CN111139023B - High-adhesion bi-component organosilicon sealant for car lamp and preparation method thereof - Google Patents
High-adhesion bi-component organosilicon sealant for car lamp and preparation method thereof Download PDFInfo
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- CN111139023B CN111139023B CN202010013448.2A CN202010013448A CN111139023B CN 111139023 B CN111139023 B CN 111139023B CN 202010013448 A CN202010013448 A CN 202010013448A CN 111139023 B CN111139023 B CN 111139023B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- 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
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
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Abstract
The invention provides a high-adhesion two-component organosilicon sealant for vehicle lamps, which comprises the following components in percentage by mass (7-12): 1, a component A and a component B; the component A comprises: 100 parts by weight of hydroxyl-terminated polydimethylsiloxane; 20-200 parts by weight of calcium carbonate; the component B comprises: 100 parts of color paste; 5-40 parts by weight of a crosslinking agent; 3-20 parts by weight of an SC coupling agent; 1-15 parts of a catalyst; the SC coupling agent is prepared from the following raw materials: 5-50 parts by weight of a titanate compound; 5-50 parts by weight of aminosiloxane; 50 parts by weight of absolute ethyl alcohol. Compared with the prior art, the high-adhesion two-component organosilicon sealant for the car lamp provided by the invention adopts specific content components, realizes better interaction, enables the product to have low volatile components, high tensile strength and good elasticity, and has excellent adhesion performance, aging resistance, humidity resistance and high and low temperature resistance on PC and PP materials for the car lamp.
Description
Technical Field
The invention relates to the technical field of double-component condensed type organosilicon sealants, in particular to a high-adhesion double-component organosilicon sealant for vehicle lamps and a preparation method thereof.
Background
The automobile lamp is an essential component of an automobile, plays an important role in night illumination, driving signals, anti-collision in foggy days, steering signs and the like, and is an important guarantee for safe driving of the automobile. Along with the development requirements of automobiles towards the directions of environmental protection, energy conservation, safety, comfort, light weight, low cost, long service life and no pollution, the development and application of novel high-quality automobile adhesives/sealants become more and more important.
The current domestic car lamp sealant mainly comprises hot-melt butyl rubber, reactive polyurethane hot-melt adhesive and organosilicon sealant. The automobile lamp sealed by the common hot melt adhesive often has the problems of fogging, water leakage, cracking of an adhesive layer, poor adhesive force and the like, and the driving safety of drivers and passengers is seriously influenced.
The organosilicon sealant product has the characteristics of excellent adhesion, excellent high and low temperature resistance, excellent weather resistance and the like due to the unique molecular structure. The common organosilicon sealant for the car lamp comprises single-component dealcoholized room temperature vulcanized silicone rubber and double-component condensed room temperature vulcanized silicone rubber, is cured at room temperature after being glued, forms an elastomer after being placed for a period of time, and has excellent adhesion to the materials of the car lamp, such as ABS, PC, PP after surface treatment and the like. However, the single-component rubber needs a longer time for complete curing, and compared with the single-component dealcoholized room temperature vulcanized silicone rubber, the double-component condensed type room temperature vulcanized silicone rubber has the advantages of low volume shrinkage, deep vulcanization and the like.
At present, a plurality of patents in China research the performance of the double-component condensed type room temperature vulcanized silicone rubber. Such as CN201510304294.1 by using organosilicon low molecular ring body D with total mass content less than 0.05%3～D10The prepared two-component organosilicon sealant for the car lamp is applied to car lamp assembly, and has good effect of inhibiting the car lamp from fogging; and a fast curing two-component organosilicon sealant for the car lamp is prepared like CN201210589513.1, so as to solve the problem of fast curing high-pressure online air tightness test in a semi-sealing structure; for example, CN201811489695.9 prepares the oil-penetration-resistant two-component organosilicon sealant by using the dodecanol ester compound. However, after the two-component organosilicon sealant for the car lamp in the market is bonded with the PC-PP material for a long time, especially in an extreme environment, the bonding effect of the sealant on the PC surface cannot reach 100 percent cohesive failure, and the aging resistance and the high and low temperature resistance are not good, so that the car lamp can be seriously affectedThe anti-water leakage and anti-fogging performance of the anti-water leakage and anti-fogging device seriously harms the personal safety of drivers and passengers.
