CN110591638B - Low-proportion bi-component dealcoholized organosilicon sealant and preparation method and application thereof - Google Patents

Low-proportion bi-component dealcoholized organosilicon sealant and preparation method and application thereof Download PDF

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CN110591638B
CN110591638B CN201911068139.9A CN201911068139A CN110591638B CN 110591638 B CN110591638 B CN 110591638B CN 201911068139 A CN201911068139 A CN 201911068139A CN 110591638 B CN110591638 B CN 110591638B
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蔡琴
李军明
陈健
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Zhenjiang Laibo New Material Technology Co ltd
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Zhenjiang Boshen New Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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 discloses a low-proportion bi-component dealcoholized organosilicon sealant and a preparation method and application thereof, wherein the sealant comprises a component A and a component B, and the component A comprises the following components in parts by weight: 35-60 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane, 35-65 parts of reinforcing filler and 0-10 parts of methyl-terminated polydimethylsiloxane; the component B comprises the following components in parts by weight: 35-60 parts of alkoxy end-capped polymer, 35-65 parts of reinforcing filler, 4-10 parts of cross-linking agent, 0.1-5 parts of coupling agent and 0.1-5 parts of organic tin catalyst. The low-proportion bi-component dealcoholized organosilicon sealant prepared by the invention is insensitive to the mixing proportion, and reduces the problems of no curing or poor bonding and the like caused by the error of the mixing proportion. The low-proportion bi-component dealcoholized organosilicon sealant can be widely used for sealing an aluminum frame of a solar photovoltaic module, bonding a junction box and a back plate and assembling electronic components.

Description

Low-proportion bi-component dealcoholized organosilicon sealant and preparation method and application thereof
Technical Field
The invention belongs to the technical field of dealcoholized room temperature vulcanized silicone rubber, and particularly relates to a low-proportion bi-component dealcoholized organosilicon sealant as well as a preparation method and application thereof.
Background
The curing speed of the single-component room temperature vulcanized silicone rubber is limited by moisture in the air, while the component of the two-component dealcoholized organosilicon sealant is divided into two components which can be mixed in proportion for curing reaction, so that the sealant has the advantages of fast deep curing, wide application temperature range, water resistance, moisture resistance, ozone resistance, weather resistance, high insulating strength, low dielectric loss, electric arc resistance, corona resistance and the like, and is widely applied to sealing of aluminum frames of solar photovoltaic components, bonding of junction boxes and back plates, assembling of electronic components and the like.
The patent No. CN 109135660A discloses a dealcoholized double-component sealant and a preparation method thereof, wherein the published mixing mass ratio of A to B is 100 to (2-20), the mixing ratio has high requirement on weighing precision, and if the mixing ratio is deviated, the mechanical property and the bonding strength of the sealant after curing are obviously reduced, even the sealant is not cured.
Patent No. CN 107868469A discloses a water-resistant ultraviolet bonding dealcoholization type bi-component room temperature vulcanized silicone rubber and a preparation method thereof, wherein a plasticizer of a component B is vinyl-terminated polydimethylsiloxane, methyl polydimethylsiloxane and hydroxyl-terminated polydimethylsiloxane, and the plasticizer is selected, so that the component B is easy to thicken, absorb oil or crystallize and directly solidify in the storage process, and the product cannot be normally used or the solidification and bonding are ineffective.
Therefore, products in the prior art are sensitive to mixing ratio, poor in curing or bonding and the like due to errors of the mixing ratio, poor in mechanical property after curing, low in deep curing speed, low in substrate bonding speed, poor in durability and poor in storage stability.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a low-proportion bi-component dealcoholized organosilicon sealant.
The invention also aims to solve the technical problem of providing a preparation method of the low-proportion bi-component dealcoholized organosilicon sealant.
The invention finally solves the technical problem by applying the low-proportion bi-component dealcoholized organosilicon sealant.
