CN110669471A - Environment-friendly high-strength organic silicon adhesive and preparation method thereof - Google Patents
Environment-friendly high-strength organic silicon adhesive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses an environment-friendly high-strength organic silicon adhesive and a preparation method thereof, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of a tackifier, 3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent; according to the invention, the alpha-aminosilane coupling agent and the porous nano-silica material are introduced into the formula, and effective formula blending is obtained through experiments, so that the defects of low bonding strength and serious environmental pollution of the dealcoholized organosilicon adhesive in the existing market are solved.
Description
Technical Field
The invention relates to the technical field of organosilicon sealants, in particular to an environment-friendly high-strength organosilicon adhesive and a preparation method thereof.
Background
The room temperature vulcanized organic silicon adhesive is developed in the sixties of the last century, can be crosslinked to form an elastomer with a three-dimensional network structure mainly by moisture in air, and has the characteristics of simple manufacture and convenient construction. Currently, single-component room temperature curing silicone adhesives can be classified into a deacetylated type, a ketoxime type, a dealcoholized type, an amide-removed type and an acetone-removed type according to different byproducts released in a vulcanization crosslinking process. Among them, the deacetylated silicone rubber has excellent physical properties, adhesion and vulcanization properties, and has disadvantages of releasing acetic acid during vulcanization, having acid odor, being corrosive to metals, and having a limited application range. The deketoxime type silicon rubber has the characteristics of moderate sulfuration and small taste of ketoxime which is a byproduct released in the sulfuration process, but is corrosive to copper-zinc metal and PC materials, and is easy to crack in the sulfuration process. The acetone-removing type silicone rubber has excellent performance but high price. The dealcoholized organosilicon adhesive releases ethanol in the vulcanization process, has no toxicity, no pungent smell, no cracking phenomenon and no corrosion to base materials. Therefore, the dealcoholized silicone adhesive is widely used as an important adhesive and sealing material in the fields of office devices, electronic and electric appliances, automobile production, civil engineering and construction, and the like. The silicone adhesive is the fastest developing silicone adhesive with the largest dosage in recent years.
However, most dealcoholized organosilicon adhesives in the current market still have some defects, such as low bonding strength, basically less than 2MPa of shear strength, and insufficient bonding force to aluminum materials, stainless steel, PC materials and other substrates; in the curing process, catalysts containing heavy metals such as metal salts, organic tin compounds, titanium complexes and the like are required to be added, so that the environment is seriously polluted, and the application range of the dealcoholized organosilicon adhesive is limited; the present invention solves such problems.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide an environment-friendly high-strength organic silicon adhesive and a preparation method thereof.
In order to achieve the above object, the present invention adopts the following technical solutions:
a kind ofThe environment-friendly high-strength organic silicon adhesive comprises the following components in parts by weight: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of a tackifier, 3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent.
The formula of the environment-friendly high-strength organic silicon adhesive comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 5-20 parts of simethicone, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, 10-20 parts of porous nano silicon dioxide, 3-7 parts of tackifier, 3-6 parts of alpha-aminosilane coupling agent, 4-10 parts of cross-linking agent and 1-10 parts of auxiliary agent.
In the environment-friendly high-strength organic silicon adhesive, the inorganic filler comprises: hydrophobic silicon dioxide by a precipitation method, nano active calcium carbonate treated by hard fatty acid, light calcium carbonate treated by hard fatty acid, heavy calcium carbonate treated by hard fatty acid, titanium dioxide, nano zinc oxide and active silicon micropowder.
In the environment-friendly high-strength organic silicon adhesive, the flame retardant comprises: aluminum hydroxide, magnesium hydroxide, antimony trioxide, zinc borate, melamine, diphosphonate and ammonium polyphosphate.
In the environment-friendly high-strength silicone adhesive, the tackifier comprises: gamma-methacryloxypropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, vinyltris (. beta. -methoxyethoxy) silane, bis (. gamma. -trimethoxysilylpropyl) amine.
