CN114921222A - Fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant and preparation method thereof - Google Patents

Fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant and preparation method thereof Download PDF

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CN114921222A
CN114921222A CN202210426540.0A CN202210426540A CN114921222A CN 114921222 A CN114921222 A CN 114921222A CN 202210426540 A CN202210426540 A CN 202210426540A CN 114921222 A CN114921222 A CN 114921222A
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hydrogen
silicone oil
heat
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vinyl
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任林峰
洪志学
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Guangdong Sirnice Industrial Co ltd
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Guangdong Sirnice Industrial Co ltd
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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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    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
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    • C—CHEMISTRY; METALLURGY
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    • 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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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • 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
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
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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
    • C08K2003/2265—Oxides; Hydroxides of metals of iron
    • C08K2003/2272—Ferric oxide (Fe2O3)
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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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
    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention belongs to the technical field of organic silicon pouring sealants, and particularly relates to an organic silicon pouring sealant with fire resistance, heat conduction, high strength and stable performance and a preparation method thereof. The organic silicon pouring sealant with the characteristics of fire prevention, heat conduction, high strength and stable performance further ensures the heat conduction and the fire prevention of electronic components, has high performance strength, and improves the protection capability of colloid on the electronic components.

Description

Fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant and preparation method thereof
Technical Field
The invention belongs to the technical field of organic silicon pouring sealants, and particularly relates to an organic silicon pouring sealant with fire resistance, heat conduction, high strength and stable performance and a preparation method thereof.
Background
The organic silicon pouring sealant is a type of electronic pouring sealant made of silicon rubber, and comprises a single-component organic silicon pouring sealant and a double-component organic silicon pouring sealant. Silicone casting compounds are generally soft and elastic. The types of the organic silicon pouring sealant are various, and different types of organic silicon pouring sealants have great differences in temperature resistance, waterproof performance, insulating performance, optical performance, adhesion performance to different materials, hardness and the like. The organic silicon pouring sealant can be added with some functional fillers to endow the organic silicon pouring sealant with the performances of electric conduction, heat conduction, magnetic conduction and the like.
At present, the requirements of pouring sealant products on flame retardance are more and more strict, and as the performance of a plurality of pouring sealant products is unstable, the longer the storage time is, the lower the flame retardance and the heat conduction system are, and the difference of the consistency of the sealant is obvious.
Disclosure of Invention
The invention aims to provide a fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant and a preparation method thereof, and aims to solve the technical problems that the longer the pouring sealant in the prior art is stored, the flame retardance and the heat-conducting system are reduced, and the difference of the colloid consistency is obvious.
In order to achieve the above object, an organic silicon pouring sealant with fire resistance, heat conduction, high strength and stable performance provided by the embodiment of the invention comprises:
the component A comprises the following raw materials in percentage by mass: 40-45% of vinyl gel, 15-20% of vinyl silicone oil, 0.1-2% of catalyst, 8-15% of first heat-conducting agent, 20-35% of first modified flame retardant and 0.3-0.9% of first coupling agent; and
the component B comprises the following raw materials in percentage by mass: 45-55% of hydrogen-containing gel, 7-15% of first hydrogen-containing silicone oil, 3-8% of second hydrogen-containing silicone oil, 0.05-0.5% of inhibitor, 15-25% of second heat-conducting agent, 0.3-1.0% of second coupling agent and 15-25% of second modified flame retardant.
Optionally, the first modified flame retardant and/or the second modified flame retardant is selected from any one or more than one of modified aluminum hydroxide, MCA flame retardant, modified magnesium hydroxide and aluminum hydroxide/platinum complex; the particle size of the first modified flame retardant and/or the second modified flame retardant is 1-5 μm; the first heat-conducting agent and/or the second heat-conducting agent is/are selected from any one or a mixture of more than one of iron oxide, nano cerium oxide or aluminum oxide, and the particle size of the first heat-conducting agent and/or the second heat-conducting agent is 5-15 mu m.