The low-proportion bi-component dealcoholized organosilicon sealant provided by the invention has the mixing mass ratio of A to B of 100 to (80-120), is insensitive to the mixing proportion, reduces the problems of poor curing or bonding and the like caused by mixing proportion errors, and has the advantages of good mechanical property after curing, high deep curing speed, high adhesion speed to a base material, good durability and stable storage. The low-proportion bi-component dealcoholized organosilicon sealant can be widely used for sealing an aluminum frame of a solar photovoltaic module, bonding a junction box and a back plate, assembling electronic components and the like.
The technical scheme is as follows: in order to solve the technical problems, the invention provides a low-proportion two-component dealcoholized organosilicon sealant which is prepared from the following components in parts by weight: the component A comprises: 35-60 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane, 35-65 parts of reinforcing filler and 0-10 parts of methyl-terminated polydimethylsiloxane; the component B comprises 30-60 parts of alkoxy end-capped polymer, 35-65 parts of reinforcing filler, 4-10 parts of cross-linking agent, 0.1-5 parts of coupling agent and 0.1-5 parts of organic tin catalyst.
In order to keep the proper construction performance of the product before curing, facilitate sizing and keep the good toughness of the cured product, the viscosity of the alpha, omega-hydroxyl-terminated polydimethylsiloxane is 1500-80000 mpa.s, and more preferably 20000-80000 mpa.s.
In order to ensure the performance retention rate of the product after aging, the viscosity of the terminal methyl polydimethylsiloxane is 50-1000 mpa.s
In order to ensure that a certain mechanical property of the product is maintained after the product is cured, A, B components of the reinforcing filler are one or more of nano calcium carbonate, silica powder, modified silica powder, titanium dioxide and aluminum hydroxide, and more preferably, the reinforcing filler is reinforced by the nano calcium carbonate and the silica powder, and the viscosity is reduced while the reinforcing filler is reinforced by the modified silica powder.
Wherein, in order to ensure the viscosity of the product, have thixotropy and are beneficial to extrusion, the specific surface area of the nano calcium carbonate is less than 60m2A more preferable range is 18 to 20 m/g2Per g, good reinforcing effect and favorable dispersion.
The specific surface area of the silicon micro powder and the modified silicon micro powder is 1-10 mu m, more preferably 3-5 mu m, the strength is improved, the viscosity of the system is not increased, and the excellent construction performance is ensured.
The modified silica micropowder is preferably treated by vinyl trimethoxy silane, KH560 and dodecyl trimethoxy silane, more preferably treated by KH560, so that the bonding of the product to a base material can be increased after the modified filler is added.
In order to ensure the storage life and the curing performance of the product, the carrier of the component B is not selected from general methyl terminated polydimethylsiloxane, but selected from alkoxy terminated polymer, the alkoxy terminated polymer is one or two of alkoxy terminated polydimethylsiloxane and alkoxy terminated modified polyether resin, and in order to ensure the mechanical performance of the product after curing, the alkoxy terminated polydimethylsiloxane is more preferable.
The cross-linking agent is one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, polymethyltriethoxysilane, methyltrimethoxysilane and methyltriethoxysilane, and in order to ensure the cross-linking density and the toughness of the product after curing, one or more of the ethyl orthosilicate and the polymethyltriethoxysilane are more preferable.
In order to ensure the bonding performance of the cured product, the coupling agent is one or more of 3-aminopropyltriethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and bisaminosilane compounds.
The organic tin catalyst is one or more of dibutyltin dilaurate, dimethyltin dilaurate, dioctyltin dilaurate and dibutyltin diacetate, and the organic tin catalyst is preferably dibutyltin dilaurate in order to ensure the curing speed of the product.