In the above-mentioned environment-friendly high-strength silicone adhesive, the α -aminosilane coupling agent comprises: alpha-diethylaminomethyltriethoxysilane, alpha-aminoethylaminomethyltrimethoxysilane, alpha-divinyltriaminomethyltrimethoxysilane.
In the environment-friendly high-strength silicone adhesive, the crosslinking agent comprises: methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane, tetraethoxysilane, anilinomethyltriethoxysilane, dichloromethyltriethoxysilane.
In the environment-friendly high-strength organic silicon adhesive, the auxiliary agent comprises: preservative, anti-yellowing agent, antioxidant and hydroxyl scavenger.
The preparation method of the environment-friendly high-strength organic silicon adhesive comprises the following steps:
preparing materials according to a formula, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of a tackifier, 3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent;
drying and dehydrating the nano porous silica and the inorganic filler at the temperature of 150-180 ℃ for 2-3 hours respectively;
adding alpha, omega-dihydroxy polydimethylsiloxane, simethicone, inorganic filler, flame retardant, nano porous silicon dioxide and tackifier into a high-speed planetary dispersion machine, fully stirring for 60-180 minutes at the temperature of 120-;
after the base material is cooled to room temperature, adding the cross-linking agent and the alpha-aminosilane coupling agent into a high-speed planetary dispersing machine filled with the base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive.
The preparation method of the environment-friendly high-strength organic silicon adhesive comprises the following steps:
preparing materials according to a formula, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of tackifier, 3-6 parts of alpha-aminosilane coupling agent, 4-10 parts of cross-linking agent and 1-10 parts of auxiliary agent;
drying and dehydrating the nano porous silica and the inorganic filler at the temperature of 150-180 ℃ for 2-3 hours respectively;
adding alpha, omega-dihydroxy polydimethylsiloxane, simethicone, inorganic filler, flame retardant, nano porous silicon dioxide, tackifier and auxiliary agent into a high-speed planetary dispersion machine, fully stirring for 60-180 minutes at the temperature of 120-;
after the base material is cooled to room temperature, adding the cross-linking agent and the alpha-aminosilane coupling agent into a high-speed planetary dispersing machine filled with the base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive.
The invention has the advantages that:
according to the organic silicon adhesive prepared by the implementation of the invention, the alpha-aminosilane coupling agent is used as a crosslinking catalyst, so that the prepared organic silicon adhesive has high curing speed, good bonding performance to a base material, no heavy metal catalyst and obvious environment-friendly effect, and small molecular alcohol substances released in the curing process have no corrosion to the base material;
the nano porous silicon dioxide is used as a reinforcing material, so that the mechanical strength of the silicone rubber is greatly improved, and the shear strength of the organic silicon adhesive prepared by the method can reach more than 3.5 MPa;
the invention obtains the mass part range capable of achieving the effective effect through experiments, so that the organic silicon adhesive can be widely applied to sealing and bonding of electronic components and other non-structural sealing and bonding.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The first formula is an environment-friendly high-strength organic silicon adhesive, and the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, and tackification3-7 parts of an agent, 3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent.
The preparation method of the formula I comprises the following steps:
preparing materials according to a formula, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of a tackifier, 3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent;
drying and dehydrating the nano porous silica and the inorganic filler at the temperature of 150-180 ℃ for 2-3 hours respectively;
adding alpha, omega-dihydroxy polydimethylsiloxane, simethicone, inorganic filler, flame retardant, nano porous silicon dioxide and tackifier into a high-speed planetary dispersion machine, fully stirring for 60-180 minutes at the temperature of 120-;
after the base material is cooled to room temperature, adding the cross-linking agent and the alpha-aminosilane coupling agent into a high-speed planetary dispersing machine filled with the base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive.
And the formula II is an environment-friendly high-strength organic silicon adhesive, and comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 5-20 parts of simethicone, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, 10-20 parts of porous nano silicon dioxide, 3-7 parts of tackifier, 3-6 parts of alpha-aminosilane coupling agent, 4-10 parts of cross-linking agent and 1-10 parts of auxiliary agent.
