CN112831313A - Single-component room-temperature curing adhesive and preparation method thereof - Google Patents
Single-component room-temperature curing 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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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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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Abstract
The invention discloses a preparation method of a single-component room-temperature curing adhesive, which comprises the following steps: stirring the basic polymer, the reinforcing filler, the semi-reinforcing filler and the composite heat-conducting filler for 3 hours under a dehydration condition, and cooling to room temperature to obtain a mixture A; adding a reactive plasticizer and a dehydrating agent, and stirring for 20-30 minutes in vacuum to obtain a mixture B; adding a coupling agent, and stirring for 20-30 minutes in vacuum to obtain a mixture C; adding a cross-linking agent, and stirring for 20-30 minutes in vacuum to obtain a mixture D; adding a catalyst, and stirring for 20-30 minutes in vacuum to obtain the single-component room-temperature curing adhesive; also discloses a single-component room temperature curing adhesive. The invention effectively optimizes the heat conduction performance of the single-component room temperature curing adhesive, enhances the mechanical property of the single-component room temperature curing adhesive, improves the toughness, and the shock resistance and the stamping resistance of the single-component room temperature curing adhesive, and further ensures that the adhesive effectively adheres to electronic components in the transportation and use processes so as to ensure the long-term electrical operation of the single-component room temperature curing adhesive.
Description
Technical Field
The invention relates to the technical field of adhesive production, in particular to a single-component room temperature curing adhesive and a preparation method thereof.
Background
In the field of electronic industry, for example, silicone rubber is often used as an adhesive, and with the rapid development of the electronic industry, the silicone rubber is endowed with more and more functions, such as adhesion, sealing, heat conduction, flame retardance, potting, water resistance, impact resistance, shock resistance, voltage resistance and the like. Although the silicone rubber has good thermal stability, cold resistance and electrical properties, the silicone rubber has low cohesive strength and weak adhesion, and therefore, a functional filler needs to be added in a targeted manner to reinforce and improve the adhesive strength and the cohesive strength. The silicon rubber is usually processed into single-component room temperature vulcanized silicon rubber, has simple package and convenient use, can be cured at room temperature without heating, has no heat release and heat absorption phenomena during curing, has small shrinkage after curing and good adhesion to materials, and is mainly used as an adhesive and a sealant. The single-component room temperature vulcanized silicone rubber is mainly endowed with functions by the reinforcing filler, and different reinforcing fillers have different defects, such as strong adhesion, weak heat conduction and flame retardant properties; or the adhesive has good heat-conducting property, slightly poor adhesive property, higher hardness, poor impact resistance and poor shock resistance, and the adhesive is easy to fall off from the adhesive surface of the electronic component in the transportation and use processes of the electric appliance, so that the function of protecting the electronic component is lost.
Therefore, how to design an adhesive with both impact resistance and shock resistance and high thermal conductivity is a major technical problem.
Disclosure of Invention
In order to overcome the technical problems, the invention discloses a preparation method of a single-component room temperature curing adhesive; also discloses a single-component room temperature curing adhesive.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of a single-component room temperature curing adhesive comprises the following steps:
step 1, stirring a base polymer, a reinforcing filler, a semi-reinforcing filler and a composite heat-conducting filler for 3 hours under a dehydration condition, and cooling to room temperature to obtain a mixture A;
step 2, adding a reactive plasticizer and a dehydrating agent into the mixture A, and stirring for 20-30 minutes in vacuum to obtain a mixture B;
step 3, adding a coupling agent into the mixture B, and stirring for 20-30 minutes in vacuum to obtain a mixture C;
step 4, adding a cross-linking agent into the mixture C, and stirring for 20-30 minutes in vacuum to obtain a mixture D;
and 5, adding a catalyst into the mixture D, and stirring for 20-30 minutes in vacuum to obtain the single-component room-temperature curing adhesive.
The preparation method of the single-component room-temperature curing adhesive comprises the following steps of: stirring and dehydrating in vacuum at 100-110 ℃, and controlling the water content to be lower than 800 PPM.
The preparation method of the single-component room temperature curing adhesive comprises, by mass, 30-50% of a base polymer, 5-10% of a reactive plasticizer, 10-20% of a reinforcing filler, 15-30% of a semi-reinforcing filler, 40-60% of a composite heat-conducting filler, 1-5% of a water removing agent, 1-5% of a coupling agent, 2-10% of a cross-linking agent and 0.5-1.5% of a catalyst.
