CN111662676A - Silicone weather-resistant sealant and preparation method thereof - Google Patents

Silicone weather-resistant sealant and preparation method thereof Download PDF

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CN111662676A
CN111662676A CN202010703178.8A CN202010703178A CN111662676A CN 111662676 A CN111662676 A CN 111662676A CN 202010703178 A CN202010703178 A CN 202010703178A CN 111662676 A CN111662676 A CN 111662676A
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resistant sealant
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潘军
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • C09J183/08Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/38Polysiloxanes modified by chemical after-treatment
    • C08G77/382Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
    • C08G77/385Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing halogens
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    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
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    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
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    • C09J11/06Non-macromolecular additives organic
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    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2312/00Crosslinking

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Abstract

The invention belongs to the technical field of high polymer sealing materials, in particular to a silicone weather-resistant sealant and a preparation method thereof, which solve the problems of difficult production operation, low production efficiency, poor elasticity, elongation and weather resistance of the produced silicone sealant and the like in the prior art, and the silicone weather-resistant sealant comprises the following raw materials: dihydroxy polydimethylsiloxane, simethicone, dichloromethylpentyl silane, nano silicon dioxide, sucrose fatty acid monoester, N,2, 3-trimethyl-2-isopropyl butyramide, N-methylpyrrolidone, water and a catalyst. The preparation raw materials are simple and easy to obtain, the production process is simple to operate, the conditions are mild, the production efficiency is high, and the obtained sealant has good elasticity, elongation and weather resistance and long service life.

Description

Silicone weather-resistant sealant and preparation method thereof
Technical Field
The invention relates to the technical field of high polymer sealing materials, in particular to a silicone weather-resistant sealant and a preparation method thereof.
Background
The sealing glue is a sealing material which deforms along with the shape of the sealing surface, is not easy to flow, has certain cohesiveness, is an adhesive used for filling a configured gap to play a role in sealing, has the functions of leakage prevention, water prevention, vibration prevention, sound insulation, heat insulation and the like, and is widely used for sealing buildings, transportation, electronic instruments and parts. The silicone sealant is a paste prepared by mixing polydimethylsiloxane as a main raw material, a cross-linking agent, a filler, a plasticizer, a coupling agent and a catalyst in a vacuum state, and is cured to form the elastic silicone rubber by reacting with water in the air at room temperature.
In recent years, with the continuous improvement of living standard of people, the decoration and fitment of families, hotels, office buildings and public places are rapidly raised, and huge market demands are provided for various building materials, the building sealant is one of the building sealants, particularly the building silicone sealant, has the highest proportion in various building sealants, has the market occupancy rate of more than 80 percent, and is widely used for the bonding and sealing of expansion joints of high-rise buildings, the bonding and sealing of glass curtain walls, stone curtain walls and synthetic material curtain walls, and the waterproof sealing of joints among doors, windows, kitchens, bathrooms and washrooms, tables, walls and furniture. The silicone sealant is convenient to use, can be vulcanized at room temperature, has good bonding performance to most of base materials, is a bonding and sealing material popular with people, and has great market prospect. Then, the existing silicone sealant generally has the problems of large addition amount of additives or fillers and the like, large difficulty in uniform dispersion in the production process, difficult production operation, low production efficiency, poor elasticity, elongation and weather resistance of the produced silicone sealant and the like. Based on the statement, the invention provides a silicone weather-resistant sealant and a preparation method thereof.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, the production operation of a silicone sealant is difficult, the production efficiency is low, and the elasticity, the elongation and the weather resistance of the produced silicone sealant are poor, and the like, and provides a silicone weather-resistant sealant and a preparation method thereof.
The silicone weather-resistant sealant comprises the following raw materials in parts by weight: 70-90 parts of dihydroxy polydimethylsiloxane, 30-50 parts of simethicone, 10-18 parts of dichloromethylpentyl silane, 20-30 parts of nano silicon dioxide, 3-15 parts of sucrose fatty acid monoester, 1-3 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 4-7 parts of N-methylpyrrolidone, 30-50 parts of water and 1-3 parts of catalyst.
Preferably, the silicone weather-resistant sealant comprises the following raw materials in parts by weight: 75-85 parts of dihydroxy polydimethylsiloxane, 35-45 parts of simethicone, 12-16 parts of dichloromethylpentyl silane, 22-28 parts of nano silicon dioxide, 4.5-12.5 parts of sucrose fatty acid monoester, 1.5-2.5 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 5-6 parts of N-methyl pyrrolidone, 35-45 parts of water and 1.5-2.5 parts of catalyst.
