CN108865052B - Single-component dealcoholized silicone structure sealant for building curtain wall and preparation method thereof - Google Patents
Single-component dealcoholized silicone structure sealant for building curtain wall 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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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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 relates to a single-component dealcoholized silicone structural sealant for a building curtain wall and a preparation method thereof, belonging to the field of silicone structural sealants and comprising the following steps: alpha, omega-dihydroxy polydimethylsiloxane, alkoxy-terminated polydimethylsiloxane, calcium carbonate, fumed silica, a plasticizer, carbon black mother pulp, antioxidant mother pulp, a silane cross-linking agent, a silane coupling agent, a titanate complex and an organic tin catalyst, wherein the antioxidant mother pulp comprises alpha, omega-dihydroxy polydimethylsiloxane, calcium carbonate and an antioxidant, and the carbon black mother pulp comprises the plasticizer and carbon black. According to the invention, the antioxidant type with environmental protection and excellent oxidation resistance is selected for compounding, so that the silicone structural sealant is endowed with excellent ageing resistance, and the preparation process of the silicone structural sealant is improved, so that the silicone structural sealant with good compatibility and stable storage is obtained, is suitable for being applied to building glass curtain walls, and meets the requirements of the industry and the market.
Description
Technical Field
The invention relates to a single-component dealcoholized silicone structural sealant for a building curtain wall and a preparation method thereof, belonging to the field of silicone structural sealants.
Background
The structural adhesive specially designed for the bonding assembly of metal and glass structures or non-structures in the glass curtain wall is a silicone structural sealant, the silicone structural sealant is produced by taking linear polysiloxane as a main raw material, a main chain of the silicone structural sealant mainly comprises Si-O-Si bonds, a silane cross-linking agent and a basic polymer react to form a net-shaped structure in the curing process, and the Si-O-Si bonds are higher than ultraviolet bond energy, so that the silicone structural sealant has excellent cohesiveness, weather resistance and ultraviolet resistance compared with other types of sealants. The silicone structural sealant is divided into a single-component silicone structural sealant and a double-component silicone structural sealant, and is mainly used for sealing curtain wall glass structures and sealing second structures of hollow glass. The single-component silicone structure sealant does not need to be added with an additional curing agent, the curing process is changed by contacting moisture in the air, the single-component silicone structure sealant 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, wherein the dealcoholization type and the ketoxime type are neutral glue, but the dealcoholization type has no corrosivity to any material, while the ketoxime type has no corrosivity to aluminum materials, coated glass, inorganic materials and the like, and has corrosivity to copper, lead, zinc and polycarbonate; the two-component silicone structural sealant is divided into two components, and the two components are cured after two groups of mucilage are mixed.
Although the silicone structural sealant has excellent ageing resistance, in practical application, the ageing of the silicone structural sealant is accelerated due to environmental and weather factors, such as light, heat, sample, rainwater, vibration, wind and the like, so that the silicone structural sealant is discolored, foamed, cracked, debonded, and the performance of the silicone structural sealant is reduced, and the service life of the silicone structural sealant is shortened. In the past, the quality and performance of silicone structural sealant in the industry are designed by referring to GB16776-2005 structural silicone sealant for building, which can only provide 10 years of quality assurance, so that most commercial silicone structural sealant products can only provide 10 years of quality assurance at present, and if the service life of the silicone structural sealant exceeds 10 years, the safety risk is greatly increased. Since the minimum requirement of the design service life of the glass curtain wall is definitely specified in JGJ 102-2003 glass curtain wall engineering technical specification to be 25 years, at present, only the silicone structural sealant which meets JG/T475-2015 Silicone structural sealant for building curtain walls and ETAG 002 structural sealant Assembly System European technical certification guidelines can reach the standard of the minimum service life of 25 years.