Disclosure of Invention
The high-adhesion two-component organosilicon sealant for the car lamp provided by the invention has the advantages of low volatile component, high tensile strength, good elasticity, excellent adhesion performance to PC and PP materials for the car lamp, aging resistance, humidity resistance and high and low temperature resistance.
The invention provides a high-adhesion two-component organosilicon sealant for vehicle lamps, which comprises the following components in percentage by mass (7-12): 1, a component A and a component B;
the component A comprises:
100 parts by weight of hydroxyl-terminated polydimethylsiloxane;
20-200 parts by weight of calcium carbonate;
the component B comprises:
100 parts of color paste;
5-40 parts by weight of a crosslinking agent;
3-20 parts by weight of an SC coupling agent;
1-15 parts of a catalyst;
the SC coupling agent is prepared from the following raw materials:
5-50 parts by weight of a titanate compound;
5-50 parts by weight of aminosiloxane;
50 parts by weight of absolute ethyl alcohol.
Preferably, the hydroxyl-terminated polydimethylsiloxane has the general formula shown in formula (I):
HO(SiMe2O)nh is formula (I);
in the formula (I), n is a positive integer which enables the viscosity of the hydroxyl-terminated polydimethylsiloxane to be 10-200000 mPas at 25 ℃.
Preferably, the calcium carbonate is nano active calcium carbonate, and the average particle size of the nano active calcium carbonate is less than 100 nm.
Preferably, the color paste is prepared from the following components in percentage by mass (3-5): 1 and carbon black.
Preferably, the crosslinking agent is selected from one or more of methyltrimethoxysilane, ethyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, methyltriethoxysilane, isopropyltrimethoxysilane, isobutyltrimethoxysilane, tetramethoxysilane and tetraethoxysilane.
Preferably, the preparation method of the SC coupling agent specifically comprises the following steps:
mixing titanate compounds, amino siloxane and absolute ethyl alcohol, heating to 90-150 ℃, and refluxing for 2-5 h while stirring to obtain the SC coupling agent.
Preferably, the catalyst is selected from one or more of dibutyltin dilaurate, dioctyltin dibutyrate, dibutyltin dioctanoate, dibutyltin bis (acetoxy), dibutyltin maleate and dimethyltin bis [ (neodecanoyl) oxy ].
The invention also provides a preparation method of the high-adhesion two-component organosilicon sealant for the car lamp, which comprises the following steps:
a) mixing hydroxyl-terminated polydimethylsiloxane and calcium carbonate, dehydrating, uniformly stirring, and discharging to obtain a component A;
b) mixing the color paste, the cross-linking agent, the SC coupling agent and the catalyst, uniformly stirring and discharging to obtain a component B;
c) mixing the component A obtained in the step a) with the component B obtained in the step B) to obtain the high-adhesion two-component organosilicon sealant for the car lamp;
the step a) and the step b) are not limited in order.
Preferably, the dehydration process in step a) is specifically:
heating the mixture of the hydroxyl-terminated polydimethylsiloxane and the calcium carbonate to 100-150 ℃, dehydrating for 2-4 h, and vacuumizing to complete the dehydration process.
Preferably, the mixing temperature in the step b) is 30-70 ℃, and the vacuum degree is not lower than-0.08 MPa.
The invention provides a high-adhesion two-component organosilicon sealant for vehicle lamps, which comprises the following components in percentage by mass (7-12): 1, a component A and a component B; the component A comprises: 100 parts by weight of hydroxyl-terminated polydimethylsiloxane; 20-200 parts by weight of calcium carbonate; the component B comprises: 100 parts of color paste; 5-40 parts by weight of a crosslinking agent; 3-20 parts by weight of an SC coupling agent; 1-15 parts of a catalyst; the SC coupling agent is prepared from the following raw materials: 5-50 parts by weight of a titanate compound; 5-50 parts by weight of aminosiloxane; 50 parts by weight of absolute ethyl alcohol. Compared with the prior art, the high-adhesion two-component organosilicon sealant for the car lamp provided by the invention adopts specific content components, realizes better interaction, enables the product to have low volatile components, high tensile strength and good elasticity, and has excellent adhesion performance, aging resistance, humidity resistance and high and low temperature resistance on PC and PP materials for the car lamp.