Preferably, the mass ratio of the sucrose fatty acid monoester to the N,2, 3-trimethyl-2-isopropyl butanamide is 3-5: 1.
Preferably, the silicone weather-resistant sealant comprises the following raw materials in parts by weight: 80 parts of dihydroxy polydimethylsiloxane, 40 parts of simethicone, 14 parts of dichloromethylpentyl silane, 25 parts of nano silicon dioxide, 8 parts of sucrose fatty acid monoester, 2 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 5.5 parts of N-methylpyrrolidone, 40 parts of water and 2 parts of catalyst.
Preferably, the catalyst is prepared by compounding spongy platinum, rhodium powder, cellulose acetate phthalate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3-4:2-7: 11; the specific preparation method comprises the following steps: a. calcining the spongy platinum and rhodium powder for 2-3h at the temperature of 900-1200 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing the 1, 4-butyrolactone and ethanol at the temperature of 50-70 ℃, adding the mixed powder and the phthalic acid cellulose acetate, heating to 80-90 ℃, performing ultrasonic dispersion for 10-20min, and performing vacuum drying at the temperature of 100-120 ℃ to obtain the catalyst.
The invention also provides a preparation method of the silicone weather-resistant sealant, which comprises the following steps:
s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40-46 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15-25min, heating to 50-58 ℃, adding dichloromethylpentyl silane, continuing stirring and mixing for 20-30min, and cooling to room temperature to obtain a base mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at 70-90 ℃ according to the specific gravity, adding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 10-20min, cooling to 40-50 ℃, adding nano silicon dioxide, and homogenizing for 20-30min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano-silica prepared in the step S2 into the basic mixture prepared in the step S1, heating to 60-90 ℃, adding the catalyst with the specific gravity, stirring and mixing at the rotating speed of 450-550r/min for 20-40min, and uniformly dispersing to obtain the silicone weather-resistant sealant.
The silicone weather-resistant sealant provided by the invention has the following beneficial effects:
1. the method utilizes dichloromethyl amyl silane to perform surface function modification on dihydroxy polydimethylsiloxane and dimethyl silicone oil, improves the binding capacity of siloxane chemical bonds, and obtains a basic mixture; carrying out surface coating treatment on the nano-silica by synergistic compounding of sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide to obtain modified nano-silica with high dispersibility and compatibility; and finally, under the action of a catalyst, mixing the basic mixture and the modified nano-silica to prepare the silicone weather-resistant sealant.
2. The sucrose fatty acid monoester and the N,2, 3-trimethyl-2-isopropyl butanamide are used for synergistic compounding, the components are dissolved and dispersed in N-methyl pyrrolidone and water, and finally the nano silicon dioxide is modified, so that the obtained modified nano silicon dioxide has high dispersibility and compatibility, and further can obtain high crosslinking density and enhanced reinforcing effect.
3. According to the invention, the catalyst is prepared by compounding spongy platinum, rhodium powder, phthalic acid cellulose acetate, 1, 4-butyrolactone and ethanol, so that the catalyst can effectively catalyze the reaction, the crosslinking rate of the sealant is increased, and the surface drying time and curing time of the silicone sealant are further obviously shortened.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 70 parts of dihydroxy polydimethylsiloxane, 30 parts of dimethyl silicone oil, 10 parts of dichloromethylpentyl silane, 20 parts of nano silicon dioxide, 3 parts of sucrose fatty acid monoester, 1 part of N,2, 3-trimethyl-2-isopropyl butanamide, 4 parts of N-methyl pyrrolidone, 30 parts of water and 1 part of catalyst; the catalyst is prepared by compounding spongy platinum, rhodium powder, phthalic acid cellulose acetate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3:2: 11;
the specific preparation method of the catalyst comprises the following steps: a. calcining the spongy platinum and rhodium powder for 2 hours at the temperature of 900 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing 1, 4-butyrolactone and ethanol at the temperature of 50 ℃, adding the mixed powder and phthalic acid cellulose acetate, heating to 80 ℃, performing ultrasonic dispersion for 10min, and performing vacuum drying at the temperature of 100 ℃ to obtain the catalyst.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps: s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15min, heating to 50 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 20min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at 70 ℃ according to the specific gravity, adding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 10min, cooling to 40 ℃, adding nano silicon dioxide, and homogenizing for 20min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano silicon dioxide prepared in the step S2 into the basic mixture prepared in the step S1, heating to 60 ℃, adding the catalyst with the specific gravity, stirring and mixing for 20min at the rotating speed of 450r/min, and uniformly dispersing to obtain the silicone weather-resistant sealant.