The invention also comprises a preparation method of the low-proportion bi-component dealcoholized organosilicon sealant, which comprises the following steps:
(1) preparation of component A
Dispersing and uniformly mixing 35-60 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane, 35-65 parts of reinforcing filler and 0-10 parts of methyl-terminated polydimethylsiloxane at a high speed, stirring at 100-1000 r/min, heating to 110-130 ℃, vacuumizing and defoaming for 1-2 h, and cooling to room temperature to obtain a component A;
(2) preparation of component B
Dispersing and mixing 30-60 parts of alkoxy end-capped polymer and 35-65 parts of reinforcing filler at a high speed uniformly, heating to 110-130 ℃, vacuumizing and defoaming for 1-2 hours, cooling to room temperature in a vacuum or dry compressed air and nitrogen state, completely eradicating air or moisture contact in the whole process, adding 4-10 parts of cross-linking agent, 0.1-5 parts of coupling agent and 0.1-5 parts of organic tin catalyst at a high speed, dispersing and mixing uniformly at a stirring speed of 100-1000 r/min, vacuumizing and defoaming to obtain a component B, and storing in a sealed manner.
Because the alkoxy-terminated polymer can generate cross-linking reaction when meeting water and be solidified, the component B needs to remove the water in the filler and prevent the water vapor from entering, and is sealed and stored.
Wherein, in order to obtain better bonding and storage effects, two or more than two crosslinking agents and coupling agents in the component B are selected for compounding.
Wherein the defoaming vacuum degree is less than or equal to-0.08 MPa.
The obtained A, B components are mixed according to the weight ratio of 100: 80-120 to obtain the low-proportion bi-component dealcoholized organosilicon sealant.
The invention has simple production process and no special requirement on equipment.
The invention also discloses a low-proportion bi-component dealcoholized organosilicon sealant which is widely applied to sealing of an aluminum frame of a solar photovoltaic module, bonding of a junction box and a back plate, assembly of electronic components and the like.
Has the advantages that: compared with the prior art, the invention has the advantages that: the low-proportion double-component dealcoholized organosilicon sealant prepared by the invention is insensitive to the mixing proportion, reduces the problems of no curing or poor bonding and the like caused by the error of the mixing proportion, has good mechanical property after curing, high deep curing speed, good durability and stable storage, can be bonded with a plurality of base materials which can be anodic aluminum oxide, glass, die-casting aluminum, ceramic and the like, and has no corrosivity to various metals.
Detailed Description
The raw material source is not particularly limited in the present invention, and a general supplier product well known in the art may be used.
Example 1 preparation of a Low-ratio two-component dealcoholized Silicone sealant
1) Preparing a component A: 60 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane with viscosity of 20000mpa.s and specific surface area of 18-20 m260 parts of nano calcium carbonate per gram and 5 parts of KH560 modified silica micropowder with the particle size of 5 mu m, uniformly mixing and stirring, heating to 130 ℃, defoaming for 1h at the rotating speed of 1000rpm under the vacuum degree of-0.09 Mpa, and cooling to the temperature of less than 40 ℃ to obtain the component A.
2) The component B is prepared: 60 parts of alkoxy-terminated polydimethylsiloxane with the specific surface area of 18-20 m260 parts of nano calcium carbonate per gram and 5 parts of KH560 modified silicon micropowder with the particle size of 5 mu m are dispersed and mixed uniformly at high speed, the temperature is raised to 130 ℃, vacuumization and deaeration are carried out for 1h, the mixture is cooled to room temperature (less than 30 ℃) in a vacuum state, 10 parts of tetraethoxysilane and polymethyltriethoxysilane (the molar ratio is 5: 2), 5 parts of 3-aminopropyltriethoxysilane, 5 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and bisaminosilane compound (the molar ratio is 1:0.5: 1) and 0.1 part of dibutyltin dilaurate are added, the mixture is stirred uniformly and deaerated, the rotating speed is 1000rpm, the vacuum degree is-0.09 MPa, the mixture is stirred for 20min, and the component B is obtained after sealing and preservation.
3) A, B components prepared by the method are mixed according to the weight ratio of 100: 100 to obtain the two-component dealcoholized organosilicon sealant.
Example 2
1) Preparing a component A: 35 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane with the viscosity of 80000mpa.s and the specific surface area of 18-20 m240 parts of nano calcium carbonate per gram, 5 parts of KH560 modified silica micropowder with the particle size of 5 mu m and 10 parts of methyl polydimethylsiloxane with the viscosity of 350mpa.s, uniformly mixing and stirring, heating to 110 ℃, defoaming for 2 hours at the rotating speed of 100rpm and the vacuum degree of-0.09 Mpa, and cooling to the temperature of less than 40 ℃ to obtain the component A.
