CN113817438A - Preparation method of bi-component condensed type room temperature vulcanized silicone rubber - Google Patents
Preparation method of bi-component condensed type room temperature vulcanized silicone rubber Download PDFInfo
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- CN113817438A CN113817438A CN202010569400.XA CN202010569400A CN113817438A CN 113817438 A CN113817438 A CN 113817438A CN 202010569400 A CN202010569400 A CN 202010569400A CN 113817438 A CN113817438 A CN 113817438A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
A preparation method of a bi-component condensed type room temperature vulcanized silicone rubber comprises a component A and a component B, wherein the component A and the component B are mixed according to a mass ratio of 1:1 to obtain the bi-component condensed type room temperature vulcanized silicone rubber. The invention has simple process, stable proportion and good fixed telephone effect, has good adhesive property to glass, ceramics, metal and the like, has excellent operation performance when the operation time is 30min at the environment temperature of 25 ℃.
Description
Technical Field
The invention relates to the technical field of vulcanized silicone rubber, in particular to a preparation method of double-component condensed type room temperature vulcanized silicone rubber.
Background
Two-component condensation type room temperature vulcanized silicone rubber is the most common room temperature vulcanized silicone rubber, and raw rubber of the two-component condensation type room temperature vulcanized silicone rubber is usually hydroxyl terminated polysiloxane which is combined with other compounding agents and catalysts to form rubber compounds, and the viscosity of the rubber compounds can range from 100 centistokes to one million centistokes.
The reaction of the two-component condensed type room temperature vulcanized silicone rubber is initiated not by the moisture of air but by a catalyst. Typically, the silica gel, filler, and crosslinking agent are packaged as one component and the catalyst is packaged separately as another component, or in other combinations, where the catalyst and crosslinking agent must be packaged separately. The two-component condensed type room temperature vulcanized silicone rubber can keep elasticity for a long time within the temperature range of-65 ℃ to 250 ℃, has excellent electrical property and chemical stability, can resist water, ozone and weather aging, and has simple usage and strong process applicability, thereby being widely used for encapsulating and film-making materials.
The side group on the main chain of the double-component condensed type room temperature vulcanized silicone rubber can be substituted by other groups, such as trifluoropropyl, cyanoethyl and the like except methyl, so as to improve the performances of low temperature resistance, heat resistance, radiation resistance, solvent resistance and the like. Meanwhile, heat-resistant, flame-retardant, heat-conducting and electric-conducting additives can be added according to the needs to prepare the silicone rubber with ablation resistance, flame retardance, heat conduction and electric conductivity.
At present, in the actual construction process, if the mixing proportion of the raw materials fluctuates, the performance of the concrete is easy to be unstable, even the concrete is not solidified, thereby limiting the application of the concrete in the field.
Disclosure of Invention
The invention aims to provide a preparation method of a double-component condensed type room temperature vulcanized silicone rubber, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of bi-component condensed type room temperature vulcanized silicone rubber comprises the following steps:
the component A comprises: mixing alpha, omega-dihydroxy polydimethylsiloxane, nano active calcium carbonate and hydrophilic fumed silica according to the weight ratio of 3: (1-2): (1.5-2) adding the mixture into a high-speed stirrer and stirring the mixture uniformly;
and B component: firstly, mixing dimethyl silicone oil and nano active calcium carbonate according to the proportion of 2: (3-5), kneading for 2 hours under the conditions that the vacuum degree is more than 0.08MPa and the temperature is 110 ℃, cooling, and adding the mixture into a kneader according to the ratio of 3: 2: 1: 1:1, adding hydrophilic fumed silica, black paste, a cross-linking agent, a coupling agent and a catalyst, vacuumizing and uniformly stirring, and subpackaging to obtain a component B;
and mixing the component A and the component B according to the mass ratio of 1:1 to obtain the double-component condensed type room temperature vulcanized silicone rubber.