Example two
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 80 parts of dihydroxy polydimethylsiloxane, 40 parts of simethicone, 14 parts of dichloromethylpentyl silane, 25 parts of nano silicon dioxide, 8 parts of sucrose fatty acid monoester, 2 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 5.5 parts of N-methylpyrrolidone, 40 parts of water and 2 parts of catalyst; wherein the catalyst is prepared by compounding spongy platinum, rhodium powder, cellulose acetate phthalate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3.5:4.5: 11;
the specific preparation method of the catalyst comprises the following steps: a. calcining the spongy platinum and rhodium powder for 2.5 hours at 1050 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing the 1, 4-butyrolactone and ethanol at the temperature of 60 ℃, adding the mixed powder and the phthalic acid cellulose acetate, heating to 85 ℃, ultrasonically dispersing for 15min, and drying in vacuum at the temperature of 110 ℃ to obtain the catalyst.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps: s1, preparing a basic mixture: according to the specific gravity, at the temperature of 43 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 20min, heating to 54 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 25min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at the temperature of 80 ℃ according to the specific gravity, adding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 15min, cooling to 45 ℃, adding nano silicon dioxide, and homogenizing for 25min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano silicon dioxide prepared in the step S2 into the basic mixture prepared in the step S1, heating to 75 ℃, adding the catalyst with the specific gravity, stirring and mixing for 30min at the rotating speed of 500r/min, and dispersing uniformly to obtain the silicone weather-resistant sealant.
EXAMPLE III
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 90 parts of dihydroxy polydimethylsiloxane, 50 parts of simethicone, 18 parts of dichloromethylpentyl silane, 30 parts of nano silicon dioxide, 15 parts of sucrose fatty acid monoester, 3 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 7 parts of N-methylpyrrolidone, 50 parts of water and 3 parts of catalyst; wherein the catalyst is prepared by compounding spongy platinum, rhodium powder, phthalic acid cellulose acetate, 1, 4-butyrolactone and ethanol according to the mass ratio of 1:1:4:7: 11;
the specific preparation method of the catalyst comprises the following steps: a. calcining the spongy platinum and rhodium powder for 3 hours at 1200 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing 1, 4-butyrolactone and ethanol at the temperature of 70 ℃, adding the mixed powder and the phthalic acid cellulose acetate, heating to 90 ℃, ultrasonically dispersing for 20min, and drying in vacuum at the temperature of 120 ℃ to obtain the catalyst.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps: s1, preparing a basic mixture: according to the specific gravity, at the temperature of 46 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 25min, heating to 58 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 30min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at the temperature of 90 ℃ according to the specific gravity, adding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 20min, cooling to 50 ℃, adding nano silicon dioxide, and homogenizing for 30min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano silicon dioxide prepared in the step S2 into the basic mixture prepared in the step S1, heating to 90 ℃, adding the catalyst with the specific gravity, stirring and mixing for 40min at the rotating speed of 550r/min, and dispersing uniformly to obtain the silicone weather-resistant sealant.
Comparative example 1
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 70 parts of dihydroxy polydimethylsiloxane, 30 parts of dimethyl silicone oil, 10 parts of dichloromethylpentyl silane, 20 parts of nano silicon dioxide, 3 parts of sucrose fatty acid monoester, 1 part of N,2, 3-trimethyl-2-isopropyl butanamide, 4 parts of N-methyl pyrrolidone, 30 parts of water and 1 part of catalyst; wherein the catalyst is dibutyltin dilaurate.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps: s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15min, heating to 50 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 20min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at 70 ℃ according to the specific gravity, adding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 10min, cooling to 40 ℃, adding nano silicon dioxide, and homogenizing for 20min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano silicon dioxide prepared in the step S2 into the basic mixture prepared in the step S1, heating to 60 ℃, adding the catalyst with the specific gravity, stirring and mixing for 20min at the rotating speed of 450r/min, and uniformly dispersing to obtain the silicone weather-resistant sealant.