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a high-adhesion two-component organosilicon sealant for vehicle lamps, which comprises the following components in percentage by mass (7-12): 1, a component A and a component B;
the component A comprises:
100 parts by weight of hydroxyl-terminated polydimethylsiloxane;
20-200 parts by weight of calcium carbonate;
the component B comprises:
100 parts of color paste;
5-40 parts by weight of a crosslinking agent;
3-20 parts by weight of an SC coupling agent;
1-15 parts of a catalyst;
the SC coupling agent is prepared from the following raw materials:
5-50 parts by weight of a titanate compound;
5-50 parts by weight of aminosiloxane;
50 parts by weight of absolute ethyl alcohol.
In the invention, the high-adhesion two-component organosilicon sealant for the automobile lamp comprises the following components in percentage by mass (7-12): 1, preferably 10: 1.
in the invention, the component A comprises hydroxyl-terminated polydimethylsiloxane and calcium carbonate. In the present invention, the hydroxyl-terminated polydimethylsiloxane preferably has a general formula shown in formula (I):
HO(SiMe2O)nh is formula (I);
in the formula (I), n is a positive integer when the viscosity of the hydroxyl-terminated polydimethylsiloxane is 10 to 200000 mPas at 25 ℃, preferably 500 to 150000 mPas, and more preferably 1500 to 100000 mPas. In a preferred embodiment of the present invention, the hydroxyl-terminated polydimethylsiloxane is composed of 50 parts by weight of hydroxyl-terminated polydimethylsiloxane having a viscosity of 20000mPa · s and 50 parts by weight of hydroxyl-terminated polydimethylsiloxane having a viscosity of 50000mPa · s; in another preferred embodiment of the present invention, the hydroxyl-terminated polydimethylsiloxane consists of 30 parts by weight of hydroxyl-terminated polydimethylsiloxane having a viscosity of 5000mPa · s and 70 parts by weight of hydroxyl-terminated polydimethylsiloxane having a viscosity of 50000mPa · s; in another preferred embodiment of the present invention, the hydroxyl-terminated polydimethylsiloxane is composed of 60 parts by weight of hydroxyl-terminated polydimethylsiloxane having a viscosity of 1500mPa · s and 40 parts by weight of hydroxyl-terminated polydimethylsiloxane having a viscosity of 80000mPa · s.
The source of the hydroxyl-terminated polydimethylsiloxane is not particularly limited in the present invention, and may be any commercially available product known to those skilled in the art or a self-product prepared by a preparation method known to those skilled in the art. In the present invention, the a component includes 100 parts by weight of hydroxyl-terminated polydimethylsiloxane.
In the present invention, the calcium carbonate is preferably nano activated calcium carbonate; the average particle size of the nano active calcium carbonate is preferably less than 100nm, and more preferably 20nm to 80 nm. The source of the calcium carbonate is not particularly limited in the present invention, and commercially available products of the aforementioned nano activated calcium carbonate known to those skilled in the art may be used. In the invention, the component A comprises 20-200 parts by weight of calcium carbonate, preferably 130-200 parts by weight.
In the invention, the component B comprises color paste, a cross-linking agent, an SC coupling agent and a catalyst. In the invention, the color paste is preferably prepared from the following components in percentage by mass (3-5): 1, more preferably 4: 1; wherein the viscosity of the methyl silicone oil at 25 ℃ is preferably 100 to 500 mPas, and more preferably 350 mPas. The method for mixing the methyl silicone oil and the carbon black is not particularly limited, and the methyl silicone oil and the carbon black can be uniformly stirred to obtain a mixture. In the invention, the component B comprises 100 parts by weight of color paste.
