by weight of solid filler; the component B comprises: 8-35 parts of a crosslinking agent; 1-20 parts by weight of tackifier; 0.1 to 1 portion of catalyst; the crosslinking agent has the general formula: (R)1O)3‑aR2 aSi‑R3‑SiR4 b(OR5)3‑b；R1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1; the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a specific Si-N bond compound. The dealcoholized double-component sealant provided by the invention adopts components with specific content, realizes better interaction, has good bonding performance, durability, sealing performance and long-term storage stability, and is suitable for sealing photovoltaic components, automobile components, electronic and electric appliances, glass for buildings, curtain wall components and the like.
Description
Technical Field
The invention relates to the technical field of organosilicon room temperature vulcanized silicone rubber, in particular to dealcoholized double-component sealant and a preparation method thereof.
Background
Room temperature vulcanizable silicone sealants that cure with moisture in the air at room temperature to provide silicone rubbers are available in a wide variety of markets and are widely used. The room temperature vulcanized silicone rubber which takes hydroxyl or alkoxy silicon-based end-capped polydimethylsiloxane and alkoxy silane as main raw materials and releases alcohol compounds to be cured in the presence of an organic metal compound catalyst has the advantages of no bromine, no corrosion to metals and the like, and is widely applied not only as a sealing material and an adhesive material in the fields of photovoltaic modules, automobiles, electric appliances and electronics, but also in the field of buildings. Specific room temperature-curable silicone rubber compositions can be made in one-component and two-component forms. The curing of the single-component adhesive depends on the humidity of the atmosphere, but the curing of the two-component adhesive does not depend on the humidity of the atmosphere. The two-component type of rubber is considered to be an excellent deep-curing silicone rubber, which can bring about almost simultaneous and uniform curing of the surface layer and the interior.
In recent years, solar cells, LED lamps, and the like have been rapidly developed as representative products of renewable energy; meanwhile, the demand of the organosilicon sealant with the characteristics of low cost, integral uniform curing, quick curing, short operation time and the like is increasing day by day, namely, deep-layer curing organosilicon rubber is more and more valued by people and is widely applied; it is also widely used in the field of automotive components.
However, there are still some problems in the practical application of two-component alcohol-type glues. For example, in a durability test, a phenomenon occurs in which a cured product of a solar cell-applied adhesive is turned into a liquid state or a re-softened state under a high-temperature and high-humidity condition. Further, the vulcanization performance and physical properties thereof gradually deteriorate or disappear with the lapse of storage time, and the adhesiveness particularly to a base material such as glass, plastic, or metal is gradually deteriorated. Therefore, in the fields of solar batteries, automobiles, LED lamps and the like, the sealant is required to have no corrosion, fast curing, good adhesion durability and storage stability while having adhesion. In the building field, low cost, uniform integral curing, short operation time and the like are also required for the organic silica gel; in particular, the requirements in the application fields of 2-time sealing, structural bonding and the like of the multilayer glass are higher and higher. However, the dealcoholized two-component sealant for buildings also has the following problems: when the glass is soaked in water or irradiated by water ultraviolet light for a long time, the reinforced glass of doors and windows for buildings often has the phenomena of reduced adhesion and peeling. In order to solve the problem, the prior art improves the bonding durability by adding some epoxy coupling agents, amine coupling agents and the like, but the bonding durability of the glue and the long-term storage stability of the glue are still lacked under the harsh environmental conditions of soaking in water and the like.
Disclosure of Invention
In view of the above, the invention aims to provide a dealcoholized two-component sealant and a preparation method thereof, and the dealcoholized two-component sealant provided by the invention has good adhesive property, durability, sealing property and long-term storage stability, and is suitable for sealing photovoltaic components, automobile components, electronic and electric appliances, glass for buildings, curtain wall components and the like.
The invention provides dealcoholized double-component sealant which comprises the following components in percentage by mass of 100: (2-20) a component A and a component B;
the component A comprises:
100 parts by weight of hydroxyl-terminated polydimethylsiloxane;
5-150 parts by weight of solid filler;
the component B comprises:
8-35 parts of a crosslinking agent;
1-20 parts by weight of tackifier;
0.1 to 1 portion of catalyst;
the crosslinking agent has a general formula shown in formula (I):
(R1O)3-aR2 aSi-R3-SiR4 b(OR5)3-bformula (I)
In the formula (I), R1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1;
the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a Si-N bond compound.
Preferably, the hydroxyl-terminated polydimethylsiloxane has the general formula shown in formula (II):
HO-(SiMe2O)nSiMe2OH formula (II);
in the formula (II), n is 25 ℃ so that the kinematic viscosity of the hydroxyl-terminated polydimethylsiloxane is 200mm2/s～1000000mm2Positive number in/s.
Preferably, the solid filler comprises one or more of calcium carbonate, white carbon, quartz powder, hollow glass microspheres, diatomite, titanium dioxide, aluminum hydroxide, aluminum oxide, zinc oxide, magnesium oxide, zinc oxide and zinc carbonate.
Preferably, the preparation method of the tackifier specifically comprises the following steps:
mixing a mixture of 1: 2: (0.2-3) mixing the amino coupling agent, the epoxy coupling agent and the Si-N bond compound, and reacting at 20-60 ℃ for 48-120 h to obtain the tackifier.