The preparation method of the single-component room-temperature curing adhesive comprises the following step of preparing a single-component room-temperature curing adhesive, wherein the base polymer is trimethoxy end-capped polydimethylsiloxane, and the viscosity of the base polymer is 1500-20000 mPa.
The preparation method of the single-component room temperature curing adhesive comprises the steps of preparing the reinforcing filler by using fumed silica, and preparing the reinforcing filler with the specific surface area of 150m2/g。
The preparation method of the single-component room-temperature curing adhesive comprises the following steps of (1): 5 and the mixture of indirect zinc oxide and aluminum oxide with the particle size of 2-3 microns.
The preparation method of the single-component room-temperature curing adhesive comprises the step of preparing a single-component room-temperature curing adhesive, wherein the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane and gamma-mercaptopropyltrimethoxysilane.
In the preparation method of the single-component room temperature curing adhesive, the cross-linking agent is one or more of tetramethoxysilane, methyltrimethoxysilane and vinyl trimethoxysilane.
In the preparation method of the single-component room-temperature curing adhesive, the catalyst is one or more of dibutyltin dilaurate, tetraisopropyl titanate, dibutyltin bis (acetyl acetonate) and diisopropyl bis (ethyl acetoacetate) titanate.
A single-component room temperature curing adhesive is prepared by the preparation method of the single-component room temperature curing adhesive.
The invention has the beneficial effects that: the single-component room-temperature curing adhesive is reasonable and ingenious in design, the basic polymer is used as a basic raw material under a strict dehydration condition, and the heat conduction performance of the single-component room-temperature curing adhesive is effectively optimized by adding the composite heat-conducting filler, so that the problem that the traditional adhesive is poor in heat conduction and flame retardant performance is solved; the reinforcing filler and the semi-reinforcing filler are used for reinforcing the mechanical property of the adhesive, improving the toughness and the shock and stamping resistant functions of the adhesive, and further ensuring that the adhesive effectively adheres to electronic components in the transportation and use processes so as to ensure the long-term electrical operation of the adhesive; moreover, the coupling agent greatly enhances the deep curing speed of the adhesive and the adhesion to the bonding base material, so that the room temperature curing efficiency and the mechanical property of the adhesive are effectively optimized.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to facilitate the understanding and appreciation of the technical solutions of the present invention, rather than to limit the invention thereto.
The invention provides a preparation method of a single-component room-temperature curing adhesive, which comprises the following steps:
step 1, stirring a base polymer, a reinforcing filler, a semi-reinforcing filler and a composite heat-conducting filler for 3 hours under a dehydration condition, and cooling to room temperature to obtain a mixture A;
step 2, adding a reactive plasticizer and a dehydrating agent into the mixture A, and stirring for 20-30 minutes in vacuum to obtain a mixture B;
step 3, adding a coupling agent into the mixture B, and stirring for 20-30 minutes in vacuum to obtain a mixture C;
step 4, adding a cross-linking agent into the mixture C, and stirring for 20-30 minutes in vacuum to obtain a mixture D;
and 5, adding a catalyst into the mixture D, and stirring for 20-30 minutes in vacuum to obtain the single-component room-temperature curing adhesive.
Specifically, under strict dehydration conditions, the basic polymer is used as a basic raw material, and the composite heat-conducting filler is added, so that the heat conduction performance of the single-component room-temperature curing adhesive is effectively optimized, and the problem of poor heat conduction and flame retardance of the traditional adhesive is solved; the reinforcing filler and the semi-reinforcing filler are used for reinforcing the mechanical property of the adhesive, improving the toughness and the shock and stamping resistant functions of the adhesive, and further ensuring that the adhesive effectively adheres to electronic components in the transportation and use processes so as to ensure the long-term electrical operation of the adhesive; moreover, the coupling agent greatly enhances the deep curing speed of the adhesive and the adhesion to the bonding base material, so that the room temperature curing efficiency and the mechanical property of the adhesive are effectively optimized.
Preferably, the dehydration conditions are: stirring and dehydrating in vacuum at 100-110 ℃, and controlling the water content to be lower than 800 PPM; the water content in the reaction system is strictly controlled to be in a trace level, so that the single-component room-temperature curing adhesive can be extruded out when in use and can be subjected to condensation reaction with trace water in the air to form an elastic colloid, and the deep curing speed of the adhesive is effectively improved.
Preferably, the mass percentage of the base polymer is 30-50%, the mass percentage of the reactive plasticizer is 5-10%, the mass percentage of the reinforcing filler is 10-20%, the mass percentage of the semi-reinforcing filler is 15-30%, the mass percentage of the composite heat-conducting filler is 40-60%, the mass percentage of the water removing agent is 1-5%, the mass percentage of the coupling agent is 1-5%, the mass percentage of the cross-linking agent is 2-10%, and the mass percentage of the catalyst is 0.5-1.5.