The preparation method of the formula II comprises the following steps:
preparing materials according to a formula, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, and tackification3-7 parts of an agent, 3-6 parts of an alpha-aminosilane coupling agent, 4-10 parts of a cross-linking agent and 1-10 parts of an auxiliary agent;
drying and dehydrating the nano porous silica and the inorganic filler at the temperature of 150-180 ℃ for 2-3 hours respectively;
adding alpha, omega-dihydroxy polydimethylsiloxane, simethicone, inorganic filler, flame retardant, nano porous silicon dioxide, tackifier and auxiliary agent into a high-speed planetary dispersion machine, fully stirring for 60-180 minutes at the temperature of 120-;
after the base material is cooled to room temperature, adding the cross-linking agent and the alpha-aminosilane coupling agent into a high-speed planetary dispersing machine filled with the base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive.
Compared with the formula II, the formula I is added with the auxiliary agents, and the auxiliary agents comprise: preservative, anti-yellowing agent, antioxidant and hydroxyl scavenger.
As an example, the inorganic filler includes: hydrophobic silicon dioxide by a precipitation method, nano active calcium carbonate treated by hard fatty acid, light calcium carbonate treated by hard fatty acid, heavy calcium carbonate treated by hard fatty acid, titanium dioxide, nano zinc oxide and active silicon micropowder. It should be noted that: inclusion herein refers to a combination of one or more of these.
As an example, the flame retardant includes: aluminum hydroxide, magnesium hydroxide, antimony trioxide, zinc borate, melamine, diphosphonate and ammonium polyphosphate. It should be noted that: inclusion herein refers to a combination of one or more of these.
As an example, the tackifier includes: gamma-methacryloxypropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, vinyltris (. beta. -methoxyethoxy) silane, bis (. gamma. -trimethoxysilylpropyl) amine. It should be noted that: inclusion herein refers to a combination of one or more of these.
As an example, an alpha-aminosilane coupling agent includes: alpha-diethylaminomethyltriethoxysilane, alpha-aminoethylaminomethyltrimethoxysilane, alpha-divinyltriaminomethyltrimethoxysilane. It should be noted that: inclusion herein refers to a combination of one or more of these.
As an example, the crosslinking agent includes: methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane, tetraethoxysilane, anilinomethyltriethoxysilane, dichloromethyltriethoxysilane. It should be noted that: inclusion herein refers to a combination of one or more of these.
And (3) a verification experiment part:
performance verification experiments were performed using samples obtained in the following examples;
example 1:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 5g of simethicone, 60g of inorganic filler (50 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 10g of flame retardant (5 g of aluminum hydroxide and 5g of magnesium hydroxide), 10g of porous nano silicon dioxide, 3g of tackifier (gamma-aminopropyltriethoxysilane), 3g of alpha-aminosilane coupling agent (2 g of alpha-diethylaminomethyl triethoxysilane and 1g of alpha-aminoethyl aminomethyl trimethoxysilane), 4g of crosslinking agent (methyl trimethoxysilane and 2g of vinyl trimethoxysilane) and 1g of auxiliary agent (hydroxyl scavenging agent);
the specific surface area is 200cm3Drying and dehydrating the porous nano silicon dioxide and the nano active calcium carbonate treated by the stearic acid at 160 ℃ for 2 to 3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide, gamma-aminopropyltriethoxysilane and hydroxyl scavenger into a vacuum mixer, fully mixing for 150 minutes at 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing 2g of methyltrimethoxysilane, 2g of vinyltrimethoxysilane, 2g of alpha-diethylaminomethyltriethoxysilane and 2g of alpha-aminoethyl aminomethylAdding 1g of trimethoxy silane into a high-speed planetary dispersion machine filled with base materials, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 2:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 20g of simethicone, 120g of inorganic filler (100 g of nano active calcium carbonate, 10g of titanium dioxide with the particle size of 0.08 micrometer, 10g of nano zinc oxide), 30g of flame retardant (20 g of aluminum hydroxide and 10g of magnesium hydroxide), 20g of porous nano silicon dioxide, 7g of tackifier (gamma-aminopropyltriethoxysilane), 6g of alpha-aminosilane coupling agent (3 g of alpha-diethylaminomethyl triethoxysilane and 3g of alpha-aminoethylaminomethyl trimethoxysilane), 5g of crosslinking agent (methyl trimethoxysilane, 5g of vinyl trimethoxysilane) and 10g of auxiliary agent (hydroxyl scavenging agent);