Comparative example No. two
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 70 parts of dihydroxy polydimethylsiloxane, 30 parts of dimethyl silicone oil, 10 parts of dichloromethylpentyl silane, 20 parts of nano silicon dioxide, 3 parts of sucrose fatty acid monoester, 1 part of N,2, 3-trimethyl-2-isopropyl butanamide, 4 parts of N-methyl pyrrolidone, 30 parts of water and 1 part of catalyst; the catalyst is prepared by compounding spongy platinum, rhodium powder, phthalic acid cellulose acetate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3:2: 11;
the specific preparation method of the catalyst comprises the following steps: a. calcining the spongy platinum and rhodium powder for 2 hours at the temperature of 900 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing 1, 4-butyrolactone and ethanol at the temperature of 50 ℃, adding the mixed powder and phthalic acid cellulose acetate, heating to 80 ℃, performing ultrasonic dispersion for 10min, and performing vacuum drying at the temperature of 100 ℃ to obtain the catalyst.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps: s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15min, heating to 50 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 20min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of the silicone weather-resistant sealant: under the vacuum condition, sequentially adding the N-methyl pyrrolidone, the water, the sucrose fatty acid monoester, the N,2, 3-trimethyl-2-isopropyl butanamide and the nano silicon dioxide with the specific gravity into the basic mixture prepared in the step S1, heating to 60 ℃, adding the catalyst with the specific gravity, stirring and mixing at the rotating speed of 450r/min for 20min, and dispersing uniformly to obtain the silicone weather-resistant sealant.
Comparative example No. three
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 70 parts of dihydroxy polydimethylsiloxane, 30 parts of dimethyl silicone oil, 10 parts of dichloromethyl amyl silane, 20 parts of nano silicon dioxide, 4 parts of sucrose fatty acid monoester, 4 parts of N-methyl pyrrolidone, 30 parts of water and 1 part of catalyst; the catalyst is prepared by compounding spongy platinum, rhodium powder, phthalic acid cellulose acetate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3:2: 11;
the specific preparation method of the catalyst comprises the following steps: a. calcining the spongy platinum and rhodium powder for 2 hours at the temperature of 900 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing 1, 4-butyrolactone and ethanol at the temperature of 50 ℃, adding the mixed powder and phthalic acid cellulose acetate, heating to 80 ℃, performing ultrasonic dispersion for 10min, and performing vacuum drying at the temperature of 100 ℃ to obtain the catalyst.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps: s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15min, heating to 50 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 20min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at 70 ℃ according to the specific gravity, adding sucrose fatty acid monoester, stirring for 10min, cooling to 40 ℃, adding nano silicon dioxide, and homogenizing for 20min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano silicon dioxide prepared in the step S2 into the basic mixture prepared in the step S1, heating to 60 ℃, adding the catalyst with the specific gravity, stirring and mixing for 20min at the rotating speed of 450r/min, and uniformly dispersing to obtain the silicone weather-resistant sealant.
Comparative example No. four
The invention provides a silicone weather-resistant sealant which comprises the following raw materials in parts by weight: 70 parts of dihydroxy polydimethylsiloxane, 30 parts of simethicone, 10 parts of dichloromethylpentyl silane, 20 parts of nano silicon dioxide, 4 parts of N,2, 3-trimethyl-2-isopropyl butyramide, 4 parts of N-methyl pyrrolidone, 30 parts of water and 1 part of catalyst; the catalyst is prepared by compounding spongy platinum, rhodium powder, phthalic acid cellulose acetate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3:2: 11;
the specific preparation method of the catalyst comprises the following steps: a. calcining the spongy platinum and rhodium powder for 2 hours at the temperature of 900 ℃ under the condition of nitrogen according to the proportion, cooling the calcined product, and then carrying out ball milling to obtain mixed powder; b. stirring and mixing 1, 4-butyrolactone and ethanol at the temperature of 50 ℃, adding the mixed powder and phthalic acid cellulose acetate, heating to 80 ℃, performing ultrasonic dispersion for 10min, and performing vacuum drying at the temperature of 100 ℃ to obtain the catalyst.
The invention provides a preparation method of a silicone weather-resistant sealant, which comprises the following steps:
s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15min, heating to 50 ℃, adding dichloromethyl amyl silane, continuing stirring and mixing for 20min, and cooling to room temperature to obtain a basic mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at 70 ℃ according to the specific gravity, adding N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 10min, cooling to 40 ℃, adding nano silicon dioxide, and homogenizing for 20min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano silicon dioxide prepared in the step S2 into the basic mixture prepared in the step S1, heating to 60 ℃, adding the catalyst with the specific gravity, stirring and mixing for 20min at the rotating speed of 450r/min, and uniformly dispersing to obtain the silicone weather-resistant sealant.