Optionally, the vinyl gel comprises the following raw materials: 60-70% of vinyl-terminated silicone oil, 15-25% of dimethyl polydimethylsiloxane, 0.3-0.5% of KH-570 and 8-15% of silicon micropowder; the viscosity of the dimethyl polydimethylsiloxane is 50cs, and the particle size of the silicon micro powder is 1-3 mu m.
Optionally, the hydrogen-containing gel comprises the following raw materials: 55-64% of hydrogen-containing silicone oil, 20-25% of dimethyl polydimethylsiloxane, 0.1-0.3% of KH-570 and 15-20% of silicon micropowder; the viscosity of the dimethyl polydimethylsiloxane is 50 cs; the particle size of the silicon micro powder is 1-3 μm.
Optionally, the hydrogen content of the first hydrogen-containing silicone oil is 0.2-0.3%; the hydrogen content of the second hydrogen-containing silicone oil is 0.4-0.5%.
Optionally, the vinyl silicone oil has a vinyl content of 1.0-1.5% and a viscosity of 250-500 mpa.s.
Optionally, the catalyst is a platinum vinyl siloxane complex with the platinum content of 3000-5000 ppm; the first coupling agent and/or the second coupling agent is/are selected from any one or a mixture of more than one of KH550, KH560 or KH 570; the inhibitor is any one or more than one of 1-ethynyl-1-cyclohexanol, 2-methyl-1-hexynyl-3-alcohol and 2-methyl-3-hexynyl-2-alcohol.
Optionally, the mass ratio of the component A to the component B is 1: 1.
in order to achieve the purpose, the preparation method of the fireproof heat-conducting organosilicon pouring sealant with high strength and stable performance provided by the embodiment of the invention comprises the following steps:
1) preparing a component A: adding the vinyl silicone oil and the first heat-conducting agent in a ratio into a planetary stirrer for dispersing and stirring, heating to 100-105 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 60-90 minutes, adding the vinyl gel in the ratio, continuing to vacuumize and stir for 20-30 minutes, adding the first modified flame retardant and the first coupling agent in the ratio, continuing to vacuumize and stir for 30-60 minutes, cooling to 40-50 ℃, adding the catalyst in the ratio, continuing to vacuumize and stir for 30-40 minutes, cooling, discharging, and obtaining the component A;
2) preparing a component B: and (3) putting the first hydrogen-containing silicone oil, the second hydrogen-containing silicone oil and the second heat-conducting agent into a planetary stirrer for dispersion stirring, heating to 100-105 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 60-90 minutes, adding the hydrogen-containing gel, continuing to vacuumize and stir for 20-30 minutes, adding the second modified flame retardant and the second coupling agent, continuing to vacuumize and stir for 30-60 minutes, cooling to 40-50 ℃, adding an inhibitor, continuing to vacuumize and stir for 30-40 minutes, cooling and discharging to obtain the component B.
Optionally, the preparation method of the fireproof heat-conducting high-strength stable-performance organosilicon potting adhesive further comprises the following steps:
3) preparation of hydrogen-containing gel: fully kneading hydrogen-containing silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder at 90-120 ℃ for 90-120 minutes to obtain uniform gel, namely the hydrogen-containing gel;
4) preparation of vinyl gel: the vinyl-terminated silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 90-120 minutes at the temperature of 100-130 ℃ to obtain uniform gel, namely vinyl gel.
The organic silicon pouring sealant with fire resistance, heat conduction, high strength and stable performance and the preparation method thereof provided by the embodiment of the invention have at least one of the following technical effects: this organosilicon casting glue that fire prevention heat conduction high strength performance is stable passes through first modified fire retardant and the second modified fire retardant through surface treatment, great improvement the dispersion effect, thereby improve the whole fire-retardant effect of colloid, realize the heat conduction function through first heat-conducting agent and second heat-conducting agent, further avoid the emergence of incident, also avoided current technology to bring the dispenser to dissolve the problem mutually and serious inhomogeneous and subside that lead to simultaneously, make product property ability unstable and the inconsistent phenomenon of glue solution performance. The organic silicon pouring sealant with the characteristics of fire prevention, heat conduction, high strength and stable performance further ensures the heat conduction and the fire prevention of electronic components, has high performance strength, and improves the protection capability of colloid on the electronic components.