The Chinese patent application publication CN 102212328A discloses a silicone one-component sealant and a preparation method thereof, and more than 30 raw materials such as room temperature vulcanized methyl silicone rubber, dimethyl silicone oil, 107 silicone rubber, fumed silica and the like are adopted, so that the ultraviolet resistance, aging resistance and strong acid and alkali resistance of the product are improved, the curing is fast, the application range is wide, the strength after curing is high, the product can be stronger than the general bearing tension by one time, particularly, the product can still keep good performance after being soaked in water for a long time, and the silicone one-component sealant has good social benefits and economic benefits. However, as can be seen from the embodiment of the invention, the silicone structural sealant is still designed according to the standard of GB16776-2005 silicone structural sealant for construction, which does not meet the future requirements, and the invention improves the aging resistance of the one-component silicone structural sealant by adding components such as an anti-aging agent, but after a plurality of tests, the inventor finds that the finished product prepared according to the technical documents is very viscous and cannot be constructed and practically applied at all, so that at present, few silicone structural sealants with the service life of more than 25 years are available in the market.
The Chinese invention patent application publication No. CN 105385408B discloses an anti-fatigue and anti-ultraviolet single-component dealcoholized silicone structural sealant and a preparation method thereof, and the formula of the sealant comprises the following raw materials in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 60-120 parts of reinforcing filler, 5-15 parts of plasticizer, 3-8 parts of cross-linking agent, 0.2-2 parts of bimetallic aluminum-zirconium coupling agent, 0.5-3 parts of catalyst and 0.5-2 parts of deep curing agent, wherein the bimetallic aluminum-zirconium coupling agent is one or more of aluminum methacrylate-zirconium coupling agent, aluminum adipate-zirconium coupling agent, aluminum itaconate-zirconium coupling agent and aluminum stearate-zirconium coupling agent. Although the single-component dealcoholized silicone sealant provided by the invention has good mechanical property and storage stability, is not easy to yellow and can be quickly cured, and also has the functions of resisting fatigue and ultraviolet radiation, the sealant is applied to insulated cables and the automobile industry and is not the sealant used for building curtain wall construction.
Therefore, the development of the high-performance environment-friendly silicone structural sealant with the service life of more than 25 years is a future requirement of the market and is a hot point of research and development.
Disclosure of Invention
The invention aims at solving the problems in the prior art, namely the technical problem to be solved is to provide the single-component dealcoholized silicone structure sealant for the building curtain wall and the preparation method thereof, the antioxidant type with environmental protection and excellent oxidation resistance is selected for compounding, so that the silicone structure sealant is endowed with excellent ageing resistance, and the preparation process of the silicone structure sealant is improved, so that the silicone structure sealant with good compatibility and stable storage is obtained, is suitable for being applied to the building glass curtain wall, and meets the requirements of the industry and the market.
In order to solve the technical problems, the technical scheme adopted by the invention is to provide a single-component dealcoholized silicone structure sealant for a building curtain wall, which comprises the following components: the antioxidant master batch comprises alpha, omega-dihydroxy polydimethylsiloxane, alkoxy-terminated polydimethylsiloxane, calcium carbonate, fumed silica, a plasticizer, carbon black master batch, antioxidant master batch, a silane cross-linking agent, a silane coupling agent, a titanate complex and an organic tin catalyst, wherein the antioxidant master batch comprises the alpha, omega-dihydroxy polydimethylsiloxane, calcium carbonate and the antioxidant, and the carbon black master batch comprises the plasticizer and carbon black.
Preferably, the composition comprises the following components in parts by weight:
wherein the antioxidant mother pulp comprises:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane
30-60 parts of calcium carbonate
2-30 parts of antioxidant
Wherein the carbon black master batch comprises:
20-80 parts of carbon black
100 portions of plasticizer
Preferably, the antioxidant is selected from one or more of hindered phenol antioxidants, phosphite antioxidants and thioester antioxidants.
Preferably, the primary antioxidant is selected from one or more of antioxidant 1010, antioxidant 1076 and antioxidant 245, and the secondary antioxidant is selected from one or more of antioxidant 168, antioxidant DLTP and antioxidant DSTP.
The antioxidant 1010 is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, is a macromolecular multifunctional hindered phenol antioxidant, is white crystalline powder in appearance, is soluble in benzene, acetone and chloroform, and is insoluble in water. No pollution, no coloring, low volatility and good drawing resistance. The antioxidant is widely applied to polyethylene, polypropylene, polyformaldehyde, ABS resin, PS resin, PVC, engineering plastics, rubber and petroleum products, has excellent antioxidant performance on the polypropylene and the polyethylene, and can effectively prolong the service life of the products.
