CN109021914B - Two-component silicone structural sealant for building curtain wall and preparation method thereof - Google Patents
Two-component silicone structural sealant for building curtain wall and preparation method thereof Download PDFInfo
- Publication number
- CN109021914B CN109021914B CN201810605664.9A CN201810605664A CN109021914B CN 109021914 B CN109021914 B CN 109021914B CN 201810605664 A CN201810605664 A CN 201810605664A CN 109021914 B CN109021914 B CN 109021914B
- Authority
- CN
- China
- Prior art keywords
- antioxidant
- component
- calcium carbonate
- carbon black
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to a two-component silicone structural sealant for a building curtain wall and a preparation method thereof, belonging to the field of silicone structural sealants and comprising a component A and a component B, wherein the component A comprises antioxidant mother slurry, alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, calcium carbonate, fumed silica and a plasticizer, and the component B comprises carbon black mother slurry, a cross-linking agent, a coupling agent and a catalyst; the antioxidant master batch comprises alpha, omega-dihydroxy polydimethylsiloxane, calcium carbonate and an antioxidant, and the carbon black master batch comprises carbon black and a plasticizer. According to the invention, the antioxidant with environmental protection and excellent oxidation resistance is selected for compounding, so that the silicone structural sealant has excellent ageing resistance, the compatibility of the adhesive cement can be effectively improved through the selected calcium carbonate and the gas-phase silica, the silicone structural sealant with good compatibility and stable storage is obtained through improving the preparation process, and the silicone structural sealant is suitable for building glass curtain walls and meets the requirements of the industry and the market.
Description
Technical Field
The invention relates to a two-component 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 GB 16776-2005 building silicone structural sealant, and only 10 years of quality assurance can be provided, so that most of commercially available silicone structural sealant products can only provide 10 years of quality assurance, 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 to be 25 years in JGJ 102-2003 glass curtain wall engineering technical specifications, 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. Therefore, the development of high performance silicone structural sealant with service life of more than 25 years is a future requirement of the market and is a hot spot of research and development.
Chinese patent application publication CN 102352214A discloses a two-component silicone structural sealant, which comprises a component A and a component B, wherein the component A comprises the following components in part by weight: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 10-15 parts of alkyl-terminated dimethyl polysiloxane and 75-88 parts of filler; the component B comprises the following components in percentage by mass: 50 parts of alkyl-terminated dimethyl polysiloxane, 8 parts of carbon black, 20 parts of alkoxy silane cross-linking agent, 15.5 parts of silane coupling agent, 1-1.5 parts of organic tin catalyst and 0.05-1 part of ultraviolet absorbent.
Chinese patent application publication No. CN 107805481A discloses a two-component silicone structural sealant, which comprises a component A: 11 parts of hydroxyl-terminated polydimethylsiloxane, 20-80 parts of alkyl-terminated polydimethylsiloxane, 50-80 parts of inorganic filler, 1-5 parts of pigment and a component B: 100 parts of alkyl-terminated polydimethylsiloxane, 10-30 parts of silane cross-linking agent, 1-4 parts of silane coupling agent, 4-8 parts of organic tin catalyst, 3-7 parts of anti-aging agent and 2-6 parts of ultraviolet absorbent.
Chinese patent application publication No. CN 101864172A discloses a two-component structural silicone sealant for construction, which comprises a component A: 80-120 parts of hydroxyl-terminated polydimethylsiloxane, 10-80 parts of alkyl-terminated polydimethylsiloxane, 100 parts of active filler and 300 parts of component B: 5-15 parts of alkoxy silane, 0.3-5 parts of silane coupling agent, 0.01-0.2 part of organic tin catalyst and 0.01-5 parts of light stabilizer.
It can be seen that the aging resistance of the two-component silicone structural sealant is improved by adding components such as an ultraviolet absorber or an anti-aging agent in the prior art documents, but the inventor finds through experiments that the finished products prepared according to the prior art documents are very viscous or can not meet the requirement of long-term storage, because the compatibility of the hindered amine ultraviolet absorber or anti-aging agent and the base adhesive is poor, the prepared adhesive cement is unstable, and construction and practical application can not be carried out, so that at present, silicone structural sealants with service lives of more than 25 years are rarely available in the market.