Detailed Description
The present invention will be further described with reference to the following examples, but the embodiments of the present invention are not limited thereto.
In the embodiment of the invention, the fireproof heat-conducting organosilicon pouring sealant with high strength and stable performance is provided, and comprises a component A and a component B.
The component A comprises the following raw materials in percentage by mass: 40-45% of vinyl gel, 15-20% of vinyl silicone oil, 0.1-2% of catalyst, 8-15% of first heat-conducting agent, 20-35% of first modified flame retardant and 0.3-0.9% of first coupling agent.
The component B comprises the following raw materials in percentage by mass: 45-55% of hydrogen-containing gel, 7-15% of first hydrogen-containing silicone oil, 3-8% of second hydrogen-containing silicone oil, 0.05-0.5% of inhibitor, 15-25% of second heat-conducting agent, 0.3-1.0% of second coupling agent and 15-25% of second modified flame retardant.
This organosilicon casting glue that fire prevention heat conduction high strength performance is stable passes through first modified fire retardant and the second modified fire retardant through surface treatment, great improvement the dispersion effect, thereby improve the whole fire-retardant effect of colloid, realize the heat conduction function through first heat-conducting agent and second heat-conducting agent, further avoid the emergence of incident, also avoided current technology to bring the dispenser to dissolve the problem mutually and serious inhomogeneous and subside that lead to simultaneously, make product property ability unstable and the inconsistent phenomenon of glue solution performance. The organic silicon pouring sealant with the fireproof, heat-conducting, high-strength and stable performance further ensures the heat-conducting and fireproof performances of electronic components, has high performance strength, and improves the protective capability of colloid on the electronic components.
In the embodiment of the invention, the first modified flame retardant and/or the second modified flame retardant is selected from any one or more than one of modified aluminum hydroxide, MCA flame retardant, modified magnesium hydroxide and aluminum hydroxide/platinum complex. The particle size of the first modified flame retardant and/or the second modified flame retardant is 1 to 5 μm, and specifically may be 1 μm, 3 μm, or 5 μm. The first heat conducting agent and/or the second heat conducting agent is/are selected from one or more of iron oxide, nano cerium oxide and aluminum oxide, and the particle size of the first heat conducting agent and/or the second heat conducting agent is 5-15 μm, specifically 5 μm, 10 μm or 15 μm.
In an embodiment of the present invention, the vinyl gel comprises the following raw materials: 60-70% of vinyl-terminated silicone oil, 15-25% of dimethyl polydimethylsiloxane, 0.3-0.5% of KH-570 and 8-15% of silicon micropowder. The viscosity of dimethyl polydimethylsiloxane was 50 cs. The particle diameter of the silicon micropowder is 1-3 μm, specifically 1 μm, 2 μm or 3 μm.
In an embodiment of the invention, the hydrogen-containing gel comprises the following raw materials: 55-64% of hydrogen-containing silicone oil, 20-25% of dimethyl polydimethylsiloxane, 0.1-0.3% of KH-570 and 15-20% of silicon micropowder; the viscosity of dimethyl polydimethylsiloxane is 50 cs; the grain diameter of the silicon micro powder is 1-3 μm.
In the embodiment of the present invention, the hydrogen content of the first hydrogen-containing silicone oil is 0.2 to 0.3%, specifically, 0.2%, 0.25%, or 0.3%. The hydrogen content of the second hydrogen-containing silicone oil is 0.4-0.5%, specifically 0.4%, 0.45% or 0.5%.
In the embodiment of the present invention, the vinyl silicone oil has a vinyl content of 1.0 to 1.5%, specifically 1%, 1.2%, or 1.5%. The viscosity of the vinyl silicone oil is 250-500mpa.s, and specifically 250mpa.s, 300mpa.s, 400mpa.s or 500 mpa.s.
In the examples of the invention, the catalyst is a complex of platinum vinylsiloxane with a platinum content of 3000-5000 ppm. The first coupling agent and/or the second coupling agent is/are selected from any one or a mixture of more than one of KH550, KH560 or KH 570. The inhibitor is selected from one or more of 1-ethynyl-1-cyclohexanol, 2-methyl-1-hexynyl-3-alcohol, and 2-methyl-3-hexynyl-2-alcohol.