The antioxidant 1076 is n-octadecyl beta- (4-hydroxy-3, 5-di-tert-butylphenyl) propionate, is a non-polluting, non-toxic hindered phenol antioxidant, is white or yellowish solid powder in appearance, is easily soluble in organic solvents such as benzene, chloroform, cyclohexane, acetone and esters, is slightly soluble in methanol, ethanol and mineral oil, is insoluble in water, is stable to light, is not prone to discoloration, is non-polluting, non-coloring, low in volatility, resistant to water extraction, good in compatibility and high in antioxidant efficiency, and is widely used in polyethylene, polypropylene, polyformaldehyde, ABS resin, polystyrene, polyvinyl chloride alcohol, engineering plastics, synthetic fibers, elastomers, adhesives, waxes, synthetic rubber and petroleum products. Preventing the thermal oxidative degradation of the substrate.
The antioxidant 245 is diethylene glycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], is a non-polluting hindered phenol antioxidant, is white or white-like crystalline powder in appearance, has good compatibility with polymers and high thermal oxidation resistance, and is suitable for high-impact polystyrene, ABS resin, AS resin, MBS resin, polyvinyl chloride, polyacetal, polyamide, polyurethane, hydroxylated styrene-butadiene rubber, styrene-butadiene latex and the like.
The antioxidant 168 is tris (2, 4-di-tert-butylphenyl) phosphite, is an excellent phosphite antioxidant, is white powder in appearance, is easily soluble in organic solvents such as benzene, chloroform and cyclohexane, is slightly soluble in ethanol and acetone, is insoluble in polar solvents such as water and alcohol, and is slightly soluble in esters. Low toxicity, low volatility, high thermal stability and excellent hydrolysis resistance, can effectively decompose hydroperoxide generated in the thermal processing process of polymeric materials, and is widely applied to high polymer materials such as polyolefin (such as polyethylene and polypropylene), olefin copolymer, polyamide, polycarbonate, PS resin, PVC, engineering plastics, rubber, petroleum products, ABS resin and the like.
The antioxidant DLTP is dilauryl thiodipropionate, white flake crystalline solid, insoluble in water, soluble in organic solvents such as acetone, carbon tetrachloride, benzene, petroleum ether and the like, can be widely used in synthetic materials such as polyethylene, polypropylene, ABS, PBT and the like, and can also be used in rubber processing and lubricating grease
The antioxidant DSTP is dioctadecyl thiodipropionate, white crystalline powder, is soluble in benzene, chloroform, carbon disulfide and carbon tetrachloride, is insoluble in dimethylformamide and toluene and is insoluble in acetone, ethanol and water, and can be widely used in synthetic materials such as polyethylene, polypropylene, ABS, PBT and the like, and can also be used in rubber processing and lubricating grease.
Although the antioxidants are all commonly used antioxidants, the antioxidant 1010, the antioxidant 1076, the antioxidant 245, the antioxidant 168, the antioxidant DLTP and the antioxidant DSTP are used as plastic additives in the past for improving the aging performance of plastics, and the antioxidants are added into the field of sealant for improving the aging performance of the sealant without any study.
Preferably, the weight ratio of the main antioxidant to the auxiliary antioxidant is 1:1-5: 1.
Preferably, the viscosity of the α, ω -dihydroxy polydimethylsiloxane is from 5000 to 80000mPa · s at 25 ℃, and the viscosity of the alkoxy-terminated polydimethylsiloxane is from 800 to 20000mPa · s at 25 ℃.
Preferably, the calcium carbonate is a mixture of heavy calcium carbonate and light calcium carbonate which are subjected to surface hydrophobic treatment, the weight ratio of the heavy calcium carbonate to the light calcium carbonate is 1:5-5:1, the average particle size of the calcium carbonate is 0.01-10 mu m, and the water content is less than or equal to 0.32%.
Preferably, the fumed silica is subjected to a hydrophobization treatment, and the specific surface area of the fumed silica is 150 to 220m 2/g. The calcium carbonate subjected to hydrophobic treatment and the fumed silica can reduce the affinity with water, and increase the compatibility and wettability with organic matters.
Preferably, the plasticizer is at least one of simethicone, MDS silicone oil and hydroxyl silicone oil.
Preferably, the silane crosslinking agent is at least one of methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane and dimethyldiethoxysilane.
Preferably, the silane coupling agent is at least one of gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropylmethyldiethoxysilane, gamma-glycidoxypropyltrimethoxysilane, and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane.