the specific surface area is 200cm3Drying and dehydrating the porous nano silicon dioxide and the nano active calcium carbonate treated by the stearic acid at 160 ℃ for 2 to 3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide, gamma-aminopropyltriethoxysilane and hydroxyl scavenger into a vacuum mixer, fully mixing for 150 minutes at 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 3:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 13g of simethicone, 90g of inorganic filler (80 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 15g of flame retardant (10 g of aluminum hydroxide and 5g of magnesium hydroxide), 15g of porous nano silicon dioxide, 5g of tackifier (gamma-aminopropyltriethoxysilane), 2.5g of alpha-aminosilane coupling agent (alpha-diethylaminomethyl triethoxysilane and 2g of alpha-aminoethylaminomethyl trimethoxysilane), 4.5g of crosslinking agent (methyl trimethoxysilane, 3g of vinyl trimethoxysilane) and 5g of auxiliary agent (hydroxyl scavenging agent);
the specific surface area is 200cm3Drying and dehydrating the porous nano silicon dioxide and the nano active calcium carbonate treated by the stearic acid at 160 ℃ for 2 to 3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide, gamma-aminopropyltriethoxysilane and hydroxyl scavenger into a vacuum mixer, fully mixing for 150 minutes at 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 4
The formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 5g of simethicone, 80g of inorganic filler (70 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 30g of flame retardant (20 g of aluminum hydroxide and 10g of magnesium hydroxide), 15g of porous nano silicon dioxide, 4g of tackifier (gamma-aminopropyltriethoxysilane), 6g of alpha-aminosilane coupling agent (alpha-diethylaminomethyl triethoxysilane and alpha-aminoethylaminomethyl trimethoxysilane), 8g of crosslinking agent (methyl trimethoxysilane and vinyl trimethoxysilane) and 3g of auxiliary agent (hydroxyl scavenging agent);
the specific surface area is 350cm3Porous nanosilica in gDrying and dehydrating the nano active calcium carbonate treated by the hard fatty acid for 2-3 hours at 160 ℃; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500 mPa.S, dimethyl silicone oil with the viscosity of 100 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide, gamma-aminopropyltriethoxysilane and hydroxyl scavenger into a vacuum mixer, fully mixing for 150 minutes at 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 5
The formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 18g of simethicone, 100g of inorganic filler (90 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 30g of flame retardant (20 g of aluminum hydroxide and 10g of magnesium hydroxide), 15g of porous nano silicon dioxide, 5g of tackifier (gamma-aminopropyltriethoxysilane), 6g of alpha-aminosilane coupling agent (alpha-diethylaminomethyl triethoxysilane and alpha-aminoethylaminomethyl trimethoxysilane), 8g of crosslinking agent (methyl trimethoxysilane and vinyl trimethoxysilane) and 3g of auxiliary agent (hydroxyl scavenging agent);
the specific surface area is 350cm3Drying and dehydrating the porous nano silicon dioxide and the nano active calcium carbonate treated by the stearic acid at 160 ℃ for 2 to 3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000 mPas, dimethyl silicone oil with viscosity of 350 mPas, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide, gamma-aminopropyltriethoxysilane and hydroxyl scavenger into a vacuum mixer, fully stirring for 150 minutes at 150 ℃ and vacuum degree of 0.06-0.1MPa, and cooling; to be treatedCooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 6: (examples 6-8 are formulation one, formulation without auxiliaries)
The formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 5g of simethicone, 60g of inorganic filler (50 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 10g of flame retardant (5 g of aluminum hydroxide and 5g of magnesium hydroxide), 10g of porous nano silicon dioxide, 3g of tackifier (gamma-aminopropyltriethoxysilane), 3g of alpha-aminosilane coupling agent (2 g of alpha-diethylaminomethyl triethoxysilane and 1g of alpha-aminoethylaminomethyl trimethoxysilane), and 4g of crosslinking agent (2 g of methyl trimethoxysilane and 2g of vinyl trimethoxysilane);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing 2g of methyltrimethoxysilane, 2g of vinyltrimethoxysilane, 2g of alpha-diethylaminomethyltriethoxysilane and 1g of alpha-aminoethyl aminomethyl trimethoxysilane, adding the mixture into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 7:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 20g of simethicone, 120g of inorganic filler (100 g of nano active calcium carbonate, 10g of titanium dioxide with the particle size of 0.08 micrometer, 10g of nano zinc oxide), 30g of flame retardant (20 g of aluminum hydroxide and 10g of magnesium hydroxide), 20g of porous nano silicon dioxide, 7g of tackifier (gamma-aminopropyltriethoxysilane), 6g of alpha-aminosilane coupling agent (3 g of alpha-diethylaminomethyl triethoxysilane and 3g of alpha-aminoethylaminomethyl trimethoxysilane), and 10g of crosslinking agent (5 g of methyl trimethoxysilane and 5g of vinyl trimethoxysilane);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Example 8:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 13g of simethicone, 90g of inorganic filler (80 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 15g of flame retardant (10 g of aluminum hydroxide and 5g of magnesium hydroxide), 15g of porous nano silicon dioxide, 5g of tackifier (gamma-aminopropyltriethoxysilane), 4.5g of alpha-aminosilane coupling agent (2.5 g of alpha-diethylaminomethyl triethoxysilane and 2g of alpha-aminoethylaminomethyl trimethoxysilane), and 7g of crosslinking agent (methyl trimethoxysilane 4g and vinyl trimethoxysilane);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Comparative example 1:
the specific surface area is 200cm3Drying and dehydrating the fumed silica and the nano active calcium carbonate treated by the stearic acid at 160 ℃ for 2 to 3 hours; adding 100g of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPas, 10g of simethicone with the viscosity of 350 mPas, 80g of nano active calcium carbonate, 20g of aluminum hydroxide, 10g of magnesium hydroxide, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide, 15g of fumed silica, 4g of gamma-aminopropyltriethoxysilane and 3g of hydroxyl scavenger into a vacuum mixer, fully stirring for 150 minutes at 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing 4g of methyltrimethoxysilane, 4g of vinyltrimethoxysilane, 3g of alpha-diethylaminomethyltriethoxysilane and 3g of alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Comparative example 2:
the specific surface area is 200cm3Drying and dehydrating the fumed silica and the nano active calcium carbonate treated by the stearic acid at 160 ℃ for 2 to 3 hours; adding 100g of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPas, 10g of simethicone with the viscosity of 350 mPas, 80g of nano active calcium carbonate, 20g of aluminum hydroxide, 10g of magnesium hydroxide, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide, 15g of fumed silica, 4g of gamma-aminopropyltriethoxysilane and 3g of hydroxyl scavenger into a vacuum mixer, fully stirring for 150 minutes at 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing 4g of methyltrimethoxysilane, 4g of vinyl trimethoxy silane and 0.5g of dibutyltin dilaurate, adding into a high-speed planetary dispersion machine filled with a base material, and stirring for 30-150 minutes under the conditions of a rotating speed of 40-60rpm and a vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
Comparative example 3:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 5g of simethicone, 60g of inorganic filler (50 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 10g of flame retardant (5 g of aluminum hydroxide and 5g of magnesium hydroxide), 5g of porous nano silicon dioxide, 3g of tackifier (gamma-aminopropyltriethoxysilane), 3g of alpha-aminosilane coupling agent (2 g of alpha-diethylaminomethyl triethoxysilane and 1g of alpha-aminoethylaminomethyl trimethoxysilane), and 4g of crosslinking agent (2 g of methyl trimethoxysilane and 2g of vinyl trimethoxysilane);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing 2g of methyltrimethoxysilane, 2g of vinyltrimethoxysilane, 2g of alpha-diethylaminomethyltriethoxysilane and 1g of alpha-aminoethyl aminomethyl trimethoxysilane, adding the mixture into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
The mass part of the porous nanosilica of comparative example 3 is within the range of 10 to 20 parts or less as required by the present invention.