Specifically, the basic polymer is trimethoxy terminated polydimethylsiloxane, the viscosity of the basic polymer is 1500-20000 mPa · s, when the polymer is extruded for use, the basic polymer and a cross-linking agent are subjected to condensation reaction with water under the action of a catalyst, a byproduct alcohol is removed, an elastic colloid is generated, the elastic colloid has excellent heat conduction performance, cohesiveness, toughness and shock resistance and stamping resistance, and the protection requirement on electronic components is further enhanced.
Specifically, the reinforcing filler is fumed silica, and the specific surface area of the reinforcing filler is 150m2The reinforcing filler effectively enhances the mechanical property of the elastic colloid, and further optimizes the toughness and the shock resistance and the stamping resistance of the elastic colloid.
Specifically, the semi-reinforcing filler is one or more of nano calcium carbonate, diatomite, calcined kaolin and precipitated white carbon black, and the semi-reinforcing filler effectively enhances the mechanical property of the elastic colloid and further optimizes the toughness and the shock resistance and the stamping resistance of the elastic colloid.
Specifically, the reactive plasticizer is triethoxysilane-terminated liquid polybutadiene, participates in a curing reaction, and is used for adjusting the hardness of the elastic colloid, and the extrudability and dielectric property of the adhesive.
Specifically, the volume ratio of the composite heat-conducting filler is 1: 5 and the mixture of indirect zinc oxide and aluminum oxide with the particle size of 2-3 microns.
Specifically, the water removal agent is one or more of hexamethyldisilazane, octamethylcyclotetrasilazane and vinyl trimethoxy silane, and trace moisture in the adhesive is removed by a chemical method, so that the stability and the storage property of the product are enhanced.
Specifically, the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane and gamma-mercaptopropyltrimethoxysilane, and the coupling agent greatly enhances the deep curing speed of the adhesive and the bonding property of the adhesive to a bonding base material.
Specifically, the cross-linking agent is one or more of tetramethoxysilane, methyltrimethoxysilane and vinyltrimethoxysilane.
Specifically, the catalyst is one or more of dibutyltin dilaurate, tetraisopropyl titanate, dibutyltin bis (acetylacetonate), and diisopropyl bis (ethyl acetoacetate) titanate.
The invention also discloses a single-component room temperature curing adhesive which is prepared by the preparation method of the single-component room temperature curing adhesive.
The preparation process according to the invention is now described in detail in the following examples:
example 1: the preparation method of the one-component room temperature curing adhesive provided by the embodiment comprises the following steps:
step 1, 500g of trimethoxy terminated polydimethylsiloxane with the viscosity of 5000 mPas and 100g of 150m of specific surface area2The preparation method comprises the following steps of (1) stirring fumed silica per gram, 200 grams of fatty acid treated nano calcium carbonate, 100 grams of calcined kaolin and 400 grams of composite heat-conducting filler in vacuum at 100 ℃ for 3 hours, and cooling to room temperature to obtain a mixture A; wherein, the volume ratio of the composite heat conduction filler is 1: 5, the indirect method zinc oxide is mixed with aluminum oxide with the particle size of 2 microns, and the water content of the component A is 680 PPM;
step 2, adding 100g of triethoxysilane-terminated liquid polybutadiene and 20g of vinyltrimethoxysilane into the mixture A, and stirring for 30 minutes in vacuum to obtain a mixture B;
step 3, adding 10g of gamma-aminopropyltriethoxysilane and 10g of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane into the mixture B, and stirring for 20 minutes in vacuum to obtain a mixture C;
step 4, adding 30g of methyltrimethoxysilane into the mixture C, and stirring for 30 minutes in vacuum to obtain a mixture D;
and 5, adding 12g of diisopropyl bis (ethyl acetoacetate) titanate into the mixture D, and stirring for 20 minutes in vacuum to obtain the single-component room-temperature curing adhesive.
Adhesive performance parameters were measured on the one-component room temperature curing adhesive prepared in example 1. The physical properties after curing for 7 days at 23 ℃ and 55% humidity were determined as shown in Table 1.