In the embodiment of the invention, the mass ratio of the component A to the component B is 1: 1.
the embodiment of the invention also provides a preparation method of the fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant, which comprises the following steps:
1) preparing a component A: adding the vinyl silicone oil and the first heat-conducting agent in proportion into a planetary stirrer for dispersing and stirring, heating to 100-105 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 60-90 minutes, adding the vinyl gel in proportion, continuing to vacuumize and stir for 20-30 minutes, adding the first modified flame retardant and the first coupling agent in proportion, continuing to vacuumize and stir for 30-60 minutes, cooling to 40-50 ℃, adding the catalyst in proportion, continuing to vacuumize and stir for 30-40 minutes, cooling, and discharging to obtain the component A.
2) Preparing a component B: and (3) putting the first hydrogen-containing silicone oil, the second hydrogen-containing silicone oil and the second heat-conducting agent into a planetary stirrer for dispersion and stirring, heating to 100-105 ℃, starting vacuum to be below 0.095MPa, stirring for 60-90 minutes at constant temperature, adding the hydrogen-containing gel, continuing to vacuumize and stir for 20-30 minutes, adding the second modified flame retardant and the second coupling agent, continuing to stir for 30-60 minutes in vacuum, cooling to 40-50 ℃, adding an inhibitor, continuing to stir for 30-40 minutes in vacuum, cooling, and discharging to obtain the component B.
In the embodiment of the invention, the preparation method of the fireproof heat-conducting high-strength stable-performance organosilicon potting adhesive further comprises the following steps:
3) preparation of hydrogen-containing gel: fully kneading hydrogen-containing silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micro powder at 90-120 ℃ for 90-120 minutes to obtain uniform gel, namely the hydrogen-containing gel.
4) Preparation of vinyl gel: the vinyl-terminated silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 90-120 minutes at the temperature of 100-130 ℃ to obtain uniform gel, namely vinyl gel.
For a further understanding of the present invention, reference will now be made to the following preferred embodiments of the invention in conjunction with the examples, but it is to be understood that the description is intended to further illustrate the features and advantages of the invention and is not intended to limit the scope of the claims which follow.
The fireproof heat-conducting high-strength stable-performance organosilicon pouring sealant of embodiments 1-5 is composed of a component A and a component B, wherein the mass ratio of the component A to the component B is 1: 1.
see table 1 for the feed of the a component of examples 1-5, table 2 for the feed of the B component of examples 1-5, table 3 for the feed of the vinyl gel of examples 1-5, and table 4 for the feed of the hydrogen-containing gel of examples 1-5.
TABLE 1
Figure BDA0003608683160000061
TABLE 2
Examples 1 2 3 4 5
Hydrogen-containing gel (%) 45 45 50 55 46
First Hydrogen-containing Silicone oil (%) 7 8 15 7 8
Second Hydrogen-containing Silicone oil (%) 7.5 5 3 6.95 8
Inhibitor (%) 0.2 0.5 0.1 0.05 0.3
Second heat-conducting agent (%) 25 16 15 15 17
Second coupling agent (%) 0.3 0.5 0.4 1 0.7
Second modified flame retardant (%) 15 25 16.5 15 20
TABLE 3
Examples 1 2 3 4 5
Terminal vinyl Silicone oil (%) 60 62 65 68 70
Dimethylpolydimethylsiloxane (%) 25 24.6 25 16.5 15
KH-570(％) 0.5 0.4 0.5 0.5 0.3
Silica micropowder (%) 14.5 13 9.5 15 8
TABLE 4
Examples 1 2 3 4 5
Hydrogen-containing silicone oil (%) 55 57 60 63 64
Dimethyl polydimethylsiloxane (%) 24.7 25 22 20 20.9
KH-570(％) 0.3 0.2 0.3 0.2 0.1
Silicon micropowder (%) 20 17.8 17.7 16.8 15
Examples 1 to 2
The preparation method of the fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant comprises the following steps:
1) preparation of hydrogen-containing gel: the hydrogen-containing silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 120 minutes at 90 ℃ to obtain uniform gel, namely the hydrogen-containing gel.