Preferably, the amino coupling agent comprises one or more of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane, gamma-aminoethylaminopropyltriethoxysilane, bis [3- (triethoxysilyl) propyl ] amine, bis (3-trimethoxysilylpropyl) amine, bis [3- (trimethoxysilyl) propyl ] ethylenediamine and bis [3- (triethoxysilyl) propyl ] ethylenediamine.
Preferably, the epoxy-based coupling agent includes one or more of gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma-glycidoxypropylmethyldiethoxysilane, gamma-glycidoxypropylmethyldimethoxysilane, and β - (3, 4-epoxycyclohexane) ethyltrimethoxysilane.
Preferably, the Si-N bond compound is a compound containing at least one or more Si-N bonds in the molecule and the nitrogen atom is linked to a silicon atom containing one or more alkoxy groups by a carbon chain of one or more carbon atoms, and includes 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane, 2-methoxy-2, 4-dimethyl-1-aza-2-silacyclopentane-1-ethylamine, 2-diethoxy-1-aza-2-silacyclopentane, [1- (3-triethoxysilyl) propyl ] -2, 2-diethoxy-1-aza-2-silacyclopentane, nitrogen- (2-aminoethyl) -2,2, 4-trimethyl-1-aza-2-silacyclopentane, 2-dimethoxy-1-aza-2-silacyclopentane-1-ethylamine, N-trimethylsilyl-3-aminopropyltrimethoxysilane and N-trimethylsilyl-3-aminopropyltriethoxysilane.
Preferably, the catalyst comprises one or more of dibutyltin dilaurate, dioctyltin dilaurate, dimethyltin dioctanoate and dibutyltin diacetate.
The invention also provides a preparation method of the dealcoholized double-component sealant, which comprises the following steps:
a) uniformly mixing hydroxyl-terminated polydimethylsiloxane and solid filler to obtain a component A;
b) stirring the crosslinking agent, the tackifier and the catalyst under vacuum to be uniform to obtain a component B;
c) mixing the component A obtained in the step a) with the component B obtained in the step B) to obtain dealcoholized bi-component sealant;
the step a) and the step b) are not limited in order.
Preferably, the rotation speed of the stirring in the step b) is 20r/min to 40r/min, the temperature is 10 ℃ to 69 ℃, and the time is 20min to 60 min.
The invention provides dealcoholized double-component sealant which comprises the following components in percentage by mass of 100: (2-20) a component A and a component B; the component A comprises: 100 parts by weight of hydroxyl-terminated polydimethylsiloxane; 5-150 parts by weight of solid filler; the component B comprises: 8-35 parts of a crosslinking agent; 1-20 parts by weight of tackifier; 0.1 to 1 portion of catalyst; the crosslinking agent has the general formula: (R)1O)3-aR2 aSi-R3-SiR4 b(OR5)3-b(ii) a Wherein R is1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1; the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a Si-N bond compound. Compared with the prior artCompared with the prior art, the dealcoholized double-component sealant provided by the invention adopts specific components, realizes better interaction, has good bonding performance, durability, sealing performance and long-term storage stability, and is suitable for sealing photovoltaic components, automobile components, electronic and electric appliances, glass for buildings, curtain wall components and the like.
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides dealcoholized double-component sealant which comprises the following components in percentage by mass of 100: (2-20) a component A and a component B;
the component A comprises:
100 parts by weight of hydroxyl-terminated polydimethylsiloxane;
5-150 parts by weight of solid filler;
the component B comprises:
8-35 parts of a crosslinking agent;
1-20 parts by weight of tackifier;
0.1 to 1 portion of catalyst;
the crosslinking agent has a general formula shown in formula (I):
(R1O)3-aR2 aSi-R3-SiR4 b(OR5)3-bformula (I)
In the formula (I), R1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1;
the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a Si-N bond compound.
In the invention, the dealcoholized double-component sealant comprises the following components in percentage by mass of 100: (2-20) the A component and the B component are preferably 100: (2.5-10).
In the present invention, the a component includes a hydroxyl terminated polydimethylsiloxane and a solid filler. In the present invention, the hydroxyl-terminated polydimethylsiloxane preferably has a general formula shown in formula (II):
HO-(SiMe2O)nSiMe2OH formula (II);
in the formula (II), n is 25 ℃ so that the kinematic viscosity of the hydroxyl-terminated polydimethylsiloxane is 200mm2/s～1000000mm2In a preferred embodiment of the invention, the hydroxyl-terminated polydimethylsiloxane is α, omega-dihydroxypolydimethylsiloxane, and the α, omega-dihydroxypolydimethylsiloxane preferably has a viscosity of 200mm2/s～1000000mm2S, more preferably 500mm2/s～100000mm2S, more preferably 1000mm2/s～80000mm2And s. The source of the hydroxyl-terminated polydimethylsiloxane is not particularly limited in the present invention, and may be any commercially available product known to those skilled in the art or a self-product prepared according to a preparation method known to those skilled in the art. In the present invention, the a component includes 100 parts by weight of hydroxyl-terminated polydimethylsiloxane.