Preferably, the coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane and 3- (2, 3-glycidoxy) propyltrimethoxysilane.
Preferably, the cross-linking agent is one or more of methyltrimethoxysilane, vinyltrimethoxysilane, tetraethoxysilane and polyethyl silicate.
Preferably, the catalyst is one or more of dioctyltin dilaurate and dibutyltin dilaurate.
The invention has simple process, stable proportion and good fixed telephone effect, has good adhesive property to glass, ceramics, metal and the like, has excellent operation performance when the operation time is 30min at the environment temperature of 25 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of bi-component condensed type room temperature vulcanized silicone rubber comprises the following steps:
the component A comprises: mixing alpha, omega-dihydroxy polydimethylsiloxane, nano active calcium carbonate and hydrophilic fumed silica according to the weight ratio of 3: 1: 2, adding the mixture into a high-speed stirrer to be stirred uniformly;
and B component: firstly, mixing dimethyl silicone oil and nano active calcium carbonate according to the proportion of 2: 3, kneading for 2 hours under the conditions that the vacuum degree is more than 0.08MPa and the temperature is 110 ℃, cooling, and adding the mixture into a kneader according to the ratio of 3: 2: 1: 1:1, adding hydrophilic fumed silica, black paste, methyltrimethoxysilane, gamma-aminopropyltriethoxysilane and dioctyltin dilaurate, vacuumizing, uniformly stirring, and subpackaging to obtain a component B;
and mixing the component A and the component B according to the mass ratio of 1:1 to obtain the double-component condensed type room temperature vulcanized silicone rubber.
Example 2
A preparation method of bi-component condensed type room temperature vulcanized silicone rubber comprises the following steps:
the component A comprises: mixing alpha, omega-dihydroxy polydimethylsiloxane, nano active calcium carbonate and hydrophilic fumed silica according to the weight ratio of 3: 1: adding the mixture into a high-speed stirrer according to the proportion of 1.5, and stirring the mixture uniformly;
and B component: firstly, mixing dimethyl silicone oil and nano active calcium carbonate according to the proportion of 2: 4, kneading for 2 hours under the conditions that the vacuum degree is more than 0.08MPa and the temperature is 110 ℃, cooling, and adding the mixture into a kneader according to the ratio of 3: 2: 1: 1:1, adding hydrophilic fumed silica, black paste, vinyl trimethoxy silane, gamma-aminopropyl trimethoxy silane and dibutyltin dilaurate in the mixture, vacuumizing and uniformly stirring, and subpackaging to obtain a component B;
and mixing the component A and the component B according to the mass ratio of 1:1 to obtain the double-component condensed type room temperature vulcanized silicone rubber.
Example 3
A preparation method of bi-component condensed type room temperature vulcanized silicone rubber comprises the following steps:
the component A comprises: mixing alpha, omega-dihydroxy polydimethylsiloxane, nano active calcium carbonate and hydrophilic fumed silica according to the weight ratio of 3: 2: 2, adding the mixture into a high-speed stirrer to be stirred uniformly;
and B component: firstly, mixing dimethyl silicone oil and nano active calcium carbonate according to the proportion of 2: 5, adding the mixture into a kneader, kneading the mixture for 2 hours under the conditions that the vacuum degree is more than 0.08MPa and the temperature is 110 ℃, and after the mixture is cooled, adding the mixture into the kneader according to the ratio of 3: 2: 1: 1:1, adding hydrophilic fumed silica, black paste, tetraethoxysilane, gamma-beta- (aminoethyl) -gamma-aminopropyl trimethoxy silane and dibutyltin dilaurate, vacuumizing and uniformly stirring, and subpackaging to obtain a component B;
and mixing the component A and the component B according to the mass ratio of 1:1 to obtain the double-component condensed type room temperature vulcanized silicone rubber.