Preferably, the organic tin catalyst is at least one of dibutyltin dilaurate, dibutyltin diacetate and stannous octoate.
Preferably, the alpha, omega-dihydroxy polydimethylsiloxane is selected from the group consisting of the alpha, omega-dihydroxy polydimethylsiloxanes produced by Jiangxi Lanxing spark chemical Co., Ltd
107V 5000-V80000, and the alkoxy-terminated polydimethylsiloxane is one or more selected from the group consisting of alkoxy-terminated polydimethylsiloxanes produced by Jiangsu Konghe New Material Co., Ltd
One or more of F-10A, F-40A, F-01A, J-15, J-200 and J-800, wherein the light calcium carbonate is selected from one or more of KLNM-S020, KLNM-S031, KLNM-S034 and KLNM-S035 produced by Kailong chemical group Limited in Hubei, and the fumed silica is selected from one or more of Kabet produced by the company of America
TS-720, wherein the plasticizer is selected from Starsil produced by Jiangxi Lanxing Star fire chemical Co., LtdTMOne or more of PDMS 47V50-47V1000, and the antioxidant is selected from those produced by Ciba refinement (China) Co., Ltd
1010、
1076、
245、
168，
PS 800FL、
One or more PS 802FL, one or more silane crosslinking agents are selected from D-20 or D-150 produced by New blue sky, Inc. in Hubei, the silane coupling agents are selected from one or more LT171, LT550 or LT560 produced by New blue sky, Inc. in Hubei, the titanate complex is selected from D-62 produced by New blue sky, Inc. in Hubei, the organic tin catalyst is selected from one or more D-80, D-82 or D-70 produced by New blue sky, Inc. in Hubei, and the carbon black is selected from DL-430 produced by Cabot, Inc. in U.S. A.
The invention also adopts another technical scheme that a preparation method of the single-component dealcoholized silicone structure sealant for the building curtain wall is provided, which comprises the following steps:
(1) preparing antioxidant mother pulp: mixing and stirring the antioxidant, alpha, omega-dihydroxy polydimethylsiloxane and calcium carbonate for 15-40min, heating to 80-130 ℃, stirring for 100-300min, and cooling to obtain antioxidant mother pulp;
(2) preparing carbon black mother pulp: grinding carbon black and a plasticizer by a three-roll mill at room temperature, uniformly dispersing the carbon black, transferring the carbon black into a kettle, heating to 80-130 ℃, stirring for 30-300min, and cooling to obtain carbon black mother pulp;
(3) preparing mucilage: mixing and stirring alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, plasticizer, calcium carbonate and silicon dioxide, heating to 80-130 ℃, stirring for 30-300min, and cooling to obtain mucilage;
(4) preparing a finished product glue: adding the rubber cement, the antioxidant mother pulp, the carbon black mother pulp, the cross-linking agent, the coupling agent and the catalyst on a planetary machine at normal temperature in proportion, vacuumizing to 0.06-0.095 MPa, stirring for 30-120min, relieving the vacuum, and packaging.
By prefabricating the antioxidant master batch, the antioxidant is dispersed into the antioxidant master batch in a molten state and can be better mixed with the calcium carbonate and the alpha, omega-dihydroxy polydimethylsiloxane, so that the uniform dispersion of the antioxidant is ensured and the antioxidant is combined with other substances, similarly, by prefabricating the carbon black master batch, the carbon black which is difficult to disperse can be better dispersed and combined with other substances, and finally, the antioxidant master batch, the carbon black master batch and the mucilage are mixed and reacted, so that the compatibility and the storage stability of the finished product glue are ensured.
In a word, the single-component dealcoholized silicone structural sealant for the building curtain wall and the preparation method thereof are adopted, the antioxidant type with environmental protection and excellent oxidation resistance is selected for compounding, so that the silicone structural sealant is endowed with excellent ageing resistance, and the preparation process of the silicone structural sealant is improved, so that the silicone structural sealant with good compatibility and stable storage is obtained, is suitable for being applied to the building glass curtain wall, and meets the requirements of the industry and the market.
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings, but not intended to limit the scope of the invention.