The performance of the silicone weather-resistant sealants prepared in examples one-three and comparative examples one-four were respectively tested under the premise that other conditions were kept unchanged, and the following results were obtained:
table 1:
Figure BDA0002593651370000121
note: in table 1, after soaking, the concrete means that the adhesive strength test is carried out immediately after soaking in water under standard conditions for 180 hours; after soaking and illumination, the method specifically means that the material is put into a water-ultraviolet radiation test box to be soaked and illuminated for 300 hours (at the temperature of 40 ℃) and then is immediately subjected to bonding strength test.
From the data in table 1, it can be seen that: the silicone weather-resistant sealant prepared in the first to third embodiments of the invention has excellent comprehensive performance.
From the first example and the first comparative example, it can be seen that: compared with the traditional catalyst (dibutyltin dilaurate), the catalyst prepared by the invention has high catalytic efficiency, is environment-friendly and pollution-free, and the surface drying time and the curing time of the sealant prepared by the catalyst are short.
As can be seen from the first embodiment and the second to fourth comparative examples, the modified nano-silica prepared by modifying nano-silica by compounding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide has better performance than the unmodified nano-silica than the modified nano-silica prepared by modifying nano-silica by only sucrose fatty acid monoester or N,2, 3-trimethyl-2-isopropyl butanamide alone.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (6)

1. The silicone weather-resistant sealant is characterized by comprising the following raw materials in parts by weight: 70-90 parts of dihydroxy polydimethylsiloxane, 30-50 parts of simethicone, 10-18 parts of dichloromethylpentyl silane, 20-30 parts of nano silicon dioxide, 3-15 parts of sucrose fatty acid monoester, 1-3 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 4-7 parts of N-methylpyrrolidone, 30-50 parts of water and 1-3 parts of catalyst.
2. The silicone weather-resistant sealant as claimed in claim 1, which is characterized by comprising the following raw materials in parts by weight: 75-85 parts of dihydroxy polydimethylsiloxane, 35-45 parts of simethicone, 12-16 parts of dichloromethylpentyl silane, 22-28 parts of nano silicon dioxide, 4.5-12.5 parts of sucrose fatty acid monoester, 1.5-2.5 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 5-6 parts of N-methyl pyrrolidone, 35-45 parts of water and 1.5-2.5 parts of catalyst.
3. The silicone weather resistant sealant according to claim 1 or 2, characterized in that the mass ratio of sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide is 3-5: 1.
4. The silicone weather-resistant sealant as claimed in claim 1 or 2, which is characterized by comprising the following raw materials in parts by weight: 80 parts of dihydroxy polydimethylsiloxane, 40 parts of simethicone, 14 parts of dichloromethylpentyl silane, 25 parts of nano silicon dioxide, 8 parts of sucrose fatty acid monoester, 2 parts of N,2, 3-trimethyl-2-isopropyl butanamide, 5.5 parts of N-methylpyrrolidone, 40 parts of water and 2 parts of catalyst.
5. The silicone weather-resistant sealant as claimed in claim 4, wherein the catalyst is prepared by compounding spongy platinum, rhodium powder, cellulose acetate phthalate, 1, 4-butyrolactone and ethanol in a mass ratio of 1:1:3-4:2-7: 11.
6. The method for preparing the silicone weather resistant sealant according to any one of claims 1 to 5, characterized by comprising the following steps:
s1, preparing a basic mixture: according to the specific gravity, at the temperature of 40-46 ℃, stirring and mixing dihydroxy polydimethylsiloxane and simethicone for 15-25min, heating to 50-58 ℃, adding dichloromethylpentyl silane, continuing stirring and mixing for 20-30min, and cooling to room temperature to obtain a base mixture;
s2, preparation of modified nano silicon dioxide: dissolving N-methyl pyrrolidone in water at 70-90 ℃ according to the specific gravity, adding sucrose fatty acid monoester and N,2, 3-trimethyl-2-isopropyl butanamide, stirring for 10-20min, cooling to 40-50 ℃, adding nano silicon dioxide, and homogenizing for 20-30min to obtain modified nano silicon dioxide;
s3, preparation of the silicone weather-resistant sealant: and (3) under the vacuum condition, adding the modified nano-silica prepared in the step S2 into the basic mixture prepared in the step S1, heating to 60-90 ℃, adding the catalyst with the specific gravity, stirring and mixing at the rotating speed of 450-550r/min for 20-40min, and uniformly dispersing to obtain the silicone weather-resistant sealant.
CN202010703178.8A 2020-07-21 2020-07-21 Silicone weather-resistant sealant and preparation method thereof Pending CN111662676A (en)

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