In the present invention, the crosslinking agent is preferably selected from one or more of methyltrimethoxysilane, ethyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, methyltriethoxysilane, isopropyltrimethoxysilane, isobutyltrimethoxysilane, tetramethoxysilane and tetraethoxysilane, more preferably one or two of methyltrimethoxysilane, vinyltrimethoxysilane and tetraethoxysilane. In a preferred embodiment of the present invention, the crosslinking agent consists of 10 parts by weight of methyltrimethoxysilane and 5 parts by weight of vinyltrimethoxysilane; in another preferred embodiment of the present invention, the crosslinking agent consists of 5 parts by weight of tetraethoxysilane and 10 parts by weight of methyltrimethoxysilane; in another preferred embodiment of the present invention, the crosslinking agent is tetraethoxysilane 15 parts by weight.
The source of the crosslinking agent is not particularly limited in the present invention, and any commercially available or self-made product of the above-mentioned silane organic compound having three alkoxy-reactive groups, which is well known to those skilled in the art, may be used. In the invention, the component B comprises 5-40 parts by weight of a cross-linking agent, preferably 15 parts by weight.
In the invention, the SC coupling agent is prepared from the following raw materials:
5-50 parts by weight of a titanate compound;
5-50 parts by weight of aminosiloxane;
50 parts by weight of absolute ethyl alcohol.
In the present invention, the titanate-based compound preferably has Ti (OR)1)3(OR2) In which R is1Is C3-C34A hydrocarbon group (e.g., branched, straight or cyclic alkyl, alkenyl, etc.), R2Is selected from C1-C7A hydrocarbon group (e.g., branched, straight or cyclic alkyl, alkenyl, alkynyl, aryl, etc.); the titanate compound is preferably one or more of n-butyl titanate, tert-butyl titanate, tetraisopropyl titanate, diisopropyl bis (ethyl acetoacetate) titanate, acyloxy (dioctylphosphonoyl) isopropyldioleate titanate and isopropyl triisostearate titanate, and more preferably one or two of n-butyl titanate, tetraisopropyl titanate and diisopropyl bis (ethyl acetoacetate) titanate. In a preferred embodiment of the present invention, the titanate-based compound is 20 parts by weight of n-butyl titanate; in another preferred embodiment of the present invention, the titanate-based compound consists of 15 parts by weight of tetraisopropyl titanate and 25 parts by weight of n-butyl titanate; in another preferred embodiment of the present invention, the titanate-based compound is composed of 15 parts by weight of diisopropyl bis (acetoacetato) titanate and 15 parts by weight of n-butyl titanate.
The source of the titanate compound is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art may be used. In the present invention, the SC coupling agent includes 5 to 50 parts by weight of a titanate-based compound, preferably 20 to 40 parts by weight.
In the present invention, the aminosilicone is preferably selected from one or more of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltriethoxysilane, gamma-aminopropylmethyldimethoxysilane, N-N-butyl-3-aminopropyltrimethoxysilane, gamma-anilinomethyltrimethoxysilane, gamma-anilinomethyltriethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane and bis- [3- (trimethoxysilane) -propyl ] -amine, more preferably gamma-aminopropyltriethoxysilane, gamma-anilinomethyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma-N-propyltrimethoxysilane, N-N-butyl-3-aminopropyltrimethoxysilane, N-3-aminopropyltrimethoxysilane, one or two of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and bis- [3- (trimethoxy silicon) -propyl ] -amine. In a preferred embodiment of the present invention, the aminosilicone is composed of 25 parts by weight of gamma-aminopropyltriethoxysilane and 25 parts by weight of gamma-anilinomethyltriethoxysilane; in another preferred embodiment of the present invention, the aminosilicone consists of 20 parts by weight of gamma-aminopropyltriethoxysilane and 20 parts by weight of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane; in another preferred embodiment of the present invention, the aminosilicone is composed of 20 parts by weight of bis- [3- (trimethoxy silicon) -propyl ] -amine and 10 parts by weight of gamma-anilinomethyltriethoxysilane.
The source of the aminosilicone of the present invention is not particularly limited, and commercially available products or self-products known to those skilled in the art may be used. In the present invention, the SC coupling agent includes 5 to 50 parts by weight of aminosiloxane, preferably 30 to 50 parts by weight.