Disclosure of Invention
The invention aims at solving the problems in the prior art, namely the technical problem to be solved is to provide a two-component silicone structural sealant for building curtain walls and a preparation method thereof, the two-component silicone structural sealant is endowed with excellent ageing resistance by selecting antioxidant types with environmental protection and excellent oxidation resistance for compounding, the compatibility of the prepared mucilage can be effectively improved by selecting 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.
In order to solve the technical problems, the technical scheme adopted by the invention is to provide a two-component silicone structural sealant for a building curtain wall, which comprises a component A and a component B, wherein the component A comprises: the antioxidant comprises antioxidant mother pulp, alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, calcium carbonate, fumed silica and a plasticizer, wherein the component B comprises the following components: carbon black mother pulp, a silane cross-linking agent, a silane coupling agent and an organic tin catalyst; the antioxidant master batch comprises alpha, omega-dihydroxy polydimethylsiloxane, calcium carbonate and an antioxidant, and the carbon black master batch comprises carbon black and a plasticizer.
Preferably, the component A 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
The component B comprises:
wherein the carbon black master batch comprises:
100 portions of plasticizer
5-20 parts of carbon black
Preferably, the antioxidant is selected from one or more of hindered phenol antioxidants, phosphite antioxidants and thioester antioxidants.
Preferably, the antioxidant comprises a primary antioxidant and a secondary antioxidant, the primary antioxidant is selected from hindered phenol antioxidants, and the secondary antioxidant is selected from one or two of 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 -dihydroxypolydimethylsiloxane at 25 ℃ is 5000-.
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, the water content is lower than 0.32%, the fumed silica is subjected to hydrophobic treatment, and the specific surface area of the fumed silica is 150-220m 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 ethyl silicate, propyl silicate, methyltrimethoxysilane oligomer and methyltriethoxysilane oligomer.
Preferably, the silane coupling agent is at least one of vinyltriethoxysilane, vinyltrimethoxysilane, 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 Kyara chemical group of HubeiOne or more of KLNM-S020, KLNM-S031, KLNM-S034 and KLNM-S035 manufactured by Co., Ltd, and the fumed silica is selected from silica manufactured by Kabot corporation, USA
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 PS802FL, one or more silane cross-linking agents are selected from one or two of D-30 or D-90 produced by New materials of Hubei New blue sky, one or more silane coupling agents are selected from one or more of LT171, LT550 and LT560 produced by New materials of Hubei New blue sky, one or more organic tin catalysts are selected from one or more of D-80, D-82 and D-70 produced by New materials of Hubei New blue sky, and carbon black is selected from DL-430 produced by American Cabot.
Preferably, the volume ratio of the component A to the component B is 8:1-12: 1.
The invention also adopts another technical scheme to provide a preparation method of the two-component silicone structural sealant for the building curtain wall, 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 30-300min, and cooling to obtain antioxidant mother pulp;
(2) preparing a component A mucilage: mixing and stirring alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, plasticizer, calcium carbonate, silicon dioxide and antioxidant mother slurry, and further grinding by using a three-roll mill to obtain component A adhesive cement;
(3) preparing carbon black mother pulp: grinding carbon black and a plasticizer by a three-roll mill, uniformly dispersing the carbon black, transferring the carbon black into a kettle, heating to 80-130 ℃, stirring for 0.5-5 hours, and cooling to prepare carbon black mother slurry;
(4) preparing a component B mucilage: adding the carbon black mother slurry into a planetary stirring kettle, adding the silane cross-linking agent, the silane coupling agent and the organic tin catalyst according to the proportion, and stirring for 30-80min at the vacuum degree of-0.06-0.095 MPa and the rotation speed of 200 plus materials of 800rpm to prepare the component B adhesive cement.
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 alpha, omega-dihydroxy polydimethylsiloxane and the calcium carbonate, so that the uniform dispersion of the antioxidant is ensured, and the compatibility and the storage stability of the prepared A-component mortar are ensured.
In a word, the two-component silicone structural sealant for the building curtain wall and the preparation method thereof are adopted, the antioxidant type with excellent environmental protection and oxidation resistance is selected for compounding, so that the silicone structural sealant is endowed with excellent ageing resistance, the compatibility of the prepared mucilage can be effectively improved by selecting 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, so that the two-component silicone structural sealant 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 embodiments of the present invention is not intended to limit the scope of the invention.