2) Preparation of vinyl gel: the vinyl-terminated silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 120 minutes at 100 ℃ to obtain uniform gel, namely vinyl gel.
3) Preparing a component A: adding the vinyl silicone oil and the first heat-conducting agent in proportion into a planetary stirrer for dispersing and stirring, heating to 100 ℃, starting vacuum to be below 0.095MPa, stirring for 90 minutes at constant temperature, adding the vinyl gel in proportion, continuing to vacuumize and stir for 30 minutes, adding the first modified flame retardant and the first coupling agent in proportion, continuing to vacuumize and stir for 60 minutes, cooling to 40 ℃, adding the catalyst in proportion, continuing to vacuumize and stir for 40 minutes, cooling, and discharging to obtain the component A.
4) Preparing a component B: and (3) putting the first hydrogen-containing silicone oil, the second hydrogen-containing silicone oil and the second heat-conducting agent into a planetary stirrer for dispersing and stirring, heating to 100 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 90 minutes, adding the hydrogen-containing gel, continuing vacuumizing and stirring for 30 minutes, adding the second modified flame retardant and the second coupling agent, continuing vacuum stirring for 60 minutes, cooling to 40 ℃, adding the inhibitor, continuing vacuum stirring for 40 minutes, cooling, and discharging to obtain the component B.
Example 3
The preparation method of the fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant comprises the following steps:
1) preparation of hydrogen-containing gel: the hydrogen-containing silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 100 minutes at 110 ℃ to obtain uniform gel, namely the hydrogen-containing gel.
2) Preparation of vinyl gel: the vinyl-terminated silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 110 minutes at 120 ℃ to obtain uniform gel, namely vinyl gel.
3) Preparing a component A: adding the vinyl silicone oil and the first heat-conducting agent in a ratio into a planetary stirrer for dispersing and stirring, heating to 102 ℃, starting vacuum to be below 0.095MPa, stirring at a constant temperature for 75 minutes, adding the vinyl gel in a ratio, continuing to vacuumize and stir for 25 minutes, adding the first modified flame retardant and the first coupling agent in a ratio, continuing to vacuumize and stir for 45 minutes, cooling to 45 ℃, adding the catalyst in a ratio, continuing to vacuumize and stir for 35 minutes, cooling, and discharging to obtain the component A.
4) Preparing a component B: and (3) putting the first hydrogen-containing silicone oil, the second hydrogen-containing silicone oil and the second heat-conducting agent into a planetary stirrer for dispersing and stirring, heating to 102 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 75 minutes, adding the hydrogen-containing gel, continuing vacuumizing and stirring for 25 minutes, adding the second modified flame retardant and the second coupling agent, continuing vacuum stirring for 45 minutes, cooling to 45 ℃, adding the inhibitor, continuing vacuum stirring for 35 minutes, cooling, and discharging to obtain the component B.
Examples 4 to 5
The preparation method of the fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant comprises the following steps:
1) preparation of hydrogen-containing gel: the hydrogen-containing silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 90 minutes at 120 ℃ to obtain uniform gel, namely the hydrogen-containing gel.
2) Preparation of vinyl gel: the vinyl-terminated silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 90 minutes at 130 ℃ to obtain uniform gel, namely vinyl gel.
3) Preparing a component A: adding the vinyl silicone oil and the first heat-conducting agent in proportion into a planetary stirrer for dispersion and stirring, heating to 105 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 60 minutes, adding the vinyl gel in proportion, continuing to stir for 20 minutes in a vacuum-pumping manner, adding the first modified flame retardant and the first coupling agent in proportion, continuing to stir in a vacuum-pumping manner for 30 minutes, cooling to 50 ℃, adding the catalyst in proportion, continuing to stir in a vacuum-pumping manner for 30 minutes, cooling, and discharging to obtain the component A.