The source of the absolute ethanol is not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used. In the present invention, the SC coupling agent includes 50 parts by weight of absolute ethanol.
In the present invention, the preparation method of the SC coupling agent is preferably specifically:
mixing titanate compounds, amino siloxane and absolute ethyl alcohol, heating to 90-150 ℃, and refluxing for 2-5 h while stirring to obtain an SC coupling agent;
more preferably:
mixing titanate compounds, amino siloxane and absolute ethyl alcohol, heating to 100-130 ℃, and refluxing for 3-4 h while stirring to obtain the SC coupling agent. In the present invention, the titanate compound, the aminosiloxane and the anhydrous ethanol are the same as those in the above technical scheme, and are not described herein again.
In the present invention, the mixing device is preferably a three-necked round-bottom flask with a reflux condenser and a thermometer; meanwhile, the mixing device is arranged on the heating device for convenient heating.
In the invention, the component B comprises 3-20 parts by weight of SC coupling agent, preferably 5-10 parts by weight.
In the present invention, the catalyst is preferably one or more selected from the group consisting of dibutyltin dilaurate, dioctyltin dibutyrate, dibutyltin dioctanoate, dibutyltin bis (acetoxy) maleate, dibutyltin bis [ (neodecanoyl) oxy ] dimethyltin, and more preferably dibutyltin dilaurate, dibutyltin bis (acetoxy) or dimethyltin bis [ (neodecanoyl) oxy ] dimethyltin. The source of the catalyst in the present invention is not particularly limited, and commercially available products of the above-mentioned organotin catalysts known to those skilled in the art may be used. In the invention, the component B comprises 1 to 15 parts by weight of catalyst, preferably 1 to 2.5 parts by weight.
The high-adhesion two-component organosilicon sealant for the car lamp provided by the invention adopts specific content components, realizes better interaction, enables the product to have low volatile content, high tensile strength and good elasticity, and has excellent adhesion performance, aging resistance, humidity resistance and high and low temperature resistance on PC and PP materials for the car lamp.
The invention also provides a preparation method of the high-adhesion two-component organosilicon sealant for the car lamp, which comprises the following steps:
a) mixing hydroxyl-terminated polydimethylsiloxane and calcium carbonate, dehydrating, uniformly stirring, and discharging to obtain a component A;
b) mixing the color paste, the cross-linking agent, the SC coupling agent and the catalyst, uniformly stirring and discharging to obtain a component B;
c) mixing the component A obtained in the step a) with the component B obtained in the step B) to obtain the high-adhesion two-component organosilicon sealant for the car lamp;
the step a) and the step b) are not limited in order.
According to the invention, the hydroxyl-terminated polydimethylsiloxane and the calcium carbonate are mixed and dehydrated, and are uniformly stirred and discharged to obtain the component A. In the present invention, the hydroxyl-terminated polydimethylsiloxane and the calcium carbonate are the same as those in the above technical solution, and are not described herein again.
The mixing apparatus of the present invention is not particularly limited, and a high-speed dispersing planetary mixer known to those skilled in the art may be used.
In the present invention, the dehydration process is preferably specifically:
heating the mixture of the hydroxyl-terminated polydimethylsiloxane and the calcium carbonate to 100-150 ℃, dehydrating for 2-4 h, and vacuumizing to complete the dehydration process;
more preferably:
heating the mixture of the hydroxyl-terminated polydimethylsiloxane and the calcium carbonate to 120-130 ℃, dehydrating for 2.5-3.5 h, and vacuumizing to complete the dehydration process.
Meanwhile, the color paste, the cross-linking agent, the SC coupling agent and the catalyst are mixed, stirred uniformly and discharged to obtain the component B. In the invention, the color paste, the cross-linking agent, the SC coupling agent and the catalyst are the same as those in the technical scheme, and are not described again.
The mixing apparatus of the present invention is not particularly limited, and a high-speed dispersing planetary mixer known to those skilled in the art may be used.
In the present invention, the mixing temperature is preferably 30 to 70 ℃, more preferably 40 to 50 ℃; the degree of vacuum of the mixing is preferably not less than-0.08 MPa.