Example 2: the preparation method of the one-component room temperature curing adhesive provided by the embodiment comprises the following steps:
step 1, 500g of trimethoxy end-capped polydimethylsiloxane with viscosity of 10000 mPas and 30g of specific surface area of 150m2The preparation method comprises the following steps of (1) stirring fumed silica per gram, 250g of fatty acid treated nano calcium carbonate, 100g of diatomite and 400g of composite heat-conducting filler in vacuum at 100 ℃ for 3 hours, and cooling to room temperature to obtain a mixture A; wherein, the volume ratio of the composite heat conduction filler is 1: 5, the indirect method zinc oxide is mixed with aluminum oxide with the particle size of 2 microns, and the water content of the component A is 700 PPM;
step 2, adding 120g of triethoxysilane-terminated liquid polybutadiene and 20g of hexamethyldisilazane into the mixture A, and stirring for 30 minutes in vacuum to obtain a mixture B;
step 3, adding 10g of gamma-aminopropyl trimethoxy silane and 15g of gamma-mercaptopropyl trimethoxy silane into the mixture B, and stirring for 20 minutes in vacuum to obtain a mixture C;
step 4, adding 30g of tetramethoxysilane into the mixture C, and stirring for 30 minutes in vacuum to obtain a mixture D;
and 5, adding 20g of tetraisopropyl titanate into the mixture D, and stirring for 20 minutes in vacuum to obtain the single-component room-temperature curing adhesive.
And (3) measuring adhesive performance parameters of the single-component room-temperature curing adhesive prepared in the example 2. The physical properties after curing for 7 days at 23 ℃ and 55% humidity were determined as shown in Table 1.
Example 3: the preparation method of the one-component room temperature curing adhesive provided by the embodiment comprises the following steps:
step 1, 500g of trimethoxy end-capped polydimethylsiloxane having a viscosity of 15000 mPas and 50g of a specific surface area of 150m2Fumed silica/g, 200g fatty acid treatmentStirring nano calcium carbonate, 200g of calcined kaolin and 500g of composite heat-conducting filler at 100 ℃ for 3 hours in vacuum, and cooling to room temperature to obtain a mixture A; wherein, the volume ratio of the composite heat conduction filler is 1: 5, the indirect method zinc oxide is mixed with aluminum oxide with the particle size of 2 microns, and the water content of the component A is 600 PPM;
step 2, adding 200g of triethoxysilane-terminated liquid polybutadiene and 30g of octamethylcyclotetrasilazane into the mixture A, and stirring for 30 minutes in vacuum to obtain a mixture B;
step 3, adding 10g of gamma-methacryloxypropyltrimethoxysilane, 10g of gamma-aminopropyltrimethoxysilane and 10g of gamma-mercaptopropyltrimethoxysilane into the mixture B, and stirring for 20 minutes in vacuum to obtain a mixture C;
step 4, adding 30g of vinyl trimethoxy silane into the mixture C, and stirring for 30 minutes in vacuum to obtain a mixture D;
and 5, adding 20g of dibutyltin bis (acetylacetonate) into the mixture D, and stirring for 20 minutes in vacuum to obtain the single-component room-temperature curing adhesive.
And (3) measuring adhesive performance parameters of the single-component room-temperature curing adhesive prepared in the example 3. The physical properties after curing for 7 days at 23 ℃ and 55% humidity were determined as shown in Table 1.
TABLE 1 determination of adhesive Performance parameters for examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Hardness of | 40HA | 38HA | 42HA |
| Tensile strength | 1.8MPa | 2MPa | 2.2MPa |
| Elongation at break | 260％ | 280％ | 320％ |
| Coefficient of thermal conductivity | >0.8W/m·K | >0.8W/m·K | >0.8W/m·K |
| Volume resistance | 8.0*1011Ω.cm | 8.5*1011Ω.cm | 7.0*1011Ω.cm |
| Dielectric strength | >25KV/mm | >25KV/mm | >25KV/mm |
| Temperature resistance | -50～200℃ | -50～200℃ | -50～200℃ |
The single-component room-temperature curing adhesive is reasonable and ingenious in design, the basic polymer is used as a basic raw material under a strict dehydration condition, and the heat conduction performance of the single-component room-temperature curing adhesive is effectively optimized by adding the composite heat-conducting filler, so that the problem that the traditional adhesive is poor in heat conduction and flame retardant performance is solved; the reinforcing filler and the semi-reinforcing filler are used for reinforcing the mechanical property of the adhesive, improving the toughness and the shock and stamping resistant functions of the adhesive, and further ensuring that the adhesive effectively adheres to electronic components in the transportation and use processes so as to ensure the long-term electrical operation of the adhesive; moreover, the coupling agent greatly enhances the deep curing speed of the adhesive and the adhesion to the bonding base material, so that the room temperature curing efficiency and the mechanical property of the adhesive are effectively optimized.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Those skilled in the art can make many possible variations and modifications to the invention using the above disclosed technical means and teachings, or can modify equivalent embodiments with equivalent variations, without departing from the scope of the invention. Therefore, all equivalent changes made according to the shape, structure and principle of the present invention should be covered by the protection scope of the present invention without departing from the contents of the technical scheme of the present invention.