4) Preparing a component B: and (3) putting the first hydrogen-containing silicone oil, the second hydrogen-containing silicone oil and the second heat-conducting agent into a planetary stirrer for dispersing and stirring, heating to 105 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 60 minutes, adding the hydrogen-containing gel, continuing vacuumizing and stirring for 20 minutes, adding the second modified flame retardant and the second coupling agent, continuing vacuum stirring for 30 minutes, cooling to 50 ℃, adding the inhibitor, continuing vacuum stirring for 30 minutes, cooling, and discharging to obtain the component B.
The silicone pouring sealant with stable fire-proof, heat-conducting, high-strength and stable performance prepared in examples 1-5 was stored for one month, and tested for flame retardancy, elongation at break, tensile strength, thermal conductivity and hardness, and the test results are shown in table 5.
TABLE 5
Figure BDA0003608683160000091
Figure BDA0003608683160000101
The data prove that the prepared vinyl gel and hydrogen-based gel are used for preparing the organic silicon pouring sealant, and the organic silicon pouring sealant has the performance characteristics of stable fire resistance, heat conduction and high strength and is uniformly distributed. Meanwhile, the phenomena of unstable performance and reduction caused by sedimentation are perfectly solved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. Organosilicon casting glue of fire prevention heat conduction high strength stable performance, its characterized in that includes:
the component A comprises the following raw materials in percentage by mass: 40-45% of vinyl gel, 15-20% of vinyl silicone oil, 0.1-2% of catalyst, 8-15% of first heat-conducting agent, 20-35% of first modified flame retardant and 0.3-0.9% of first coupling agent; and
the component B comprises the following raw materials in percentage by mass: 45-55% of hydrogen-containing gel, 7-15% of first hydrogen-containing silicone oil, 3-8% of second hydrogen-containing silicone oil, 0.05-0.5% of inhibitor, 15-25% of second heat-conducting agent, 0.3-1.0% of second coupling agent and 15-25% of second modified flame retardant.
2. The silicone pouring sealant with fire prevention, heat conduction, high strength and stable performance as claimed in claim 1, wherein the first modified flame retardant and/or the second modified flame retardant is selected from any one or more of modified aluminum hydroxide, MCA flame retardant, modified magnesium hydroxide, aluminum hydroxide/platinum complex; the particle size of the first modified flame retardant and/or the second modified flame retardant is 1-5 μm; the first heat-conducting agent and/or the second heat-conducting agent is/are selected from any one or a mixture of more than one of iron oxide, nano cerium oxide or aluminum oxide, and the particle size of the first heat-conducting agent and/or the second heat-conducting agent is 5-15 mu m.
3. The silicone pouring sealant with characteristics of fire prevention, heat conduction, high strength and stable performance as claimed in claim 1, wherein the vinyl gel comprises the following raw materials: 60-70% of vinyl-terminated silicone oil, 15-25% of dimethyl polydimethylsiloxane, 0.3-0.5% of KH-570 and 8-15% of silicon micropowder; the viscosity of the dimethyl polydimethylsiloxane is 50cs, and the particle size of the silicon micro powder is 1-3 mu m.
4. The silicone pouring sealant with fire prevention, heat conduction, high strength and stable performance as claimed in claim 1, wherein the hydrogen-containing gel comprises the following raw materials: 55-64% of hydrogen-containing silicone oil, 20-25% of dimethyl polydimethylsiloxane, 0.1-0.3% of KH-570 and 15-20% of silicon micropowder; the viscosity of the dimethyl polydimethylsiloxane is 50 cs; the particle size of the silicon micro powder is 1-3 μm.
5. The silicone pouring sealant with stable fire prevention, heat conduction, high strength and performance as claimed in claim 1, wherein the hydrogen content of the first hydrogen-containing silicone oil is 0.2-0.3%; the hydrogen content of the second hydrogen-containing silicone oil is 0.4-0.5%.
6. The silicone pouring sealant with fire prevention, heat conduction, high strength and stable performance as claimed in any one of claims 1 to 5, wherein the vinyl silicone oil has a vinyl content of 1.0 to 1.5% and a viscosity of 250-500 mpa.s.