After the component A and the component B are respectively obtained, the component A and the component B are mixed to obtain the high-adhesion two-component organosilicon sealant for the car lamp. In the invention, the mixing of the component A and the component B actually realizes the uniform mixing of the component A and the component B for use.
The preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
The invention provides a high-adhesion two-component organosilicon sealant for vehicle lamps, which comprises the following components in percentage by mass (7-12): 1, a component A and a component B; the component A comprises: 100 parts by weight of hydroxyl-terminated polydimethylsiloxane; 20-200 parts by weight of calcium carbonate; the component B comprises: 100 parts of color paste; 5-40 parts by weight of a crosslinking agent; 3-20 parts by weight of an SC coupling agent; 1-15 parts of a catalyst; the SC coupling agent is prepared from the following raw materials: 5-50 parts by weight of a titanate compound; 5-50 parts by weight of aminosiloxane; 50 parts by weight of absolute ethyl alcohol. Compared with the prior art, the high-adhesion two-component organosilicon sealant for the car lamp provided by the invention adopts specific content components, realizes better interaction, enables the product to have low volatile components, high tensile strength and good elasticity, and has excellent adhesion performance, aging resistance, humidity resistance and high and low temperature resistance on PC and PP materials for the car lamp.
In addition, the preparation method provided by the invention is simple to operate, mild in condition and suitable for large-scale production and application.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are commercially available products or self-products.
Example 1
(1) The component A comprises: adding 50 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas, 50 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 50000 mPas and 150 parts by weight of nano active calcium carbonate with the particle size of 50nm into a high-speed dispersion planetary stirrer, heating to 125 ℃, dehydrating for 3 hours, vacuumizing, uniformly stirring and discharging to obtain the component A.
(2) And B component: firstly, adding 20 parts by weight of n-butyl titanate, 25 parts by weight of gamma-aminopropyltriethoxysilane, 25 parts by weight of gamma-anilinomethyltriethoxysilane and 50 parts by weight of absolute ethyl alcohol (analytically pure) into a three-neck round-bottom flask, heating, controlling the temperature to be between 105 and 115 ℃, and refluxing for 3 hours while stirring to obtain an SC coupling agent;
then adding 100 parts by weight of color paste, 10 parts by weight of methyltrimethoxysilane, 5 parts by weight of vinyl trimethoxysilane, 10 parts by weight of the SC coupling agent obtained in the step and 1.5 parts by weight of dibutyltin dilaurate into a high-speed dispersion planetary stirrer, and uniformly stirring and discharging under the conditions that the temperature is 40 ℃ and the vacuum degree is not lower than-0.08 MPa to obtain a component B.
(3) Mixing the component A and the component B at the room temperature in a ratio of 10: 1, and then uniformly mixing the components to obtain the high-adhesion bi-component organic silicon sealant for the car lamp.
Example 2
(1) The component A comprises: adding 30 parts by weight of terminal hydroxyl polydimethylsiloxane with the viscosity of 5000 mPas, 70 parts by weight of terminal hydroxyl polydimethylsiloxane with the viscosity of 50000 mPas and 200 parts by weight of nano active calcium carbonate with the particle size of 80nm into a high-speed dispersion planetary stirrer, heating to 125 ℃, dehydrating for 3h, vacuumizing, uniformly stirring and discharging to obtain the component A.
(2) And B component: firstly, adding 15 parts by weight of tetraisopropyl titanate, 25 parts by weight of N-butyl titanate, 20 parts by weight of gamma-aminopropyltriethoxysilane, 20 parts by weight of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and 50 parts by weight of absolute ethyl alcohol (analytically pure) into a three-neck round-bottom flask, heating, controlling the temperature to be between 105 and 115 ℃, and refluxing for 3 hours while stirring to obtain an SC coupling agent;
then adding 100 parts by weight of color paste, 5 parts by weight of tetraethoxysilane, 10 parts by weight of methyltrimethoxysilane, 5 parts by weight of SC coupling agent obtained in the step and 1 part by weight of bis (acetoxyl) dibutyltin into a high-speed dispersion planetary stirrer, and uniformly stirring and discharging under the conditions that the temperature is 40 ℃ and the vacuum degree is not lower than-0.08 MPa to obtain a component B.