In the invention, the hydroxyl-terminated polydimethylsiloxane is used as a basic sizing material, in the preferred embodiment of the invention, α -hydroxyl-omega-trimethylsilyl-terminated polydimethylsiloxane is added to the basic sizing material to achieve the purposes of low modulus, low hardness, high elongation and reduction of free silicone oil of the sizing material, in the invention, the kinematic viscosity of α -hydroxyl-omega-trimethylsilyl-terminated polydimethylsiloxane is preferably 100mm2/s～100000mm2S, more preferably 1000mm2/s～50000mm2The source of the α -hydroxy-omega-trimethylsilyl terminated polydimethylsilane is not particularly limited in this invention, and those skilled in the art will be familiar withThe addition amount of α -hydroxy-omega-trimethylsilyl terminated polydimethylsiloxane in the base rubber material is preferably 0-150 parts by weight.
In the present invention, the solid filler preferably includes one or more of calcium carbonate, white carbon, quartz powder, hollow glass microspheres, diatomaceous earth, titanium dioxide, aluminum hydroxide, alumina, zinc oxide, magnesium oxide, zinc oxide, and zinc carbonate, and more preferably one or more of calcium carbonate, white carbon, and quartz powder. The source of the solid filler in the present invention is not particularly limited, and commercially available products or self-products known to those skilled in the art may be used. In the present invention, the a component includes 5 to 150 parts by weight of a solid filler, preferably 40 to 140 parts by weight.
In the present invention, the calcium carbonate is preferably selected from one or more of nano calcium carbonate, light calcium carbonate and heavy calcium carbonate, and more preferably nano calcium carbonate. In a preferred embodiment of the invention, the calcium carbonate is nano calcium carbonate, and the BET specific surface area of the nano calcium carbonate is 25m2/g～60m2(ii)/g; the nano calcium carbonate is adopted in the invention, so that the nano calcium carbonate is beneficial to the dispersion in the component A, and the reinforcing effect is provided. The calcium carbonate is preferably subjected to fatty acid surface treatment, so that the dispersibility of the calcium carbonate in the component A can be improved; the amount of the fatty acid surface-treated is 3 to 10 parts by weight based on 100 parts by weight of the solid filler.
In the present invention, the white carbon black is preferably selected from fumed white carbon black and/or precipitated white carbon black, and more preferably fumed white carbon black. In the present invention, the white carbon black is preferably subjected to surface treatment with hexamethylsilazane, dimethoxydimethylsilane, dimethyldichlorosilane or a siloxane oligomer.
In addition, the invention can also add additives widely applied in silicon rubber on the premise of not influencing the performance of products; inorganic additives other than the solid filler described in the above technical means, antifungal agents, flame retardants (optionally platinum compound, zinc carbonate powder, etc.), heat-resistant agents (optionally iron oxide, oxygen)Cerium oxide, etc.), plasticizers, thickeners, water, etc. In a preferred embodiment of the present invention, the component a further comprises 0 to 30 parts by weight of a plasticizer, preferably 5 to 20 parts by weight; the plasticizer is preferably dimethyl silicone oil; the kinematic viscosity of the dimethyl silicone oil is preferably 50mm2/s～12000mm2S, more preferably 100mm2/s～5000mm2And s. In a preferred embodiment of the present invention, the component a further comprises 0 to 10 parts by weight of water, preferably 0.1 to 1 part by weight.
In the present invention, the B component includes a crosslinking agent, a tackifier and a catalyst. In the present invention, the crosslinking agent has a general formula represented by formula (I):
(R1O)3-aR2 aSi-R3-SiR4 b(OR5)3-bformula (I)
In the formula (I), R1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1; the crosslinking agent is an organic compound which contains at least two alkoxy functional groups in a molecule and does not contain a siloxane bond between silicon atom groups, preferably one or more of 1, 6-bis (trimethoxysilyl) hexane, 1, 6-bis (triethoxysilyl) hexane, 1, 2-bis (trimethoxysilyl) ethane and 1, 2-bis (triethoxysilyl) ethane, more preferably 1, 2-bis (trimethoxysilyl) ethane or 1, 6-bis (trimethoxysilyl) hexane. The source of the crosslinking agent is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art may be used. In the present invention, the B component includes 8 to 35 parts by weight of a crosslinking agent, preferably 10 to 33 parts by weight.
In addition, in the present invention, in addition to the above-mentioned crosslinking agent, one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, isopropyltrimethoxysilane, isopropyltriethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane, methyl orthosilicate, ethyl orthosilicate, which are well known to those skilled in the art, may be preferably added to adjust the crosslinking density, the curing speed, and the like, and the present invention is not particularly limited thereto.
In the invention, the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a Si-N bond compound. In the present invention, the amino coupling agent preferably includes one or more of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane, gamma-aminoethylaminopropyltriethoxysilane, bis [3- (triethoxysilyl) propyl ] amine, bis (3-trimethoxysilylpropyl) amine, bis [3- (trimethoxysilyl) propyl ] ethylenediamine and bis [3- (triethoxysilyl) propyl ] ethylenediamine, more preferably aminopropyltrimethoxysilane. The source of the amino coupling agent is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art may be used.
In the present invention, the epoxy-based coupling agent preferably includes one or more of gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma-glycidoxypropylmethyldiethoxysilane, gamma-glycidoxypropylmethyldimethoxysilane and β - (3, 4-epoxycyclohexane) ethyltrimethoxysilane, and more preferably gamma-glycidoxypropyltrimethoxysilane.