7. The silicone pouring sealant with fire prevention, heat conduction, high strength and stable performance as claimed in any one of claims 1-5, wherein the catalyst is a platinum vinyl siloxane complex with platinum content of 3000-5000 ppm; the first coupling agent and/or the second coupling agent is/are selected from any one or a mixture of more than one of KH550, KH560 or KH 570; the inhibitor is selected from any one or more than one of 1-ethynyl-1-cyclohexanol, 2-methyl-1-hexynyl-3-alcohol and 2-methyl-3-hexynyl-2-alcohol.
8. The fireproof heat-conducting high-strength stable-performance organosilicon pouring sealant according to any one of claims 1-5, wherein the mass ratio of the component A to the component B is 1: 1.
9. the preparation method of the fireproof heat-conducting high-strength stable-performance organosilicon pouring sealant according to any one of claims 1 to 8, characterized by comprising the following steps:
1) preparing a component A: adding the vinyl silicone oil and the first heat-conducting agent in a ratio into a planetary stirrer for dispersing and stirring, heating to 100-105 ℃, starting vacuum to be below 0.095MPa, stirring at constant temperature for 60-90 minutes, adding the vinyl gel in the ratio, continuing to vacuumize and stir for 20-30 minutes, adding the first modified flame retardant and the first coupling agent in the ratio, continuing to vacuumize and stir for 30-60 minutes, cooling to 40-50 ℃, adding the catalyst in the ratio, continuing to vacuumize and stir for 30-40 minutes, cooling, discharging, and obtaining the component A;
2) preparing a component B: and (3) putting the first hydrogen-containing silicone oil, the second hydrogen-containing silicone oil and the second heat-conducting agent into a planetary stirrer for dispersion and stirring, heating to 100-105 ℃, starting vacuum to be below 0.095MPa, stirring for 60-90 minutes at constant temperature, adding the hydrogen-containing gel, continuing to vacuumize and stir for 20-30 minutes, adding the second modified flame retardant and the second coupling agent, continuing to stir for 30-60 minutes in vacuum, cooling to 40-50 ℃, adding an inhibitor, continuing to stir for 30-40 minutes in vacuum, cooling, and discharging to obtain the component B.
10. The preparation method of the fireproof heat-conducting high-strength stable-performance organosilicon pouring sealant according to claim 9, characterized by further comprising the following steps:
3) preparation of hydrogen-containing gel: fully kneading hydrogen-containing silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder at 90-120 ℃ for 90-120 minutes to obtain uniform gel, namely the hydrogen-containing gel;
4) preparation of vinyl gel: the vinyl-terminated silicone oil, dimethyl polydimethylsiloxane and KH-570 modified silicon micropowder are fully kneaded for 90-120 minutes at the temperature of 100-130 ℃ to obtain uniform gel, namely vinyl gel.
CN202210426540.0A 2022-04-21 2022-04-21 Fireproof heat-conducting high-strength stable-performance organic silicon pouring sealant and preparation method thereof Pending CN114921222A (en)

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CN103131381A (en) * 2013-03-06 2013-06-05 广州市高士实业有限公司 High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof
CN107793992A (en) * 2017-11-01 2018-03-13 杭州之江有机硅化工有限公司 A kind of additional organosilicon casting glue and preparation method thereof
CN107892898A (en) * 2017-11-09 2018-04-10 南京科孚纳米技术有限公司 A kind of preparation method of high heat conduction low-gravity flame-proof organosilicon casting glue
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CN103131381A (en) * 2013-03-06 2013-06-05 广州市高士实业有限公司 High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof
CN107793992A (en) * 2017-11-01 2018-03-13 杭州之江有机硅化工有限公司 A kind of additional organosilicon casting glue and preparation method thereof
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* Cited by examiner, † Cited by third party
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CN115491171A (en) * 2022-10-28 2022-12-20 广东施奈仕实业有限公司 High-temperature-aging-resistant organic silicon pouring sealant and preparation method thereof
CN115491171B (en) * 2022-10-28 2024-04-19 广东施奈仕实业有限公司 High-temperature aging resistant organic silicon pouring sealant and preparation method thereof

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