2) The component B is prepared: 30 parts of alkoxy-terminated polydimethylsiloxane and 18-20 m of specific surface area of reinforcing filler220 parts of nano calcium carbonate per gram and 15 parts of KH560 modified silicon micropowder with the particle size of 5 mu m are dispersed and mixed uniformly at a high speed, the temperature is raised to 110 ℃, the mixture is vacuumized and defoamed for 2 hours, the mixture is cooled to room temperature (less than 30 ℃) in a vacuum state, 4 parts of tetraethoxysilane, polymethyltriethoxysilane (the molar ratio is 5: 2), 0.1 part of 3-aminopropyltriethoxysilane, 0.1 part of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and bisaminosilane compound (the molar ratio is 1:0.5: 1) and 5 parts of dibutyltin dilaurate are added, the mixture is stirred uniformly and defoamed, the rotating speed is 100rpm, the vacuum degree is-0.09 Mpa, the mixture is stirred for 15 minutes, and the component B is obtained after sealed preservation and sealed preservation.
3) A, B components prepared by the method are mixed according to the weight ratio of 100: 80 to obtain the two-component dealcoholized organosilicon sealant.
Example 3
1) Preparing a component A: 50 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000mpa.s and 80000mpa.s (the molar ratio is 1: 1) and the specific surface area of 18-20 m255 parts of nano calcium carbonate per gram, 10 parts of KH560 modified silica micropowder with the particle size of 5 mu m and 5 parts of methyl polydimethylsiloxane with the viscosity of 350mpa.s, uniformly mixing and stirring, heating to 110 ℃, defoaming for 2 hours at the rotating speed of 600rpm and the vacuum degree of-0.09 Mpa, and cooling to the temperature of less than 40 ℃ to obtain the component A.
2) The component B is prepared: 60 parts of alkoxy end capping modified polyether resin with the specific surface area of 18-20 m245 parts of nano calcium carbonate/g, 5 parts of KH560 modified silicon micropowder with the particle size of 3 mu m and 10 parts of silicon micropowder with the particle size of 5 mu m, dispersing and mixing uniformly at a high speed, heating to 110 ℃, vacuumizing and defoaming for 2h, cooling to room temperature (less than 30 ℃) in a vacuum state, adding 8 parts of tetraethoxysilane, polymethyl triethoxy silane (the molar ratio is 5: 3), 3-aminopropyl triethoxy silane, 3 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxy silane bisaminosilane compound (the molar ratio is 1:0.5: 1) and 1 part of dibutyltin dilaurate, mixing and stirring uniformly and defoaming at the rotating speed of 600rpm and the vacuum degree of-0.09 MPa, stirring for 15min and the temperature of 25 ℃ to obtain a component B, and sealing and storing.
3) A, B components prepared by the method are mixed according to the weight ratio of 100: 120 to obtain the two-component dealcoholized organosilicon sealant.
Example 4
1) Preparing a component A: 60 parts of alpha, omega-hydroxyl-terminated polydimethylsiloxane with viscosity of 20000mpa.s and specific surface area of 50m250 parts of nano calcium carbonate per gram, 5 parts of KH560 modified silica micropowder with the particle size of 5 mu m and 5 parts of silica micropowder with the particle size of 5 mu m are mixed, stirred uniformly, heated to 110 ℃, defoamed for 2 hours at the rotating speed of 1000rpm and the vacuum degree of-0.09 Mpa, and cooled to the temperature of less than 40 ℃ to obtain the component A.