(3) Mixing the component A and the component B at the room temperature in a ratio of 10: 1, and then uniformly mixing the components to obtain the high-adhesion bi-component organic silicon sealant for the car lamp.
Example 3
(1) The component A comprises: adding 60 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 1500 mPas, 40 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 80000 mPas and 130 parts by weight of nano active calcium carbonate with the particle size of 30nm into a high-speed dispersion planetary stirrer, heating to 125 ℃, dehydrating for 3h, vacuumizing, uniformly stirring and discharging to obtain the component A.
(2) And B component: firstly, adding 15 parts by weight of diisopropyl bis (ethyl acetoacetate) titanate, 15 parts by weight of n-butyl titanate, 20 parts by weight of bis- [3- (trimethoxy silicon) -propyl ] -amine, 10 parts by weight of gamma-anilinomethyl triethoxysilane and 50 parts by weight of absolute ethyl alcohol (analytically pure) into a three-neck round-bottom flask, heating, controlling the temperature to be 105-115 ℃, and refluxing for 3 hours while stirring to obtain an SC coupling agent;
then adding 100 parts by weight of color paste, 15 parts by weight of tetraethoxysilane, 5 parts by weight of the SC coupling agent obtained in the step and 2.5 parts by weight of bis [ (neodecanoyl) oxy ] dimethyltin into a high-speed dispersion planetary stirrer, and uniformly stirring and discharging under the conditions that the temperature is 40 ℃ and the vacuum degree is not lower than-0.08 MPa to obtain a component B.
(3) Mixing the component A and the component B at the room temperature in a ratio of 10: 1, and then uniformly mixing the components to obtain the high-adhesion bi-component organic silicon sealant for the car lamp.
Comparative example 1
(1) The component A comprises: adding 100 parts by weight of hydroxyl-terminated polydimethylsiloxane with viscosity of 20000 mPas and 150 parts by weight of nano active calcium carbonate with particle size of 80nm into a high-speed dispersion planetary stirrer, heating to 125 ℃, dehydrating for 3h, vacuumizing, uniformly stirring, and discharging to obtain the component A.
(2) And B component: adding 100 parts by weight of color paste, 10 parts by weight of methyltrimethoxysilane, 5 parts by weight of gamma-aminopropyltriethoxysilane and 1 part by weight of dibutyltin dilaurate into a high-speed dispersion planetary stirrer, and uniformly stirring and discharging under the conditions that the temperature is 105-115 ℃ and the vacuum degree is not lower than-0.08 MPa to obtain the component B.
(3) Mixing the component A and the component B at the room temperature in a ratio of 10: 1, and then uniformly mixing the components to obtain the high-adhesion bi-component organic silicon sealant for the car lamp.
The performances of the high-adhesion two-component silicone sealant for the vehicle lamp provided in the embodiments 1 to 3 and the comparative example 1 were tested, and the results are shown in table 1.