In the present invention, the Si-N bond compound preferably includes 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane, 2-methoxy-2, 4-dimethyl-1-aza-2-silacyclopentane-1-ethylamine, 2-diethoxy-1-aza-2-silacyclopentane, [1- (3-triethoxysilyl) propyl ] -2, 2-diethoxy-1-aza-2-silacyclopentane, aza- (2-aminoethyl) -2,2, 4-trimethyl-1-aza-2-silacyclopentane, 2-dimethoxy-1-aza-2-silacyclopentane -ethylamine, N-trimethylsilyl-3-aminopropyltrimethoxysilane and N-trimethylsilyl-3-aminopropyltriethoxysilane, more preferably 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane or N-trimethylsilyl-3-aminopropyltrimethoxysilane. The source of the Si-N bond compound is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art may be used. The invention adopts Si-N bond compound, the molecule at least contains one or more Si-N bonds, and the nitrogen atom is linked to the silicon atom containing more than one alkoxy by the carbon chain of more than one carbon atom, thus obviously improving the performance of the tackifier.
In the present invention, the preparation method of the tackifier is preferably as follows:
mixing a mixture of 1: 2: (0.2-3) mixing the amino coupling agent, the epoxy coupling agent and the Si-N bond compound, and reacting at 20-60 ℃ for 48-120 h to obtain the tackifier;
more preferably:
mixing a mixture of 1: 2: and (0.5-1) mixing the amino coupling agent, the epoxy coupling agent and the Si-N bond compound, and reacting at 50 ℃ for 110 hours to obtain the tackifier.
In the present invention, the B component includes 1 to 20 parts by weight of a tackifier, preferably 3 to 10 parts by weight.
In addition, other coupling agents known to those skilled in the art, such as α, omega-trimethylsiloxy polydimethylsiloxane, aminopropyltrimethoxysilane, aminopropyltriethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane, bis [3- (triethoxysilyl) propyl ] amine, bis (3-trimethoxysilylpropyl) amine, bis [3- (trimethoxysilyl) propyl ] ethylenediamine, bis [3- (triethoxysilyl) propyl ] ethylenediamine, gamma-methacryloxypropyltrimethoxysilane and gamma-glycidoxypropyltrimethoxysilane, may be preferably added in an amount of 0 to 10 parts by weight, more preferably 3 to 5 parts by weight, to make the product more suitable for sealing different types of products, without impairing the properties of the target product.
In the present invention, the catalyst preferably includes one or more of dibutyltin dilaurate, dioctyltin dilaurate, dimethyltin dioctanoate and dibutyltin diacetate, more preferably dibutyltin dilaurate or dimethyltin dioctanoate. The source of the catalyst in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used. In the present invention, the B component includes 0.1 to 1 part by weight of the catalyst, preferably 0.2 to 0.5 part by weight.
In the present invention, the B component preferably further comprises:
0 to 100 parts by weight of white carbon black, more preferably 5 to 20 parts by weight. In the present invention, the white carbon black is preferably selected from fumed white carbon black and/or precipitated white carbon black, and more preferably fumed white carbon black. In the present invention, the silica preferably has a specific surface area of 150m2/g～200m2/g。
In the present invention, the B component preferably further comprises:
the color paste is 0 to 100 parts by weight, and more preferably 20 to 61 parts by weight. In the invention, the color paste plays a role of color mixing, and a person skilled in the art can select the color of the color paste according to the actual use requirement, such as a black color paste, a white color paste and a silver color paste; in a preferred embodiment of the invention, the color paste is a black color paste. The source of the color paste is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art can be used. In addition, the invention can also be used for color matching by directly adding color paste raw materials such as carbon black. In a preferred embodiment of the present invention, the B component further comprises 10 parts by weight of carbon black.
In the invention, the component A and the component B are uniformly mixed according to the specific proportion, and a condensation type crosslinking reaction can occur to vulcanize the components into a rubber elastomer; the dealcoholized double-component sealant provided by the invention adopts components with specific content, realizes better interaction, and ensures that the product has excellent adhesion and bonding durability to various substrates, in particular to various solar photovoltaic components such as photovoltaic cell glass, aluminum frame, back plate and junction box, various plastics of automobile lamp components for automobiles, pot seal of LED display screen modules, glass for buildings, curtain wall components and the like, and has waterproof and moistureproof performances and long-term storage stability.
The invention also provides a preparation method of the dealcoholized double-component sealant, which comprises the following steps:
a) uniformly mixing hydroxyl-terminated polydimethylsiloxane and solid filler to obtain a component A;
b) stirring the crosslinking agent, the tackifier and the catalyst under vacuum to be uniform to obtain a component B;
c) mixing the component A obtained in the step a) with the component B obtained in the step B) to obtain dealcoholized bi-component sealant;
the step a) and the step b) are not limited in order.
The invention firstly mixes the hydroxyl end-capping polydimethylsiloxane and the solid filler evenly to obtain the component A. In the present invention, the radical-terminated polydimethylsiloxane and the solid filler are the same as those described in the above technical solution, and are not described herein again.
The mixing method is not particularly limited in the present invention, and any technical scheme of manual stirring or mechanical stirring known to those skilled in the art can be adopted. The temperature and time for mixing are not particularly limited in the present invention, and if the temperature is less than 100 ℃ and the time is 2-4 hours, which are well known to those skilled in the art, the uniform mixing can be ensured. In a preferred embodiment of the present invention, the component a further includes other raw materials described in the above technical scheme, and the components are mixed to be uniform by adopting the manner described in the above step a).
Meanwhile, the crosslinking agent, the tackifier and the catalyst are stirred to be uniform under vacuum to obtain the component B. In the present invention, the crosslinking agent, the tackifier and the catalyst are the same as those described in the above technical solution, and are not described herein again.
In the present invention, the pressure of the vacuum is preferably-0.09 MPa to-0.1 MPa. In the invention, the rotating speed of the stirring is preferably 20 r/min-40 r/min, and more preferably 25 r/min-30 r/min; the stirring temperature is preferably 10-69 ℃, and more preferably 20-40 ℃; the stirring time is preferably 20min to 60min, and more preferably 30min to 40 min.
In a preferred embodiment of the present invention, the component B further comprises other raw materials described in the above technical scheme, and the mixture is stirred to be uniform in the manner described in the above step B).
In the present invention, after the stirring to be uniform, it is preferable to further include:
and (4) carrying out vacuum defoaming treatment on the obtained mixture to obtain a component B.
After the component A and the component B are obtained, the component A and the component B are mixed to obtain the dealcoholized double-component sealant.
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
The invention provides dealcoholized double-component sealant which comprises the following components in percentage by mass of 100: (2-20) a component A and a component B; the component A comprises: 100 parts by weight of hydroxyl-terminated polydimethylsiloxane; 5-150 parts by weight of solid filler; the component B comprises: 8-35 parts of a crosslinking agent; 1-20 parts by weight of tackifier; 0.1 to 1 portion of catalyst; the crosslinking agent has the general formula: (R)1O)3-aR2 aSi-R3-SiR4 b(OR5)3-b(ii) a Wherein R is1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1; the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a Si-N bond compound. Compared with the prior art, the dealcoholized double-component sealant provided by the invention adopts components with specific content, realizes better interaction, has good bonding performance, durability, sealing performance and long-term storage stability, and is suitable for sealing photovoltaic components, automobile components, electronic and electric appliances, glass for buildings, curtain wall components and the like.
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available products or self-products; the preparation method of the black color paste comprises the following steps: mixing silicone oil and carbon black according to a weight ratio of 3: 1, mixing, and stirring and dispersing at high speed for 3-4 h under the conditions that the temperature is 100-150 ℃ and the vacuum dehydration pressure is-0.09-0.1 MPa to obtain the black color paste.
Example 1
(1) The component A comprises: the kinematic viscosity is 20000mm2α, omega-dihydroxy dimethyl silicone polymer of 100 weight portions, nanometer calcium carbonate treated by fatty acid of 100 weight portions, specific surface area of 150m25 parts by weight of fumed silica/g and kinematic viscosity of 350mm25 parts by weight of dimethyl silicone oil/s are mixed and stirred uniformly to obtain the component A of the dealcoholized bi-component sealant.
(2) And B component: firstly, 20 parts by weight of black color paste and 13 parts by weight of 1, 2-bis trimethoxysilyl ethane are mixed, stirred for 10-20 min and added with the specific surface area of 150m210 parts by weight of fumed silica per gram, dispersing at high speed for 30-40 min until the fumed silica is uniformly dispersed, then adding 3 parts by weight of tackifier (prepared by mixing aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane in a molar ratio of 1: 2: 0.5 and reacting for 110h at 50 ℃) and 0.5 part by weight of catalyst (dibutyltin dilaurate) under the pressure
Stirring the mixture for 30 to 40min at the temperature of between 20 and 40 ℃ in a vacuum state of between-0.09 and-0.1 MPa at the rotating speed of 25r/min until the mixture is uniform, thereby obtaining a component B of the dealcoholized bi-component sealant.
(3) Mixing the component A and the component B in a ratio of 100: 10 to obtain the dealcoholized bi-component sealant.
Example 2
(1) Component A comprising α omega-dihydroxy polydimethylsiloxane (kinematic viscosity of 20000 mm)2α, [ omega ] -dihydroxypolydimethylsiloxane,/s and a kinematic viscosity of 80000mm2α of/s, mixed according to the mass ratio of 1: 1) 100 parts by weight, 100 parts by weight of nano calcium carbonate treated by fatty acid and 350mm of kinematic viscosity2And 10 parts by weight of dimethyl silicone oil/s are mixed and stirred uniformly to obtain the component A of the dealcoholized bi-component sealant.
(2) And B component: firstly, 61 parts by weight of black color paste and 33 parts by weight of 1, 6-bis (trimethoxysilyl) hexane are mixed, stirred for 10-20 min, dispersing at high speed for 30-40 min until the dispersion is uniform, then adding 6 parts by weight of tackifier (prepared by mixing aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane in a molar ratio of 1: 2: 1 and reacting for 110h at 50 ℃), 3 parts by weight of gamma-aminoethylaminopropyltrimethoxysilane and 0.2 part by weight of catalyst (dimethyltin dioctanodecanoate), stirring the mixture for 30 to 40min to be uniform under the vacuum state with the pressure of-0.09 to-0.1 MPa and the rotating speed of 25r/min at the temperature of 20 to 40 ℃ to obtain the component B of the dealcoholized bi-component sealant (bonding type to the building base material).
(3) Mixing the component A and the component B in a ratio of 120: 10 to obtain the dealcoholized bi-component sealant.
Example 3
(1) The component A comprises: the kinematic viscosity is 5000mm2α parts by weight of omega-dihydroxy polydimethylsiloxane, 100 parts by weight of nano calcium carbonate treated by fatty acid and 40 parts by weight of heavy calcium carbonate without fatty acid treatment are mixed and stirred uniformly to obtain the component A of the dealcoholized two-component sealant.
(2) And B component: firstly, the kinematic viscosity is 5000mm2α parts by weight of omega-trimethylsiloxy polydimethylsiloxane, 10 parts by weight of carbon black and 30 parts by weight of 1, 6-bis (trimethoxysilyl) hexane are mixed, stirred for 10-20 min, dispersed at high speed for 30-40 min until the mixture is uniformly dispersed, 10 parts by weight of tackifier (prepared by mixing aminopropyltrimethoxysilane, gamma-glycidyl ether oxypropyltrimethoxysilane and 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane in a molar ratio of 1: 2: 1, and reacting for 110h at 50 ℃) and 5 parts by weight of gamma-aminoethylaminopropyltrimethoxysilane and 0.1 part by weight of catalyst (dioctadecanoic acid dimethyltin) are added, and the mixture is stirred for 30-40 min at a vacuum state with a pressure of-0.09 to-0.1 MPa and a rotating speed of 25r/min and at a temperature of 20-40 ℃ until the mixture is uniform, so as to obtain a component B of the dealcoholized sealant.
(3) Mixing the component A and the component B in a ratio of 100: 10 to obtain the dealcoholized bi-component sealant.
Example 4
(1) The component A comprises: the kinematic viscosity is 3000mm2α, 100 parts by weight of omega-dihydroxy polydimethylsiloxane,/s, 40 parts by weight of quartz powder, kinematic viscosity 350mm220 parts by weight of dimethyl silicone oil/s and 0.2 part by weight of water are mixed until being uniformly stirred, and the component A of the dealcoholized bi-component sealant is obtained.
(2) And B component: adding 6.5 parts by weight of a tackifier (prepared by mixing aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N-trimethylsilyl-3-aminopropyltriethoxysilane in a molar ratio of 1: 2: 0.5 and reacting for 110 hours at 50 ℃) into 10 parts by weight of 1, 6-bis (trimethoxysilyl) hexane, 3.5 parts by weight of gamma-aminoethylaminopropyltrimethoxysilane and 0.5 part by weight of a catalyst (dimethyl tin dioctanodecanoate), and stirring uniformly at 20-40 ℃ for 30-40 minutes under a vacuum state with a pressure of-0.09 to-0.1 MPa and a rotating speed of 30r/min to obtain a component B of the dealcoholized bi-component sealant (bonding to a photovoltaic rubber substrate).
(3) Mixing the component A and the component B in a ratio of 40: 1 to obtain the dealcoholized bi-component sealant.
Comparative example 1
(1) The component A comprises: the kinematic viscosity is 20000mm2α, omega-dihydroxy dimethyl silicone polymer of 100 weight portions, nanometer calcium carbonate treated by fatty acid of 100 weight portions, specific surface area of 150m25 parts by weight of fumed silica/g and kinematic viscosity of 350mm25 parts by weight of dimethyl silicone oil/s are mixed and stirred uniformly to obtain the component A of the dealcoholized bi-component sealant.
(2) And B component: firstly, 20 parts by weight of black color paste and 13 parts by weight of 1, 2-bis trimethoxysilyl ethane are mixed, stirred for 10-20 min and added with the specific surface area of 150m210 parts by weight of fumed silica per gram, dispersing at high speed for 30-40 min until the fumed silica is uniformly dispersed, adding 0.5 part by weight of catalyst (dibutyltin dilaurate), and stirring at 20-40 ℃ and at the vacuum state with the pressure of-0.09 to-0.1 MPa and the rotating speed of 25r/minAnd (3) homogenizing for 0min to obtain the component B of the dealcoholized bi-component sealant.
(3) Mixing the component A and the component B in a ratio of 100: 10 to obtain the dealcoholized bi-component sealant.
Comparative example 2
(1) Component A comprising α omega-dihydroxy polydimethylsiloxane (kinematic viscosity of 20000 mm)2α, [ omega ] -dihydroxypolydimethylsiloxane,/s and a kinematic viscosity of 80000mm2α of/s, mixed according to the mass ratio of 1: 1) 100 parts by weight, 100 parts by weight of nano calcium carbonate treated by fatty acid and 350mm of kinematic viscosity2And 10 parts by weight of dimethyl silicone oil/s are mixed and stirred uniformly to obtain the component A of the dealcoholized bi-component sealant.
(2) And B component: firstly, 61 parts by weight of black color paste and 33 parts by weight of methyl triethoxysilane oligomer are mixed, after stirring for 10-20 min, the mixture is dispersed at a high speed for 30-40 min until the mixture is uniformly dispersed, then 6 parts by weight of tackifier (aminopropyltrimethoxysilane) and 0.2 part by weight of catalyst (dioctyl decanoic acid dimethyl tin) are added, and the mixture is stirred for 30-40 min until the mixture is uniformly dispersed under the vacuum state with the pressure of-0.09 to-0.1 MPa and the rotating speed of 25r/min at the temperature of 20-40 ℃, so that the component B of the dealcoholized double-component sealant (bonding type to building base materials) is obtained.
(3) Mixing the component A and the component B in a ratio of 120: 10 to obtain the dealcoholized bi-component sealant.
Comparative example 3
(1) The component A comprises: the kinematic viscosity is 3000mm2α, [ omega ] -dihydroxy polydimethylsiloxane, [ 40 parts by weight of quartz powder, [ 350 ] kinematic viscosity220 parts by weight of dimethyl silicone oil/s and 0.2 part by weight of water are mixed until being uniformly stirred, and the component A of the dealcoholized bi-component sealant is obtained.
(2) And B component: 10 parts by weight of ethyl orthosilicate oligomer, 10 parts by weight of gamma-aminoethyl aminopropyltrimethoxysilane and 0.5 part by weight of catalyst (dioctyl decanoate dimethyl tin) are stirred for 30-40 min to be uniform under the vacuum state with the pressure of-0.09 to-0.1 MPa and the rotating speed of 25r/min at the temperature of 20-40 ℃, and the component B of the dealcoholization type bi-component sealant (bonding to a photovoltaic rubber substrate) is obtained.
(3) Mixing the component A and the component B in a ratio of 40: 1 to obtain the dealcoholized bi-component sealant.
The curing performance, initial adhesion, adhesion durability and reversion resistance of the dealcoholized two-component sealant provided in examples 1 to 4 and comparative examples 1 to 3 were tested by the following specific methods:
the viscosity was measured at 25 degrees.
Initial adhesion: extruding dealcoholized double-component sealant on the surfaces of glass plate, metal plate (aluminum, stainless steel, copper plate) and plastic plate (vinyl chloride resin, PC, PMC, etc.) to form threads, curing at 25 deg.C and 50% humidity, and standing for 3 days; then, pulling the colloid from one end of the solidified colloid by hand to strip the substrate, and measuring the adhesiveness; the measurement results are expressed by the following methods:
○ seal (organic silica gel fracture 100%);
△ printing that a part of the organic silicon colloid layer and the interface of the substrate are peeled off (the agglutination destruction rate is 50-99%);
and (4) printing: the interface between the silicone gel layer and the substrate is mostly peeled off (the cohesive failure rate is 0-49%).
Bonding durability: extruding dealcoholized double-component sealant on the surfaces of glass plate, metal plate (aluminum, stainless steel, copper plate) and plastic plate (vinyl chloride resin, PC, PMC, etc.) to form threads, curing at 25 deg.C and 50% humidity, and standing for 3 days; then placing the test body in water with the temperature of 25 ℃ and placing for 3 days; then taking out the test body from the water, pulling the test body from one end of the solidified colloid by hand to peel the colloid from the substrate, and measuring the adhesiveness; the measurement results are expressed by the following methods:
○ seal (organic silica gel fracture 100%);
△ printing that a part of the organic silicon colloid layer and the interface of the substrate are peeled off (the agglutination destruction rate is 50-99%);
and (4) printing: the interface between the silicone gel layer and the substrate is mostly peeled off (the cohesive failure rate is 0-49%).
Sulfuration resistance and reversion resistance: uniformly mixing the component A and the component B, filling the mixture into a 20mL plastic container to the height of 2cm, and standing for 24 hours at the temperature of 25 ℃ and the humidity of 50% for curing; then covering the cover, and placing the container for a week at the temperature of 85 ℃ and the humidity of 85%; cooling to room temperature, and carrying out hardness test according to GB/T528-; the measured hardness values were zero and marked as poor, except for good.
Through tests, the curing performance, initial adhesion, adhesion durability and anti-reversion resistance data of the dealcoholized two-component sealant provided in the examples 1 to 4 and the comparative examples 1 to 3 are shown in tables 1 to 2.
TABLE 1 curing Performance and initial adhesion data for the dealcoholized two-component sealants provided in examples 1-4 and comparative examples 1-3
Table 2 data on the adhesion durability and resistance to reversion of dealcoholized two-component sealants, provided in examples 1-4 and comparative examples 1-3
As can be seen from tables 1 to 2, the dealcoholized silicone rubber sealants provided in embodiments 1 to 4 of the present invention have good greenhouse curing performance and long-term storage stability, and are excellent in adhesion and good in adhesion durability; after being cured, the epoxy resin has good cohesiveness to metals such as stainless steel, aluminum, copper, aluminum oxide and the like, various plastics such as PC/PP and the like, ceramics, glass and other materials, and can be used for sealing photovoltaic modules, buildings, automobiles, electronic appliances and the like.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A dealcoholized two-component sealant comprises the following components in percentage by mass of 100: (2-20) a component A and a component B;
the component A comprises:
100 parts by weight of hydroxyl-terminated polydimethylsiloxane;
5-150 parts by weight of solid filler;
the component B comprises:
8-35 parts of a crosslinking agent;
1-20 parts by weight of tackifier;
0.1 to 1 portion of catalyst;
the crosslinking agent has a general formula shown in formula (I):
(R1O)3-aR2 aSi-R3-SiR4 b(OR5)3-bformula (I);
in the formula (I), R1、R2、R4、R5Independently selected from monovalent hydrocarbon radicals; r3Is a divalent hydrocarbon group with 2-20 carbon atoms; a is 0 or 1, b is 0 or 1;
the tackifier is prepared from an amino coupling agent, an epoxy coupling agent and a Si-N bond compound; the Si-N bond compound is 2, 2-diethoxy-1- (trimethylsilyl) -1-aza-2-silacyclopentane or N-trimethylsilyl-3-aminopropyltriethoxysilane.
2. The dealcoholized two-component sealant according to claim 1, wherein the hydroxyl terminated polydimethylsiloxane has the general formula of formula (II):
HO-(SiMe2O)nSiMe2OH formula (II);
in the formula (II), n is 25 ℃ so that the kinematic viscosity of the hydroxyl-terminated polydimethylsiloxane is 200mm2/s～1000000mm2Positive number in/s.
3. The dealcoholized two-component sealant according to claim 1, wherein the solid filler comprises one or more of calcium carbonate, white carbon, quartz powder, hollow glass microspheres, diatomaceous earth, titanium dioxide, aluminum hydroxide, aluminum oxide, zinc oxide, magnesium oxide, zinc oxide, and zinc carbonate.
4. The dealcoholized two-component sealant according to claim 1, wherein the tackifier is prepared by a method comprising the following steps:
mixing a mixture of 1: 2: (0.2-3) mixing the amino coupling agent, the epoxy coupling agent and the Si-N bond compound, and reacting at 20-60 ℃ for 48-120 h to obtain the tackifier.
5. The dealcoholized two-component sealant according to claim 1, wherein the amino coupling agent comprises one or more of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane, gamma-aminoethylaminopropyltriethoxysilane, bis [3- (triethoxysilyl) propyl ] amine, bis (3-trimethoxysilylpropyl) amine, bis [3- (trimethoxysilyl) propyl ] ethylenediamine and bis [3- (triethoxysilyl) propyl ] ethylenediamine.
6. The dealcoholized two-component sealant according to claim 1, wherein the epoxy-based coupling agent comprises one or more of gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, gamma-glycidoxypropylmethyldiethoxysilane, gamma-glycidoxypropylmethyldimethoxysilane, and β - (3, 4-epoxycyclohexane) ethyltrimethoxysilane.
7. The dealcoholized two-component sealant according to claim 1, wherein the catalyst comprises one or more of dibutyltin dilaurate, dioctyltin dilaurate, dimethyltin dioctanodecanoate and dibutyltin diacetate.
8. A method of preparing a dealcoholized two component sealant according to any one of claims 1 to 7, comprising the steps of:
a) uniformly mixing hydroxyl-terminated polydimethylsiloxane and solid filler to obtain a component A;
b) stirring the crosslinking agent, the tackifier and the catalyst under vacuum to be uniform to obtain a component B;
c) mixing the component A obtained in the step a) with the component B obtained in the step B) to obtain dealcoholized bi-component sealant;
the step a) and the step b) are not limited in order.
9. The preparation method according to claim 8, wherein the stirring in step b) is performed at a rotation speed of 20r/min to 40r/min, at a temperature of 10 ℃ to 69 ℃ and for a time of 20min to 60 min.
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| CN110982272A (en) * | 2019-12-28 | 2020-04-10 | 深圳市旗盛科技有限公司 | A fill colloid for precious internal battery that charges is fixed |
| CA3166152A1 (en) * | 2020-02-03 | 2021-08-12 | Michael Schlumpf | Fast curing two-component silicone composition having adjustable pot life |
| CN111394052B (en) * | 2020-05-27 | 2022-04-26 | 绵阳惠利电子材料有限公司 | Dealcoholized condensed type double-component room temperature vulcanized silicone rubber and preparation method thereof |
| CN112662370B (en) * | 2020-12-16 | 2022-10-28 | 江西晨光新材料股份有限公司 | Single-component dealcoholized silicone sealant and preparation method thereof |
| CN113717684A (en) * | 2021-09-23 | 2021-11-30 | 广州以恒有机硅有限公司 | Low-modulus silicone weather-resistant sealant and preparation method thereof |
| CN114031314A (en) * | 2021-11-16 | 2022-02-11 | 华中光电技术研究所（中国船舶重工集团公司第七一七研究所） | Ultrahigh vacuum non-magnetic sealing method for quartz glass metal |
| CN114507504B (en) * | 2022-01-14 | 2023-12-29 | 杭州之江有机硅化工有限公司 | Low-modulus high-elongation single-component organic silicon sealant and application thereof |
| CN114507503B (en) * | 2022-01-14 | 2024-01-26 | 杭州之江有机硅化工有限公司 | Low-modulus high-elongation two-component organic silicon sealant and application thereof |
| CN115322572B (en) * | 2022-08-11 | 2023-06-13 | 深圳市泰科科技有限公司 | Flame-retardant fireproof silicone rubber material for cables and preparation method thereof |
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