Comparative example 4:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 5g of simethicone, 60g of inorganic filler (50 g of nano active calcium carbonate, 3g of titanium dioxide with the particle size of 0.08 micrometer, 7g of nano zinc oxide), 10g of flame retardant (5 g of aluminum hydroxide and 5g of magnesium hydroxide), 5g of porous nano silicon dioxide, 3g of tackifier (gamma-aminopropyltriethoxysilane), 0.5g of alpha-aminosilane coupling agent (alpha-diethylaminomethyl triethoxysilane and 0.5g of alpha-aminoethylaminomethyl trimethoxysilane), 1g of crosslinking agent (methyl trimethoxysilane 2g and vinyl trimethoxysilane 2 g);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing 2g of methyltrimethoxysilane, 2g of vinyltrimethoxysilane, 2g of alpha-diethylaminomethyltriethoxysilane and 1g of alpha-aminoethyl aminomethyl trimethoxysilane, adding the mixture into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
The mass parts of the porous nano silica and the alpha-aminosilane coupling agent of comparative example 4 are within the range of 10 to 20 parts and below 3 to 6 parts as required by the present invention.
Comparative example 5:
the formula is as follows:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 20g of simethicone, 120g of inorganic filler (100 g of nano active calcium carbonate, 10g of titanium dioxide with the particle size of 0.08 micrometer, 10g of nano zinc oxide), 30g of flame retardant (20 g of aluminum hydroxide and 10g of magnesium hydroxide), 30g of porous nano silicon dioxide, 7g of tackifier (gamma-aminopropyltriethoxysilane), 6g of alpha-aminosilane coupling agent (3 g of alpha-diethylaminomethyl triethoxysilane and 3g of alpha-aminoethylaminomethyl trimethoxysilane), and 10g of crosslinking agent (5 g of methyl trimethoxysilane and 5g of vinyl trimethoxysilane);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
The mass part of the porous nanosilica of comparative example 5 is within the range of 10 to 20 parts or more as required by the present invention.
Comparative example 6:
the formula is as follows:
the formula is as follows: 100g of alpha, omega-dihydroxy polydimethylsiloxane, 20g of simethicone, 120g of inorganic filler (100 g of nano active calcium carbonate, 10g of titanium dioxide with the particle size of 0.08 micrometer, 10g of nano zinc oxide), 30g of flame retardant (20 g of aluminum hydroxide and 10g of magnesium hydroxide), 30g of porous nano silicon dioxide, 7g of tackifier (gamma-aminopropyltriethoxysilane), 8g of alpha-aminosilane coupling agent (4 g of alpha-diethylaminomethyl triethoxysilane and 4g of alpha-aminoethylaminomethyl trimethoxysilane), and 10g of crosslinking agent (5 g of methyl trimethoxysilane and 5g of vinyl trimethoxysilane);
drying and dehydrating porous nano silicon dioxide with the specific surface area of 200cm3/g and nano active calcium carbonate treated by hard fatty acid at 160 ℃ for 2-3 hours; adding alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 5000 mPa.S, dimethyl silicone oil with the viscosity of 350 mPa.S, nano activated calcium carbonate, aluminum hydroxide, magnesium hydroxide, titanium dioxide with the particle size of 0.08 micrometer, nano zinc oxide, porous nano silicon dioxide and gamma-aminopropyltriethoxysilane into a vacuum mixer, fully mixing for 150 minutes at the temperature of 150 ℃ and the vacuum degree of 0.06-0.1MPa, and cooling; cooling the base material to room temperature. Accurately weighing methyltrimethoxysilane, vinyltrimethoxysilane, alpha-diethylaminomethyltriethoxysilane and alpha-aminoethyl aminomethyl trimethoxysilane, adding into a high-speed planetary dispersing machine filled with a base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive. The product performance test results are shown in table 1.