Example 1
The invention provides a single-component dealcoholized silicone structural sealant for a building curtain wall, which comprises the following components in parts by weight: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 5 parts of alkoxy-terminated polydimethylsiloxane, 140 parts of calcium carbonate, 10 parts of fumed silica, 20 parts of plasticizer, 20 parts of carbon black mother slurry, 20 parts of antioxidant mother slurry, 15 parts of silane cross-linking agent, 8 parts of silane coupling agent, 5 parts of titanate complex and 5 parts of organic tin catalyst, wherein the antioxidant mother slurry comprises 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 60 parts of calcium carbonate and 30 parts of antioxidant, and the carbon black mother slurry comprises 80 parts of carbon black and 100 parts of plasticizer.
Wherein the alpha, omega-dihydroxy polydimethylsiloxane is selected from the group consisting of the alpha, omega-dihydroxy polydimethylsiloxanes produced by Jiangxi Lanxing Star flame chemical Co., Ltd
107V 5000, and the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is about 5000 mPas at 25 ℃.
The alkoxy-terminated polydimethylsiloxane is selected from the group consisting of those produced by Jiangsu Konghe New Material Ltd
J-200, wherein the viscosity of the alkoxy-terminated polydimethylsiloxane at 25 ℃ is 20000 mPas.
The calcium carbonate is a mixture of heavy calcium carbonate and light calcium carbonate which are subjected to surface hydrophobic treatment, the light calcium carbonate is selected from KLNM-S020 produced by Kyoto Kailong chemical group Co., Ltd, the weight ratio of the heavy calcium carbonate to the light calcium carbonate is 1:5, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 0.01 mu m, and the water content is 0.32%.
The fumed silica is selected from those produced by Cambot corporation, USA
TS-720, the fumed silica is subjected to hydrophobic treatment, and the specific surface area of the fumed silica is 150m2/g。
The plasticizer is selected from Starsil produced by Jiangxi Lanxing Star fire chemical Co LtdTM PDMS 47V50。
The main antioxidant is selected from Ciba extract (China) Co Ltd
1010, the secondary antioxidant is selected from those produced by Ciba specialty Chemicals (China)
168, the weight ratio of the main antioxidant to the auxiliary antioxidant is 1:1, and the concentration of the main antioxidant to the auxiliary antioxidant is 98%.
The carbon black is selected from DL-430 produced by Cabot corporation, USA.
The silane cross-linking agent is selected from D-20 produced by New materials of New blue sky, Hubei.
The silane coupling agent is selected from LT171 produced by New Material Ltd of New blue sky of Hubei.
The titanate complex is selected from D-62 produced by New materials of New blue sky, Hubei.
The organic tin catalyst is selected from D-80 produced by New materials of New blue sky, Hubei.
The preparation method of the single-component dealcoholized silicone structural sealant for the building curtain wall comprises the following steps:
(1) preparing antioxidant mother pulp: mixing and stirring the antioxidant, alpha, omega-dihydroxy polydimethylsiloxane and calcium carbonate for 15min, heating to 130 ℃, stirring for 100min, and cooling to obtain antioxidant mother pulp;
(2) preparing carbon black mother pulp: grinding carbon black and a plasticizer by a three-roller mill at room temperature, uniformly dispersing the carbon black, transferring the carbon black into a kettle, heating to 130 ℃, stirring for 30min, and cooling to obtain carbon black mother slurry;
(3) preparing mucilage: mixing and stirring alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, plasticizer, calcium carbonate and silicon dioxide, heating to 130 ℃, stirring for 30min, and cooling to obtain mucilage;
(4) preparing a finished product glue: adding the mucilage, the antioxidant mother pulp, the carbon black mother pulp, the cross-linking agent, the coupling agent and the catalyst on a planetary machine at normal temperature in proportion, vacuumizing to 0.06MPa, stirring for 120min, relieving the vacuum, and packaging.
Example 2
The one-component dealcoholized silicone structure sealant for the building curtain wall of example 2 is different from that of example 1 in that: the weight ratio of the main antioxidant to the auxiliary antioxidant is 3: 1.
The weight ratio of the heavy calcium carbonate to the light calcium carbonate is 3:5, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 5 mu m, and the water content is 0.3%.