Example 1
The invention provides a bi-component silicone structural sealant for a building curtain wall, which comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 10 parts of antioxidant mother pulp, 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 5 parts of alkoxy end-capped polydimethylsiloxane, 120 parts of calcium carbonate, 10 parts of fumed silica and 20 parts of plasticizer, wherein the component B comprises the following components: 100 parts of carbon black mother pulp, 80 parts of silane cross-linking agent, 30 parts of silane coupling agent and 8 parts of organic tin catalyst; the antioxidant master batch comprises 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 60 parts of calcium carbonate and 30 parts of antioxidant, the carbon black master batch comprises 20 parts of carbon black and 100 parts of plasticizer, and the volume ratio of the component A to the component B is 8: 1.
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 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 proportion 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 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 LtdTMPDMS 47V50。
The carbon black is selected from DL-430 produced by Cabot corporation, USA.
The silane cross-linking agent is selected from D-30 produced by New Material Ltd of New blue sky in Hubei.
The silane coupling agent is selected from LT171 produced by New Material Ltd of New blue sky of Hubei.
The organic tin catalyst is selected from D-80 produced by New materials of New blue sky, Hubei.
The preparation method of the bi-component 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 30min, and cooling to obtain antioxidant mother pulp;
(2) preparing a component A mucilage: mixing and stirring alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, plasticizer, calcium carbonate, silicon dioxide and antioxidant mother slurry, and further grinding by using a three-roll mill to obtain component A adhesive cement;
(3) preparing carbon black mother pulp: grinding carbon black and a plasticizer by a three-roll mill, uniformly dispersing the carbon black, transferring the carbon black into a kettle, heating to 130 ℃, stirring for 0.5 hour, and cooling to prepare carbon black mother pulp;
(4) preparing a component B mucilage: adding the carbon black mother slurry into a planetary stirring kettle, adding the silane cross-linking agent, the silane coupling agent and the organic tin catalyst according to the proportion, and stirring for 30min at the vacuum degree of-0.06 MPa and the rotating speed of 800rpm to prepare the component B adhesive slurry.
Example 2
The two-component silicone structural sealant for building curtain walls of example 2 differs from example 1 in that: the 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 two-component silicone structural 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 30min in the step (1), heating to 100 ℃, and stirring for 160 min; heating to 100 ℃ in the step (3), and stirring for 2.5 hours; in the step (4), the mixture is stirred for 50min under the conditions that the vacuum degree is-0.08 MPa and the rotating speed is 500 rpm.
Example 3
The two-component silicone structural sealant for an architectural curtain wall of example 3 differs from example 1 in that: the 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 two-component silicone structural 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 (3), and stirring for 5 hours; in the step (4), the mixture is stirred for 80min under the conditions that the vacuum degree is-0.095 MPa and the rotating speed is 200 rpm.
Example 4
The two-component silicone structural sealant for building curtain walls of example 4 differs from 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 two-component silicone structural sealant for an architectural curtain wall of example 5 differs from example 1 in that: the component A comprises the following components in parts by weight: 5 parts of antioxidant mother pulp, 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 12 parts of alkoxy end-capped polydimethylsiloxane, 100 parts of calcium carbonate, 7 parts of fumed silica and 12 parts of plasticizer, wherein the component B comprises the following components: 100 parts of carbon black mother slurry, 55 parts of silane cross-linking agent, 20 parts of silane coupling agent and 4 parts of organic tin catalyst; the antioxidant master batch comprises 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 45 parts of calcium carbonate and 16 parts of antioxidant, and the carbon black master batch comprises 12 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, the average particle size of the heavy calcium carbonate and the light calcium carbonate is 3 mu m, and the water content is 0.3%.