Table 1 data of various performances of high-adhesion two-component silicone sealant for vehicle lamp provided in examples 1-3 and comparative example 1
As can be seen from Table 1, the high-adhesion two-component organosilicon sealant for the car lamp provided by the embodiments 1-3 of the invention has better aging resistance, damp-heat resistance and high-low temperature resistance than the comparative example 1; experimental results show that the high-adhesion two-component organosilicon sealant for the car lamp provided by the embodiments 1-3 of the invention has excellent adhesion performance to PC and PP materials for the car lamp under the synergistic effect of the self-made SC coupling agent, the cross-linking agent and the catalyst, and the prepared two-component organosilicon sealant has low volatile, high tensile strength, good elasticity, aging resistance, humidity resistance and high and low temperature resistance; and the high-adhesion two-component organosilicon sealant for the car lamp prepared in the embodiment 2 has the best performance.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A high-adhesion two-component organosilicon sealant for vehicle lamps is prepared from the following components in percentage by mass: 1, component A and component B;
the component A is prepared from the following raw materials:
100 parts by weight of hydroxyl-terminated polydimethylsiloxane;
130-200 parts by weight of calcium carbonate;
the hydroxyl-terminated polydimethylsiloxane consists of 50 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000 mPas and 50 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 50000 mPas, or consists of 30 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 5000 mPas and 70 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 50000 mPas, or consists of 60 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 1500 mPas and 40 parts by weight of hydroxyl-terminated polydimethylsiloxane with the viscosity of 80000 mPas;
the component B is prepared from the following raw materials:
100 parts of color paste;
15 parts by weight of a crosslinking agent;
5-10 parts by weight of an SC coupling agent;
1-15 parts of a catalyst;
the cross-linking agent consists of 10 parts by weight of methyltrimethoxysilane and 5 parts by weight of vinyltrimethoxysilane, or consists of 5 parts by weight of tetraethoxysilane and 10 parts by weight of methyltrimethoxysilane, or is 15 parts by weight of tetraethoxysilane;
the preparation method of the SC coupling agent comprises the following steps:
adding 20 parts by weight of n-butyl titanate, 25 parts by weight of gamma-aminopropyltriethoxysilane, 25 parts by weight of gamma-anilinomethyltriethoxysilane and 50 parts by weight of absolute ethanol into a three-neck round-bottom flask, heating, controlling the temperature to be 105-115 ℃, and refluxing for 3 hours while stirring to obtain an SC coupling agent;
or adding 15 parts by weight of tetraisopropyl titanate, 25 parts by weight of N-butyl titanate, 20 parts by weight of gamma-aminopropyltriethoxysilane, 20 parts by weight of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and 50 parts by weight of absolute ethyl alcohol into a three-neck round-bottom flask, heating, controlling the temperature to be 105-115 ℃, and refluxing for 3 hours while stirring to obtain an SC coupling agent;
or adding 15 parts by weight of diisopropyl bis (ethyl acetoacetate) titanate, 15 parts by weight of n-butyl titanate, 20 parts by weight of bis- [3- (trimethoxy silicon) -propyl ] -amine, 10 parts by weight of gamma-anilinomethyl triethoxysilane and 50 parts by weight of absolute ethyl alcohol into a three-neck round-bottom flask, heating, controlling the temperature to be between 105 ℃ and 115 ℃, and refluxing for 3 hours while stirring to obtain the SC coupling agent.
2. The high adhesion two-component silicone sealant for vehicle lamps according to claim 1, wherein the calcium carbonate is nano-active calcium carbonate, and the average particle size of the nano-active calcium carbonate is less than 100 nm.
3. The high-adhesion two-component organosilicon sealant for the automobile lamp according to claim 1, wherein the color paste is prepared from (3-5) by mass: 1 and carbon black.
4. The high adhesion two-component silicone sealant for vehicle lamps according to claim 1, wherein the catalyst is selected from one or more of dibutyltin dilaurate, dioctyltin dibutyrate, dibutyltin bis (acetoxy), dibutyltin maleate and dimethyltin bis [ (neodecanoyl) oxy ] dimethyltin.
5. A preparation method of the high-adhesion two-component organosilicon sealant for the car lamp as claimed in any one of claims 1 to 4, comprising the following steps:
a) mixing hydroxyl-terminated polydimethylsiloxane and calcium carbonate, dehydrating, uniformly stirring, and discharging to obtain a component A;
b) mixing the color paste, the cross-linking agent, the SC coupling agent and the catalyst, uniformly stirring and discharging to obtain a component B;
c) mixing the component A obtained in the step a) with the component B obtained in the step B) to obtain the high-adhesion two-component organosilicon sealant for the car lamp;
the step a) and the step b) are not limited in order.
6. The preparation method according to claim 5, wherein the dehydration in step a) is specifically performed by:
heating the mixture of the hydroxyl-terminated polydimethylsiloxane and the calcium carbonate to 100-150 ℃, dehydrating for 2-4 h, and vacuumizing to complete the dehydration process.
7. The method of claim 5, wherein the mixing in step b) is carried out at a temperature of 30 ℃ to 70 ℃ under a vacuum of not less than-0.08 MPa.
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