2) The component B is prepared: 60 parts of alkoxy-terminated polydimethylsiloxane with the specific surface area of 50m245 parts of nano calcium carbonate per gram, 5 parts of KH560 modified silicon micropowder with the grain diameter of 3 mu m and 10 parts of silicon micropowder with the grain diameter of 5 mu m, and the components are dispersed at high speedUniformly mixing, heating to 130 ℃, vacuumizing and defoaming for 1h, cooling to room temperature (less than 30 ℃) in a vacuum state, adding 7 parts of tetraethoxysilane, 7 parts of polymethyltriethoxysilane (molar ratio of 5: 2), 5 parts of 3-aminopropyltriethoxysilane, 5 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and bisaminosilane compound (molar ratio of 1:0.5: 1) and 1 part of dibutyltin dilaurate, uniformly mixing, stirring and defoaming at the rotating speed of 1000rpm and the vacuum degree of-0.09 MPa for 20min and the temperature of 25 ℃ to obtain a component B, and sealing and storing.
3) A, B components prepared by the method are mixed according to the weight ratio of 100: 100 to obtain the two-component dealcoholized organosilicon sealant.
Comparative example 1
In this comparative example, 30 parts of alkoxy-terminated polydimethylsiloxane of component B was replaced with dimethylsilicone oil, otherwise the same as in example 1.
Comparative example 2
In the comparative example, 60 parts of alkoxy-terminated polydimethylsiloxane, 10 parts of fumed silica with the specific surface area of 150m2/g and 55 parts of heavy calcium carbonate with the particle size of 1500 meshes are uniformly dispersed and mixed at a high speed, and the water content of the heavy calcium carbonate is generally lower than 0.1%, so that the temperature rise and dehydration are not needed, after the filler and the polymer are mixed, 10 parts of tetraethoxysilane, polymethyltriethoxysilane (molar ratio 5: 2), 3-aminopropyltriethoxysilane, 5 parts of gamma- (2, 3-glycidoxy) propyltrimethoxysilane bisaminosilane compound (molar ratio 1:0.5: 1) and 0.1 part of dibutyltin dilaurate are added, the mixture is uniformly stirred and defoamed, the rotating speed is 1000rpm, the vacuum degree is-0.09 MPa, the stirring is carried out for 20min, the component B is obtained and the component B is hermetically stored. The rest is the same as example 1.
Comparative example 3
In the comparative example, 60 parts of alkoxy-terminated polydimethylsiloxane having a specific surface area of 18 to 20m was used265 portions of nano calcium carbonate per gram are dispersed and mixed evenly at high speed, 4 portions of tetraethoxysilane, polymethyl triethoxy silane (the mol ratio is 5: 2) and 3-aminopropyl triethoxy silane and gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane bisamino silane compound (the mol ratio is 1:0.5: 1) are added5 parts of dibutyltin dilaurate and 1 part of dibutyltin dilaurate, uniformly mixing and stirring, defoaming, stirring at the rotation speed of 1000rpm and the vacuum degree of-0.09 Mpa for 15min at the temperature of 25 ℃ to obtain a component B, and sealing and storing. The rest is the same as example 1.
Example 5
In the comparative example, 60 parts of alkoxy-terminated polydimethylsiloxane having a specific surface area of 18 to 20m was used260 parts of nano calcium carbonate per gram and 5 parts of KH560 modified silicon micropowder with the particle size of 5 mu m are dispersed and mixed uniformly at high speed, the temperature is raised to 130 ℃, vacuumization and deaeration are carried out for 1h, the mixture is cooled to room temperature (less than 30 ℃) in a vacuum state, 10 parts of ethyl orthosilicate, 5 parts of 3-aminopropyltriethoxysilane, 5 parts of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane (the molar ratio is 2: 1) and 0.1 part of dibutyltin dilaurate are added, the mixture is mixed, stirred uniformly and deaerated, the rotating speed is 1000rpm, the vacuum degree is-0.09 MPa, the mixture is stirred for 20min, and the component B is obtained and stored in a sealing way. The rest is the same as example 1.
Experimental example:
the curing conditions of the two-component dealcoholized silicone sealants of examples 1 to 5 of the present invention are not particularly limited, and the curing is preferably performed at a temperature of 25 to 30 ℃ and in a humidity environment of 45% to 65%, and the sealant gels after surface drying, and is preferably cured at a temperature of 25 to 30 ℃ and in a humidity environment of 45% to 65% for 24 hours.
The two-component dealcoholized silicone sealants prepared in examples 1 to 5 and comparative examples 1 to 3 were tested for initial tack-free time, gel time, tensile strength, elongation at break, and adhesion to a substrate, and the results are shown in table 1:
TABLE 1
Figure BDA0002259776680000071
Figure BDA0002259776680000081
The two-component dealcoholized silicone sealant A, B prepared in examples 1 to 5 and comparative examples 1 to 3 was tested for surface dry time, gel time, tensile strength, elongation at break, and adhesion to a substrate after storage at 80 ℃ for 7 days, and the results are shown in table 2:
TABLE 2
Figure BDA0002259776680000082
And carrying out qualitative bonding test on the substrate, cleaning the bonding surface according to engineering requirements, ensuring that the sealant is completely bonded with the bonding surface, wherein the area of the bonding material is more than 200mm x 10mm, curing for 168h in a standard environment, pulling the sealant with force at an angle of 90 degrees, and calculating the area percentage of the residual sealant on the surface of the substrate. The failure of the substrate surface sealant is denoted by CXX. For example, C100 indicates 100% cohesive failure, no interfacial failure, and full effective adhesion, C90 indicates 90% cohesive failure effective adhesion, 10% interfacial failure partial adhesion failure, C50 indicates 50% cohesive failure effective adhesion, 50% interfacial failure partial adhesion failure, and C00 indicates full interfacial failure with no effective adhesion.
As can be seen from tables 1-2, the two-component dealcoholized organosilicon sealant prepared in the embodiments 1-4 of the invention is insensitive to the mixing ratio, has good mechanical property after curing, fast deep curing speed, fast adhesion speed to a substrate, good durability and good storage stability, and can be widely applied to photovoltaic module aluminum frame sealing, junction box and back plate adhesion, automobile electronic component assembly, building curtain wall assembly and the like. The cross-linking agent and the coupling agent in the component B of the example 5 are prepared singly, but are not prepared in the example 1, so that the bonding property and the stability of the component B are much poorer than those of the component B of the example 1, and therefore, the preparation method is selected in the actual preparation process.

Claims (1)

1. The preparation method of the low-proportion bi-component dealcoholized organosilicon sealant is characterized by comprising the following steps:
1) preparing a component A: mixing the mixture with the molar ratio of 20000mpa.s to 80000mpa.s of 1: 50 parts of 1 alpha, omega-hydroxyl-terminated polydimethylsiloxane, and the specific surface area of the 1 alpha, omega-hydroxyl-terminated polydimethylsiloxane is 18-20 m2Per g nano calcium carbonate 55 parts of KH560 modified silica micropowder with the particle size of 5 mu m and 5 parts of methyl polydimethylsiloxane with the viscosity of 350mpa.s, uniformly mixing and stirring, heating to 110 ℃, defoaming for 2h at the rotating speed of 600rpm and the vacuum degree of-0.09 Mpa, and cooling to the temperature of less than 40 ℃ to obtain a component A;
2) the component B is prepared: 60 parts of alkoxy end capping modified polyether resin with the specific surface area of 18-20 m245 parts of nano calcium carbonate per gram, 5 parts of KH560 modified silica micropowder with the particle size of 3 mu m and 10 parts of silica micropowder with the particle size of 5 mu m, dispersing and mixing uniformly at a high speed, heating to 110 ℃, vacuumizing and defoaming for 2 hours, cooling to room temperature in a vacuum state, adding tetraethoxysilane and polymethyltriethoxysilane with the molar ratio of 5: 3 to 8 portions, 3-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and a diamino silane compound with the molar ratio of 1:0.5:1, 3 portions and 1 portion of dibutyltin dilaurate, mixing, stirring uniformly and defoaming at the rotating speed of 600rpm and the vacuum degree of-0.09 MPa for 15min at the temperature of 25 ℃ to obtain a component B, and sealing and storing;
3) a, B components prepared by the method are mixed according to the weight ratio of 100: 120 to obtain the two-component dealcoholized organosilicon sealant.
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