Comparative example
The component A comprises: 100 parts of 107 gums (i.e. the α, ω -dihydroxypolydimethylsiloxane described in the present invention, where n is 600 and viscosity is 5000cs), 10 parts of dimethylpolysiloxane (viscosity 100cs), 50 parts of stearic acid-treated calcium carbonate (particle size less than 2 μm, stearic acid used in an amount of 2.5% by weight relative to calcium carbonate);
and B component: 10 parts of tetraethoxysilane, 2 parts of gamma-aminopropyltriethoxysilane and 0.1 part of dibutyltin dilaurate;
the preparation process comprises the following steps:
the preparation process of the component A comprises putting the raw materials into a planetary stirrer one by one, setting the temperature at 100 deg.C, the rotation speed at 30rpm, maintaining the vacuum state (pressure less than 0.01MPa), and the dispersion time at 1h, and naturally cooling for use;
the preparation process of the component B comprises putting the raw materials into a planetary mixer one by one, setting the temperature at 25 deg.C, the rotation speed at 30rpm, maintaining the vacuum state (the pressure is less than 0.01Mpa), and the dispersion time at 0.5h, and finishing the dispersion for use;
and then, adding the prepared component A and the prepared component B into an electric stirrer, stirring at 60rpm at room temperature for 3 minutes, and uniformly mixing the components to obtain the product, namely the bi-component condensed type room temperature vulcanized silicone rubber.
The mechanical tests of examples 1 to 3 of the present invention and comparative examples were conducted, and the results are shown in Table 1 below
Table 1 results of performance testing
As shown in the table, the two-component condensed type room temperature vulcanized silicone rubber prepared by the invention has excellent mechanical property and flame retardant property (V0 grade), large resistivity, relatively high breakdown voltage and various properties superior to those of a comparative example.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (4)
1. The preparation method of the double-component condensed type room temperature vulcanized silicone rubber is characterized by comprising the following steps:
the component A comprises: mixing alpha, omega-dihydroxy polydimethylsiloxane, nano active calcium carbonate and hydrophilic fumed silica according to the weight ratio of 3: (1-2): (1.5-2) adding the mixture into a high-speed stirrer and stirring the mixture uniformly;
and B component: firstly, mixing dimethyl silicone oil and nano active calcium carbonate according to the proportion of 2: (3-5), kneading for 2 hours under the conditions that the vacuum degree is more than 0.08MPa and the temperature is 110 ℃, cooling, and adding the mixture into a kneader according to the ratio of 3: 2: 1: 1:1, adding hydrophilic fumed silica, black paste, a cross-linking agent, a coupling agent and a catalyst, vacuumizing and uniformly stirring, and subpackaging to obtain a component B;
and mixing the component A and the component B according to the mass ratio of 1:1 to obtain the double-component condensed type room temperature vulcanized silicone rubber.
2. The method of claim 1, wherein the coupling agent is one or more of γ -aminopropyltriethoxysilane, γ -aminopropyltrimethoxysilane, γ - β - (aminoethyl) - γ -aminopropyltrimethoxysilane, and 3- (2, 3-glycidoxy) propyltrimethoxysilane.
3. The method of claim 1, wherein the cross-linking agent is one or more selected from the group consisting of methyltrimethoxysilane, vinyltrimethoxysilane, tetraethoxysilane and polyethyl silicate.
4. The method of claim 1, wherein the catalyst is one or more of dioctyltin dilaurate and dibutyltin dilaurate.
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CN202010569400.XA CN113817438A (en) | 2020-06-20 | 2020-06-20 | Preparation method of bi-component condensed type room temperature vulcanized silicone rubber |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116515387A (en) * | 2022-10-12 | 2023-08-01 | 中国航发北京航空材料研究院 | Low-internal-stress high-weather-resistance wave-absorbing coating and preparation method thereof |
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2020
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116515387A (en) * | 2022-10-12 | 2023-08-01 | 中国航发北京航空材料研究院 | Low-internal-stress high-weather-resistance wave-absorbing coating and preparation method thereof |
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Application publication date: 20211221 |