The mass parts of the porous nano silica and the alpha-aminosilane coupling agent in comparative example 6 are within the range of 10-20 parts and 3-6 parts or more, which are required by the present invention.
TABLE 1 Performance test results for environmentally friendly room temperature curing one-component organosilicon adhesive
TABLE 1
The results prove that the organic silicon adhesive prepared by the method adopts the alpha-aminosilane coupling agent as the crosslinking catalyst, and the alpha-aminosilane coupling agent integrates the effects of the crosslinking agent, the coupling agent and the curing agent in the organic silicon adhesive, so that the prepared organic silicon adhesive is high in curing speed, good in bonding performance to the base material, free of heavy metal catalyst, obvious in environment-friendly effect, and free of corrosion of small molecular alcohol substances released in the curing process to the base material. The nano porous silica is used as a reinforcing material, and the porous nano silica is a light porous nano structure material formed by coalescence of ultrafine silica particles. The aperture is 20-50 nm, and the specific surface area reaches 150-350cm3The silicon rubber has a porosity of 95-97%, when the silicon rubber is mixed with base rubber, a coupling agent and the like, the contact area of the nano porous silicon dioxide and the silicon rubber is increased by 2-10 times, and in the vulcanization crosslinking process of the silicon rubber, part of high molecules can penetrate through a cavity structure of the nano porous silicon dioxide to form an organic-inorganic hybrid interpenetrating network structure, so that the mechanical strength of the silicon rubber is greatly improved. Therefore, the organic silicon adhesive prepared by the method has higher shear strength which can reach more than 3.5 MPa. The method is widely applied to sealing and bonding of electronic components and other non-structural sealing and bonding.
In contrast, in the case of the silicone adhesive prepared in comparative example 1, since the porous nano-silica is not added and the fumed silica is used as a reinforcing material, the shear strength of the prepared silicone adhesive is significantly reduced to only 1.63 MPa. In the organosilicon adhesive prepared in comparative example 2, the shear strength and the bonding property to the base material of the prepared organosilicon adhesive are reduced by using common dibutyltin dilaurate as a catalyst and using fumed silica as a reinforcing material.
From comparative examples 3 to 6 in comparison with examples 1 to 8, it is clear that: the mass parts of the formula only have higher shear strength and more excellent bonding property within the range of the invention.
Compared with examples 6-8, the addition of the auxiliary agent has little influence on the shear strength and the adhesive property, and the addition of the auxiliary agent enhances other physical and chemical properties, so long as the extension of the formula of the invention is within the protection scope of the invention.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It should be understood by those skilled in the art that the above embodiments do not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent variations fall within the scope of the present invention.
Claims (10)
1. The environment-friendly high-strength organic silicon adhesive is characterized by comprising the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of a tackifier, 3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent.
2. The environment-friendly high-strength organic silicon adhesive as claimed in claim 1, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 5-20 parts of simethicone, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, 10-20 parts of porous nano silicon dioxide, 3-7 parts of tackifier, 3-6 parts of alpha-aminosilane coupling agent, 4-10 parts of cross-linking agent and 1-10 parts of auxiliary agent.
3. The environment-friendly high-strength silicone adhesive according to claim 1 or 2, wherein the inorganic filler comprises: hydrophobic silicon dioxide by a precipitation method, nano active calcium carbonate treated by hard fatty acid, light calcium carbonate treated by hard fatty acid, heavy calcium carbonate treated by hard fatty acid, titanium dioxide, nano zinc oxide and active silicon micropowder.
4. The environment-friendly high-strength silicone adhesive according to claim 1 or 2, wherein the flame retardant comprises: aluminum hydroxide, magnesium hydroxide, antimony trioxide, zinc borate, melamine, diphosphonate and ammonium polyphosphate.
5. The environment-friendly high-strength silicone adhesive according to claim 1 or 2, wherein the tackifier comprises: gamma-methacryloxypropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, vinyltris (. beta. -methoxyethoxy) silane, bis (. gamma. -trimethoxysilylpropyl) amine.
6. The environment-friendly high-strength silicone adhesive according to claim 1 or 2, wherein the α -aminosilane coupling agent comprises: alpha-diethylaminomethyltriethoxysilane, alpha-aminoethylaminomethyltrimethoxysilane, alpha-divinyltriaminomethyltrimethoxysilane.
7. The environment-friendly high-strength silicone adhesive according to claim 1 or 2, wherein the crosslinking agent comprises: methyltrimethoxysilane, vinyltrimethoxysilane, tetramethoxysilane, tetraethoxysilane, anilinomethyltriethoxysilane, dichloromethyltriethoxysilane.
8. The environment-friendly high-strength silicone adhesive according to claim 2, wherein the auxiliary agent comprises: preservative, anti-yellowing agent, antioxidant and hydroxyl scavenger.
9. The preparation method of the environment-friendly high-strength organic silicon adhesive is characterized by comprising the following steps of:
preparing materials according to a formula, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of tackifier,3-6 parts of an alpha-aminosilane coupling agent and 4-10 parts of a cross-linking agent;
drying and dehydrating the nano porous silica and the inorganic filler at the temperature of 150-180 ℃ for 2-3 hours respectively;
adding alpha, omega-dihydroxy polydimethylsiloxane, simethicone, inorganic filler, flame retardant, nano porous silicon dioxide and tackifier into a high-speed planetary dispersion machine, fully stirring for 60-180 minutes at the temperature of 120-;
after the base material is cooled to room temperature, adding the cross-linking agent and the alpha-aminosilane coupling agent into a high-speed planetary dispersing machine filled with the base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive.
10. The preparation method of the environment-friendly high-strength organic silicon adhesive is characterized by comprising the following steps of:
preparing materials according to a formula, wherein the formula comprises the following components in parts by mass: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500-20000 mPas, 5-20 parts of dimethyl silicone oil with the viscosity of 100-350 mPas, 60-120 parts of inorganic filler, 10-30 parts of flame retardant, and the specific surface area of 150-350cm310-20 parts of porous nano silicon dioxide per gram, 3-7 parts of tackifier, 3-6 parts of alpha-aminosilane coupling agent, 4-10 parts of cross-linking agent and 1-10 parts of auxiliary agent;
drying and dehydrating the nano porous silica and the inorganic filler at the temperature of 150-180 ℃ for 2-3 hours respectively;
adding alpha, omega-dihydroxy polydimethylsiloxane, simethicone, inorganic filler, flame retardant, nano porous silicon dioxide, tackifier and auxiliary agent into a high-speed planetary dispersion machine, fully stirring for 60-180 minutes at the temperature of 120-;
after the base material is cooled to room temperature, adding the cross-linking agent and the alpha-aminosilane coupling agent into a high-speed planetary dispersing machine filled with the base material, and stirring for 30-150 minutes under the conditions of the rotating speed of 40-60rpm and the vacuum degree of 0.06-0.1MPa to prepare the environment-friendly high-strength organic silicon adhesive.
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| CN115785895A (en) * | 2022-12-20 | 2023-03-14 | 广州市白云化工实业有限公司 | Solvent-free sprayable condensed type silicone sealant and preparation method thereof |
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Application publication date: 20200110 |