Claims (10)
1. A preparation method of the single-component room temperature curing adhesive is characterized by comprising the following steps:
step 1, stirring a base polymer, a reinforcing filler, a semi-reinforcing filler and a composite heat-conducting filler for 3 hours under a dehydration condition, and cooling to room temperature to obtain a mixture A;
step 2, adding a reactive plasticizer and a dehydrating agent into the mixture A, and stirring for 20-30 minutes in vacuum to obtain a mixture B;
step 3, adding a coupling agent into the mixture B, and stirring for 20-30 minutes in vacuum to obtain a mixture C;
step 4, adding a cross-linking agent into the mixture C, and stirring for 20-30 minutes in vacuum to obtain a mixture D;
and 5, adding a catalyst into the mixture D, and stirring for 20-30 minutes in vacuum to obtain the single-component room-temperature curing adhesive.
2. The preparation method of the one-component room temperature curing adhesive according to claim 1, wherein the dehydration conditions are as follows: stirring and dehydrating in vacuum at 100-110 ℃, and controlling the water content to be lower than 800 PPM.
3. The preparation method of the one-component room temperature curing adhesive according to claim 2, wherein the one-component room temperature curing adhesive comprises, by mass, 30-50% of a base polymer, 5-10% of a reactive plasticizer, 10-20% of a reinforcing filler, 15-30% of a semi-reinforcing filler, 40-60% of a composite heat-conducting filler, 1-5% of a water removing agent, 1-5% of a coupling agent, 2-10% of a crosslinking agent, and 0.5-1.5% of a catalyst.
4. The preparation method of the one-component room temperature curing adhesive according to claim 3, wherein the base polymer is trimethoxy terminated polydimethylsiloxane, and the viscosity of the base polymer is 1500-20000 mPa-s.
5. The preparation method of the one-component room temperature curing adhesive as claimed in claim 4, wherein the reinforcing filler is fumed silica, and the specific surface area of the reinforcing filler is 150m2/g。
6. The preparation method of the one-component room temperature curing adhesive according to claim 5, wherein the composite heat-conducting filler is a mixture of 1: 5 and the mixture of indirect zinc oxide and aluminum oxide with the particle size of 2-3 microns.
7. The preparation method of the single-component room temperature curing adhesive as claimed in claim 6, wherein the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane and gamma-mercaptopropyltrimethoxysilane.
8. The method for preparing the one-component room temperature curing adhesive according to claim 7, wherein the cross-linking agent is one or more of tetramethoxysilane, methyltrimethoxysilane and vinyltrimethoxysilane.
9. The method for preparing the one-component room temperature curing adhesive according to claim 8, wherein the catalyst is one or more of dibutyltin dilaurate, tetraisopropyl titanate, dibutyltin bis (acetylacetonate), and diisopropyl bis (ethyl acetoacetate) titanate.
10. A one-component room temperature curing adhesive, which is prepared by the preparation method of the one-component room temperature curing adhesive as claimed in any one of claims 1 to 9.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618208A (en) * | 2011-01-28 | 2012-08-01 | 深圳市百丽春粘胶实业有限公司 | Halogen-free flame-retardant heat-conduction organosilicon electronic pouring sealant and preparation technology thereof |
| CN111073591A (en) * | 2019-12-13 | 2020-04-28 | 深圳市丰盛源科技有限公司 | Single-component room temperature curing liquid silicone rubber and preparation method thereof |
-
2021
- 2021-01-06 CN CN202110012527.6A patent/CN112831313A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618208A (en) * | 2011-01-28 | 2012-08-01 | 深圳市百丽春粘胶实业有限公司 | Halogen-free flame-retardant heat-conduction organosilicon electronic pouring sealant and preparation technology thereof |
| CN111073591A (en) * | 2019-12-13 | 2020-04-28 | 深圳市丰盛源科技有限公司 | Single-component room temperature curing liquid silicone rubber and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 杨思忠 等: "《装配式混凝土新型构件生产与高效施工关键技术》", 31 March 2020, 中国建材工业出版社 * |
| 汪锡安 等: "《粘合剂及其应用》", 30 November 1981, 上海科学技术文献出版社 * |
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