The fumed silica has a specific surface area of 160m2/g。
Example 6
The two-component silicone structural sealant for an architectural curtain wall of example 6 differs from example 1 in that: the component A comprises the following components in parts by weight: 1 part of antioxidant mother pulp, 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 20 parts of alkoxy end-capped polydimethylsiloxane, 80 parts of calcium carbonate, 4 parts of fumed silica and 4 parts of plasticizer, wherein the component B comprises the following components: 100 parts of carbon black mother pulp, 30 parts of silane cross-linking agent, 10 parts of silane coupling agent and 1 part of organic tin catalyst; the antioxidant master batch comprises 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 30 parts of calcium carbonate and 2 parts of antioxidant, and the carbon black master batch comprises 5 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 embodiment, and the two-component silicone structural sealant for building curtain walls of example 7 differs from 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
PS802FL, wherein the weight ratio of the primary antioxidant to the secondary antioxidant is 3: 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 two-component silicone structural sealant for building curtain walls, also formulated at a volume ratio of 8:1 between component a and component B.
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:
as can be seen from the above table, R at 23 ℃ for tensile adhesion and shear strength of the two-component silicone sealant obtained in accordance with the present inventionu,5The values and other performance data are better than those of the commercial products, so that the two-component silicone structural sealant obtained by the invention has more excellent ageing resistance.
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 (6)
1. The two-component silicone structural sealant for the building curtain wall is characterized by comprising a component A and a component B, wherein the component A comprises: the antioxidant comprises antioxidant mother pulp, alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, calcium carbonate, fumed silica and a plasticizer, wherein the component B comprises the following components: carbon black mother pulp, a silane cross-linking agent, a silane coupling agent and an organic tin catalyst; the antioxidant master batch comprises alpha, omega-dihydroxy polydimethylsiloxane, calcium carbonate and an antioxidant, the carbon black master batch comprises carbon black and a plasticizer, the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the weight ratio of the main antioxidant to the auxiliary antioxidant is 1:1-5:1, the main antioxidant is selected from hindered phenol antioxidants, the auxiliary antioxidant is selected from one or two of phosphite antioxidants and thioester antioxidants, and the carbon isThe calcium carbonate is a mixture of heavy calcium carbonate and light calcium carbonate 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, the water content is lower than 0.32 percent, the fumed silica is subjected to hydrophobic treatment, and the specific surface area of the fumed silica is 150-220m2/g。
2. The two-component silicone structural sealant for building curtain walls as claimed in claim 1, wherein, in parts by weight,
the component A comprises:
wherein the antioxidant mother pulp comprises:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane
30-60 parts of calcium carbonate
2-30 parts of antioxidant
The component B comprises:
wherein the carbon black master batch comprises:
100 portions of plasticizer
5-20 parts of carbon black.
3. The two-component silicone structural sealant for the building curtain wall as claimed in claim 1, wherein 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.
4. The two-component silicone structural sealant for building curtain walls as claimed in claim 1, wherein the volume ratio of the component A to the component B is 8:1-12: 1.
5. The two-component silicone sealant for building curtain wall as claimed in claim 1, wherein the viscosity of the α, ω -dihydroxy polydimethylsiloxane at 25 ℃ is 5000-.
6. The two-component silicone structural sealant for building curtain walls as claimed in claim 1, which is prepared by 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 30-300min, and cooling to obtain antioxidant mother pulp;
(2) preparing a component A mucilage: mixing and stirring alpha, omega-dihydroxy polydimethylsiloxane, alkoxy end-capped polydimethylsiloxane, plasticizer, calcium carbonate, silicon dioxide and antioxidant mother slurry, and further grinding by using a three-roll mill to obtain component A adhesive cement;
(3) preparing carbon black mother pulp: grinding carbon black and a plasticizer by a three-roll mill, uniformly dispersing the carbon black, transferring the carbon black into a kettle, heating to 80-130 ℃, stirring for 0.5-5 hours, and cooling to prepare carbon black mother slurry;