The fumed silica has a specific surface area of 200m2/g。
The preparation method of the one-component dealcoholized silicone sealant for the building curtain wall in the embodiment 2 is different from that in the embodiment 1 in that: mixing and stirring the antioxidant, alpha, omega-dihydroxy polydimethylsiloxane and calcium carbonate for 25min in the step (1), heating to 100 ℃, and stirring for 200 min; heating to 100 ℃ in the step (2), and stirring for 100 min; heating to 100 ℃ in the step (3), and stirring for 100 min; and (4) vacuumizing to 0.08MPa, and stirring for 70 min.
Example 3
The one-component dealcoholized silicone structure sealant for the building curtain wall of example 3 is different from that of example 1 in that: the weight ratio of the main antioxidant to the auxiliary antioxidant is 5: 1.
The weight ratio of the heavy calcium carbonate to the light calcium carbonate is 5:1, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 10 mu m, and the water content is 0.2%.
The fumed silica has a specific surface area of 220m2/g。
The preparation method of the one-component dealcoholized silicone sealant for the building curtain wall in the embodiment 3 is different from that in the embodiment 1 in that: mixing and stirring the antioxidant, alpha, omega-dihydroxy polydimethylsiloxane and calcium carbonate for 40min in the step (1), heating to 80 ℃, and stirring for 300 min; heating to 80 ℃ in the step (2), and stirring for 300 min; heating to 80 ℃ in the step (3), and stirring for 300 min; and (4) vacuumizing to 0.095MPa, and stirring for 30 min.
Example 4
The one-component dealcoholized silicone structure sealant for the building curtain wall of example 4 is different from that of example 1 in that: the secondary antioxidant was not added.
The weight ratio of the heavy calcium carbonate to the light calcium carbonate is 3:1, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 7 mu m, and the water content is 0.2%.
The fumed silica has a specific surface area of 180m2/g。
Example 5
The one-component dealcoholized silicone structure sealant for the building curtain wall of example 5 is different from that of example 1 in that: comprises the following components in parts by weight: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 12 parts of alkoxy-terminated polydimethylsiloxane, 110 parts of calcium carbonate, 5 parts of fumed silica, 11 parts of plasticizer, 12 parts of carbon black master slurry, 12 parts of antioxidant master slurry, 10 parts of silane cross-linking agent, 4 parts of silane coupling agent, 2.5 parts of titanate complex and 2.5 parts of organic tin catalyst, wherein the antioxidant master slurry comprises 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 45 parts of calcium carbonate and 16 parts of antioxidant, and the carbon black master slurry comprises 50 parts of carbon black and 100 parts of plasticizer.
The weight ratio of the heavy calcium carbonate to the light calcium carbonate is 5:3, and the average particle size of the heavy calcium carbonate and the light calcium carbonate is 3 mu m.
The fumed silica has a specific surface area of 160m2/g。
Example 6
The one-component dealcoholized silicone structure sealant for the building curtain wall of example 6 is different from that of example 1 in that: comprises the following components in parts by weight: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 20 parts of alkoxy-terminated polydimethylsiloxane, 80 parts of calcium carbonate, 0 part of fumed silica, 2 parts of plasticizer, 5 parts of carbon black master slurry, 2 parts of antioxidant master slurry, 5 parts of silane cross-linking agent, 0.6 part of silane coupling agent, 0.1 part of titanate complex and 0.1 part of organic tin catalyst, wherein the antioxidant master slurry comprises 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of calcium carbonate and 2 parts of antioxidant, and the carbon black master slurry comprises 20 parts of carbon black and 100 parts of plasticizer.
The weight ratio of the heavy calcium carbonate to the light calcium carbonate is 1:3, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 1 mu m, and the water content is 0.1%.
The fumed silica has a specific surface area of 170m2/g。
Example 7
Example 7 is a preferred example, and the one-component dealcoholized silicone structure sealant for the building curtain wall of example 7 is different from that of example 1 in that: the main antioxidant is selected from those produced by Ciba refinement (China) Co
1076 and the secondary antioxidant is selected from the group consisting of those produced by Ciba specialty Chemicals (China) Co., Ltd
168, the weight ratio of the main antioxidant to the auxiliary antioxidant is 4: 1.
The weight ratio of the heavy calcium carbonate to the light calcium carbonate is 1:5, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 1 mu m, and the water content is 0.1%.
The fumed silica has a specific surface area of 150m2/g。
Comparative example
The comparative example used a commercial product which was also a one-component dealcoholized silicone structural sealant for building curtain walls.
The relevant physicochemical properties and the test standards of the finished products obtained in the invention after the examples 1 to 7 and the comparative examples are shown in the following table:
the invention has the beneficial effects that: the silicone structural sealant is endowed with excellent ageing resistance by selecting and compounding the antioxidant types with excellent environmental protection and oxidation resistance, the compatibility of the prepared mucilage can be effectively improved by selecting and using specific calcium carbonate and fumed silica, and the silicone structural sealant with good compatibility and stable storage is obtained by improving the preparation process of the silicone structural sealant, is suitable for being applied to building glass curtain walls and meets the requirements of industry and market.
Claims (7)
1. The sealant with the single-component dealcoholized silicone structure for the building curtain wall is characterized by comprising the following components in percentage by weight: the carbon black master slurry comprises a plasticizer and carbon black, the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is selected from one or more of antioxidants 1010, 1076 and 245, and the auxiliary antioxidant is selected from one or more of antioxidants 168, DLTP and DSTP.
2. The one-component dealcoholized silicone sealant for building curtain walls according to claim 1, which comprises the following components in parts by weight:
wherein the antioxidant mother pulp comprises:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane
30-60 parts of calcium carbonate
2-30 parts of antioxidant
Wherein the carbon black master batch comprises:
20-80 parts of carbon black
And 100 parts of a plasticizer.
3. The one-component dealcoholized silicone sealant for building curtain walls according to claim 1, wherein the ratio of the primary antioxidant to the secondary antioxidant is 1:1-5: 1.
4. The one-component dealcoholization type silicone structural sealant for the building curtain wall according to claim 1, wherein the viscosity of the α, ω -dihydroxy polydimethylsiloxane is 10000 to 80000mPa · s at 25 ℃, and the viscosity of the alkoxy-terminated polydimethylsiloxane is 800 to 20000mPa · s at 25 ℃.
5. The one-component dealcoholized silicone structural sealant for the building curtain wall according to claim 1, wherein the calcium carbonate is a mixture of heavy calcium carbonate and light calcium carbonate which are subjected to surface hydrophobic treatment, the weight ratio of the heavy calcium carbonate to the light calcium carbonate is 1:5-5:1, the average particle size of the calcium carbonate is 0.01-10 μm, and the water content is less than or equal to 0.32%.
6. The sealant in a one-component dealcoholized silicone structure for building curtain wall as claimed in claim 1, wherein the fumed silica is subjected to hydrophobic treatment, and the fumed silica has a specific surface area of 150-220m2/g。
7. The preparation method of the single-component dealcoholized silicone structure sealant for the building curtain wall is characterized by comprising the following steps of:
(1) preparing antioxidant mother pulp: mixing and stirring the antioxidant, alpha, omega-dihydroxy polydimethylsiloxane and calcium carbonate for 15-40min, heating to 80-130 ℃, stirring for 100-300min, and cooling to obtain antioxidant mother pulp;
(2) preparing carbon black mother pulp: grinding carbon black and a plasticizer by a three-roll mill at room temperature, uniformly dispersing the carbon black, transferring the carbon black into a kettle, heating to 80-130 ℃, stirring for 30-300min, and cooling to obtain carbon black mother pulp;
(3) preparing mucilage: mixing and stirring alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, plasticizer, calcium carbonate and silicon dioxide, heating to 80-130 ℃, stirring for 30-300min, and cooling to obtain mucilage;
(4) preparing a finished product glue: adding the rubber cement, the antioxidant mother pulp, the carbon black mother pulp, the cross-linking agent, the coupling agent and the catalyst on a planetary machine at normal temperature in proportion, vacuumizing to 0.06-0.095 MPa, stirring for 30-120min, relieving the vacuum, and packaging.
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| CN111138919A (en) * | 2020-03-11 | 2020-05-12 | 河北精涂科技有限公司 | Novel anti-friction super-long-acting super-hydrophobic material and preparation method thereof |
| CN111961408A (en) * | 2020-06-24 | 2020-11-20 | 厦门中思诺新材料有限公司 | Bottom sealant special for stone wet pasting and preparation method thereof |
| CN117467401B (en) * | 2023-12-04 | 2024-05-24 | 佛山市顺德区创世纪实业有限公司 | Anti-aging silicone sealant and preparation method thereof |
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