(4) preparing a component B mucilage: adding the carbon black mother slurry into a planetary stirring kettle, adding the silane cross-linking agent, the silane coupling agent and the organic tin catalyst according to the proportion, and stirring for 30-80min at the vacuum degree of-0.06-0.095 MPa and the rotation speed of 200 plus materials of 800rpm to prepare the component B adhesive cement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810605664.9A CN109021914B (en) | 2018-06-13 | 2018-06-13 | Two-component silicone structural sealant for building curtain wall and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810605664.9A CN109021914B (en) | 2018-06-13 | 2018-06-13 | Two-component silicone structural sealant for building curtain wall and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109021914A CN109021914A (en) | 2018-12-18 |
| CN109021914B true CN109021914B (en) | 2021-05-18 |
Family
ID=64609197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810605664.9A Active CN109021914B (en) | 2018-06-13 | 2018-06-13 | Two-component silicone structural sealant for building curtain wall and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109021914B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861934A (en) * | 2021-11-05 | 2021-12-31 | 东莞市山力高分子材料科研有限公司 | Industrial glue for electronic and electric appliances |
| CN114045150B (en) * | 2021-11-12 | 2023-07-14 | 湖北回天新材料股份有限公司 | Multifunctional silica gel for indoor decoration and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580688B (en) * | 2009-06-12 | 2011-07-13 | 深圳市百丽春粘胶实业有限公司 | Dual-component silicone sealant formula used for construction and preparation thereof |
| CN103087642A (en) * | 2011-11-03 | 2013-05-08 | 阿特斯(中国)投资有限公司 | Solar cell packaging adhesive film and preparation method thereof |
| WO2013168600A1 (en) * | 2012-05-08 | 2013-11-14 | 丸尾カルシウム株式会社 | Surface-treated calcium carbonate filler, and curable resin composition containing said filler |
| CN103232832B (en) * | 2013-04-27 | 2015-08-12 | 广州市白云化工实业有限公司 | A kind of fast setting solar photovoltaic assembly seal gum and preparation method thereof |
-
2018
- 2018-06-13 CN CN201810605664.9A patent/CN109021914B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN109021914A (en) | 2018-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108865052B (en) | Single-component dealcoholized silicone structure sealant for building curtain wall and preparation method thereof | |
| CN110105907B (en) | Single-component silane modified polyether sealant for quick assembly of automobile glass and preparation method thereof | |
| CN106147694B (en) | Instant sealing silicone sealant and preparation method thereof | |
| CN109233731B (en) | Reactive hot-melt adhesive composition and preparation method and application thereof | |
| CN109021914B (en) | Two-component silicone structural sealant for building curtain wall and preparation method thereof | |
| CN107652938B (en) | Flame-retardant polyurethane caulking glue and preparation method thereof | |
| CN108059945B (en) | Organosilicon sealant for photovoltaic dual-glass assembly and preparation method thereof | |
| CN112322250A (en) | Silicone weather-resistant flame-retardant sealant and preparation method thereof | |
| CN109762511B (en) | Single-component dealcoholized room temperature vulcanized silicone sealant and preparation method thereof | |
| CN113512393A (en) | Soaking-resistant flame-retardant single-component silane modified polyether sealant and preparation method thereof | |
| CN113337245B (en) | Dealcoholized photovoltaic module sealant and preparation method thereof | |
| CN111394054A (en) | Silicone rubber for self-adhesive tape and preparation method thereof | |
| CN108865051B (en) | Single-component oxime-removing silicone structural sealant for building curtain wall and preparation method thereof | |
| CN112980375A (en) | Single-component silane modified polyether sealant and preparation method thereof | |
| CN106190013B (en) | silicone resin type bi-component elastic silicone sealant for hollow glass and preparation method thereof | |
| CN114621724B (en) | Double-component organic silicon sealant and preparation method thereof | |
| CN112210341B (en) | Double-vulcanization system building sealant and preparation method thereof | |
| CN113845869A (en) | Aging-resistant silane modified polyether sealant for buildings and preparation method thereof | |
| CN111592850B (en) | Modified silane adhesive and preparation method and application thereof | |
| CN115260584B (en) | Environment-friendly stabilizer for new energy charging cable | |
| CN116376187A (en) | Polyvinyl chloride composite material and preparation method and application thereof | |
| CN110922940B (en) | Environment-friendly MS sealant with rapid solidification and stable storage at room temperature and preparation method thereof | |
| CN115746565A (en) | Room temperature vulcanized silicone rubber and preparation method and application thereof | |
| CN113583608A (en) | Mildew-proof yellowing-resistant silane modified transparent adhesive and preparation method thereof | |
| CN102399527A (en) | Room temperature curing lamp adhesive and manufacturing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |