CN116694298A - Heat-conducting oil-resistant fluorosilicone pouring sealant and preparation method thereof - Google Patents

Heat-conducting oil-resistant fluorosilicone pouring sealant and preparation method thereof Download PDF

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Publication number
CN116694298A
CN116694298A CN202310690287.4A CN202310690287A CN116694298A CN 116694298 A CN116694298 A CN 116694298A CN 202310690287 A CN202310690287 A CN 202310690287A CN 116694298 A CN116694298 A CN 116694298A
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fluorosilicone
oil
component
heat
pouring sealant
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Inventor
高欣
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Wuhu Fusier Aviation Materials Co ltd
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Wuhu Fusier Aviation Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The application discloses a heat-conducting oil-resistant fluorosilicone pouring sealant, which consists of a fluorosilicone A component and a fluorosilicone B component, wherein the fluorosilicone A component consists of vinyl fluorosilicone oil, a hydrophobic heat-conducting filler F1 and a platinum catalyst, the fluorosilicone B component consists of hydrogen-containing fluorosilicone oil and a hydrophobic heat-conducting filler F2, the fluorosilicone A component and the fluorosilicone B component are uniformly mixed according to the mass ratio of 1:0.5-1.5, and cured for 2-24 hours at room temperature to obtain a cured adhesive, the heat conductivity coefficient of the cured adhesive is 0.6-1.5W/(m.K), and the volume expansion rate of the cured adhesive in gasoline is not higher than 50%. The heat-conducting oil-resistant fluorosilicone pouring sealant can meet the requirement of pouring and sealing electronic products in severe environments, prevents electronic devices from being corroded by oil, acid and alkali and corrosive chemicals, and has good heat dissipation effect.

Description

Heat-conducting oil-resistant fluorosilicone pouring sealant and preparation method thereof
Technical Field
The application belongs to the technical field of high polymer materials, and particularly relates to a heat-conducting oil-resistant fluorosilicone pouring sealant and a preparation method thereof.
Background
With the rapid development of electronic information technology, electronic components develop to be small, dense and light, so that the heat dissipation problem is outstanding, and the pouring sealant of electronic products with high heat conduction is widely focused.
The electronic pouring sealant has very many types, and three types of epoxy resin pouring sealant, organic silicon pouring sealant and polyurethane pouring sealant are common. Before being cured, the epoxy resin composite material is liquid, has fluidity, and can play roles in water resistance, moisture resistance, dust resistance, insulation, heat conduction, vibration resistance and the like after being cured. The organic silicon pouring sealant has excellent electrical insulation and high and low temperature resistance, and is specially used for coating, pouring protection and the like of waterproof, moistureproof and gas pollution prevention of precision electronic components, automobile electronic modules, LED power supply driving modules, solar component junction boxes, electric vehicle charging column modules, lithium battery packs, capacitor packs, magnetic induction coils, inverter power supplies and the like. The common organic silicon pouring sealant has poor oil resistance and chemical corrosion resistance, and is difficult to be used in the occasions contacted with oil and chemicals.
Therefore, a pouring sealant product which can meet the pouring of electronic products in severe environments, prevent the electronic devices from being corroded by oil, acid and alkali and corrosive chemicals and has good heat dissipation effect is needed.
Disclosure of Invention
The application aims to solve the problems and provide the heat-conducting oil-resistant fluorosilicone pouring sealant which can be used for pouring and sealing electronic products in severe environments, so that the electronic devices are prevented from being corroded by oil, acid and alkali and corrosive chemicals, and meanwhile, the heat-conducting oil-resistant fluorosilicone pouring sealant has a good heat dissipation effect.
The purpose of the application is realized in the following way:
the application provides a heat-conducting oil-resistant fluorosilicone pouring sealant which consists of a fluorosilicone A component and a fluorosilicone B component, wherein the fluorosilicone A component consists of the following components in parts by weight:
100 parts of vinyl fluorosilicone oil;
50-200 parts of hydrophobic heat-conducting filler F;
0.01-0.5 part of platinum catalyst;
the fluorine silicon B component consists of the following components in parts by weight:
100 parts of hydrogen-containing fluorosilicone oil;
50-200 parts of hydrophobic heat-conducting filler F2;
the viscosity of the vinyl fluorosilicone oil is 200-5000 mPa.s, and the chemical structural formula of the vinyl fluorosilicone oil is shown in formula 1:
wherein a is an integer of 30-300, and b is an integer of 0-50;
the viscosity of the hydrogen-containing fluorosilicone oil is 200-5000 mPa.s, and the chemical structural formula of the hydrogen-containing fluorosilicone oil is shown as formula 2:
wherein x is an integer of 30-300, y is an integer of 0-50, and z is an integer of 0-10.
The above fluorosilicone pouring sealant, wherein the hydrophobic heat conductive filler F1 is silicon carbide, silicon nitride, boron nitride or aluminum hydroxide treated with hydroxy fluorosilicone oil, hydroxy silicone oil or hexamethyldisilazane.
The fluorosilicone pouring sealant, wherein the heat conductivity coefficient of the hydrophobic heat conducting filler F1 is more than 10W/(m.K), and the average particle size is 20-50 mu m.
The above fluorosilicone pouring sealant, wherein the hydrophobic heat conductive filler F2 is silicon carbide, silicon nitride, boron nitride or aluminum hydroxide treated with hydroxy fluorosilicone oil, hydroxy silicone oil or hexamethyldisilazane.
The fluorosilicone pouring sealant, wherein the heat conductivity coefficient of the hydrophobic heat conducting filler F2 is more than 10W/(m.K), and the average particle size is 1-20 mu m.
The fluorosilicone pouring sealant, wherein the platinum catalyst is selected from Karstedt's catalyst, and the effective content of platinum is 1000-10000ppm.
The fluorine-silicon pouring sealant has the density of the fluorine-silicon A component of 1.40-2.0g/cm 3 The viscosity is 3000-10000 mPa.s; the density of the fluorosilicone B component is 1.40-2.0g/cm 3 The viscosity is 3000-10000 mPa.s.
The fluorine-silicon pouring sealant comprises the fluorine-silicon A component and the fluorine-silicon B component in a mass ratio of 1:0.5-1.5.
The application also provides a preparation method of the heat-conducting oil-resistant fluorosilicone pouring sealant, which comprises the following steps:
step 1: uniformly dispersing a certain amount of vinyl fluorosilicone oil and a hydrophobic heat-conducting filler F1, then adding a platinum catalyst, and uniformly mixing to obtain a fluorosilicone A component;
step 2: uniformly dispersing a certain amount of hydrogen-containing fluorosilicone oil and hydrophobic heat-conducting filler F2 to obtain a fluorosilicone B component;
step 3: uniformly mixing the fluorosilicone A component prepared in the step 1 and the fluorosilicone B component prepared in the step 2 according to the mass ratio of 1:0.5-1.5, and curing at room temperature for 2-24 hours to obtain the curing adhesive.
According to the preparation method, the thermal conductivity coefficient of the cured adhesive prepared in the step 3 is 0.6-1.5W/(m.K), and the volume expansion rate of the cured adhesive in gasoline is not higher than 50%.
The curing principle of the heat-conducting oil-resistant fluorosilicone pouring sealant is as follows: the difunctional vinyl fluorosilicone oil and the polyfunctional hydrogen-containing fluorosilicone oil undergo hydrosilylation reaction under the catalysis of a platinum catalyst to form a three-dimensional crosslinked network structure.
In the heat-conducting oil-resistant fluorosilicone pouring sealant, after the heat-conducting filler is subjected to hydrophobic modification, the dispersion performance of the heat-conducting filler in a system is improved, and the tackifying effect is reduced; the filler system with double particle size distribution in the curing system shows better heat conduction effect.
Compared with the common organic silicon pouring sealant, the heat-conducting oil-resistant fluorosilicone pouring sealant has the advantages that the introduction of fluorine-containing groups effectively improves the performances of oil resistance, stain resistance, acid and alkali resistance, chemical corrosion resistance and the like of the pouring sealant.
Detailed Description
In order that those skilled in the art will better understand the present application, a technical solution in the embodiments of the present application will be clearly and completely described below, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present application without making any inventive effort, shall fall within the scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and in the claims are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate in order to describe the embodiments of the application herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In this example, the choice of each component is only one choice, and can be replaced with the same chemical properties and composition.
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The present application will be described in detail with reference to examples.
The application relates to a preparation method of a heat-conducting oil-resistant fluorosilicone pouring sealant, which comprises the following steps of
Step 1: uniformly dispersing a certain amount of vinyl fluorosilicone oil and a hydrophobic heat-conducting filler F1, then adding a platinum catalyst, and uniformly mixing to obtain a fluorosilicone A component;
step 2: uniformly dispersing a certain amount of hydrogen-containing fluorosilicone oil and hydrophobic heat-conducting filler F2 to obtain a fluorosilicone B component;
step 3: uniformly mixing the fluorosilicone A component prepared in the step 1 and the fluorosilicone B component prepared in the step 2 according to the mass ratio of 1:0.5-1.5, and curing at room temperature for 2-24 hours to obtain the curing adhesive.
The fluorine-silicon component A consists of the following components in parts by weight:
100 parts of vinyl fluorosilicone oil;
50-200 parts of hydrophobic heat-conducting filler F;
0.01-0.5 part of platinum catalyst;
the fluorine silicon B component consists of the following components in parts by weight:
100 parts of hydrogen-containing fluorosilicone oil;
50-200 parts of hydrophobic heat-conducting filler F2.
The viscosity of the vinyl fluorosilicone oil is 200-5000 mPa.s, and the chemical structural formula is shown as follows:
wherein a is an integer of 30-300, and b is an integer of 0-50;
the viscosity of the fluorine-containing silicone oil is 200-5000 mPa.s, and the chemical structural formula is shown as follows:
wherein x is an integer of 30-300, y is an integer of 0-50, and z is an integer of 0-10.
The hydrophobic heat-conducting filler F1 is silicon carbide, silicon nitride, boron nitride or aluminum hydroxide which is treated by hydroxyl fluorine silicone oil, hydroxyl silicone oil or hexamethyldisilazane, the heat conductivity coefficient of the hydrophobic heat-conducting filler F1 is more than 10W/(m.K), and the average grain diameter is 20-50 mu m.
The hydrophobic heat-conducting filler F2 is silicon carbide, silicon nitride, boron nitride or aluminum hydroxide which is treated by hydroxyl fluorosilicone oil, hydroxyl silicone oil or hexamethyldisilazane, the heat conductivity coefficient of the hydrophobic heat-conducting filler F2 is more than 10W/(m.K), and the average grain diameter is 1-20 mu m.
The platinum catalyst is selected from Karstedt catalyst, and its effective content of platinum is 1000-10000ppm.
The density of the fluorosilicone A component is 1.40-2.0g/cm 3 The viscosity is 3000-10000 mPa.s;
the density of the fluorosilicone B component is 1.40-2.0g/cm 3 The viscosity is 3000-10000 mPa.s.
Example 1:
preparation of a fluorosilicone A component: dispersing 100kg of vinyl fluorosilicone oil with viscosity of 500 mPas (a: b: 3:1) and 100kg of silicon carbide treated with hydroxy fluorosilicone oil (500 mesh) uniformly in a planetary mixer, adding 0.25kg of Karstedt catalyst (effective concentration of platinum is 4000 ppm) and mixing uniformly to obtain a density of 1.75g/cm 3 A fluorosilicone A component with the viscosity of 4000+/-500 mPa.s.
Preparation of a fluorosilicone B component: 100kg of the mixture having a viscosity of 300 mPasUniformly dispersing vinyl fluorosilicone oil (x: y: z: 3: 1: 0.03) and 100kg of hydroxyl fluorosilicone oil-treated silicon carbide (2000 mesh) in a planetary stirrer to obtain a density of 1.76g/cm 3 A fluorosilicone B component with the viscosity of 4000+/-500 mPa.s.
And mixing the fluorosilicone A component and the fluorosilicone B component according to the mass ratio of 1:1.02, and placing the mixture in a mold to cure for 4 hours at room temperature to obtain the curing adhesive.
The heat conductivity coefficient of the cured adhesive prepared in the embodiment is tested by a transient heat source method;
the cured gel prepared in this example was immersed in gasoline, kerosene and motor oil for 72 hours, respectively, and the volume expansion rate was measured.
Example 2:
preparation of a fluorosilicone A component: dispersing 100kg of vinyl fluorosilicone oil with viscosity of 800 mPas (a: b: 4:1) and 130kg of silicon carbide treated with hydroxy fluorosilicone oil (200 mesh) uniformly in a planetary mixer, adding 0.35kg of Karstedt catalyst (effective concentration of platinum is 4000 ppm) and mixing uniformly to obtain a density of 1.92g/cm 3 The viscosity of the fluorine-silicon component A is 8000+/-1000 mPa.s.
Preparation of a fluorosilicone B component: dispersing 100kg of vinyl fluorosilicone oil with viscosity of 500 mPas (x: y: z. Apprxeq.4:1:0.03) and 130kg of hydroxy fluorosilicone oil treated alumina (1000 mesh) uniformly in a planetary mixer to obtain a density of 1.93g/cm 3 And the viscosity of the fluorine-silicon B component is 7500+/-500 mPa.s.
And mixing the fluorosilicone A component and the fluorosilicone B component according to the mass ratio of 1:1.05, and placing the mixture into a mold to be cured for 3 hours at room temperature to obtain the curing adhesive.
The heat conductivity coefficient of the cured adhesive prepared in the embodiment is tested by a transient heat source method;
the cured gel prepared in this example was immersed in gasoline, kerosene and motor oil for 72 hours, respectively, and the volume expansion rate was measured.
Comparative example 1
Curing a certain organosilicon pouring sealant (LT-168, shenzhen Letian Industrial materials Co., ltd.) in the market according to the instruction to obtain a curing adhesive, and testing the heat conductivity coefficient of the curing adhesive by using a transient heat source method; the volume expansion rate was measured by immersing in gasoline, kerosene and motor oil for 72 hours, respectively.
The test results of examples 1, 2 and comparative example 1 are summarized as follows:
from the test results in the above table, it can be clearly seen that: the examples and the comparative examples both have higher thermal conductivity, but the oil resistance of the examples is far better than that of the comparative examples. This is because the matrix material polydimethylsiloxane in the comparative example is a nonpolar polymer and is not inherently oil-resistant; in the examples, fluorine-containing polysiloxane is used as a matrix, and the resin composition has good oil resistance. Therefore, the heat conduction filling adhesive provided by the application has good oil resistance and heat conduction, can be used for filling and sealing electronic products in severe environments, prevents electronic devices from being corroded by oil, acid and alkali and corrosive chemicals, and has good heat dissipation effect.
The above embodiments are provided for illustrating the present application and not for limiting the present application, and various changes and modifications may be made by one skilled in the relevant art without departing from the spirit and scope of the present application, and thus all equivalent technical solutions should be defined by the claims.

Claims (10)

1. The heat-conducting oil-resistant fluorosilicone pouring sealant is characterized by comprising a fluorosilicone A component and a fluorosilicone B component, wherein the fluorosilicone A component comprises the following components in parts by weight:
100 parts of vinyl fluorosilicone oil;
50-200 parts of hydrophobic heat-conducting filler F;
0.01-0.5 part of platinum catalyst;
the fluorine silicon B component consists of the following components in parts by weight:
100 parts of hydrogen-containing fluorosilicone oil;
50-200 parts of hydrophobic heat-conducting filler F2;
the viscosity of the vinyl fluorosilicone oil is 200-5000 mPa.s, and the chemical structural formula of the vinyl fluorosilicone oil is shown in formula 1:
wherein a is an integer of 30-300, and b is an integer of 0-50;
the viscosity of the hydrogen-containing fluorosilicone oil is 200-5000 mPa.s, and the chemical structural formula of the hydrogen-containing fluorosilicone oil is shown as formula 2:
wherein x is an integer of 30-300, y is an integer of 0-50, and z is an integer of 0-10.
2. The fluorosilicone pouring sealant according to claim 1, wherein the hydrophobic heat conductive filler F1 is silicon carbide, silicon nitride, boron nitride or aluminum hydroxide treated with hydroxy fluorosilicone oil, hydroxy silicone oil or hexamethyldisilazane.
3. The fluorosilicone pouring sealant according to claim 2, wherein the hydrophobic heat conductive filler F1 has a heat conductivity coefficient of more than 10W/(m-K) and an average particle diameter of 20-50 μm.
4. The fluorosilicone pouring sealant according to claim 1, wherein the hydrophobic heat conductive filler F2 is silicon carbide, silicon nitride, boron nitride or aluminum hydroxide treated with hydroxy fluorosilicone oil, hydroxy silicone oil or hexamethyldisilazane.
5. The fluorosilicone pouring sealant according to claim 4, wherein the hydrophobic heat conductive filler F2 has a heat conductivity of more than 10W/(m.K) and an average particle diameter of 1-20 μm.
6. The fluorosilicone pouring sealant according to claim 1, wherein the platinum catalyst is selected from Karstedt catalyst, and the effective platinum content is 1000-10000ppm.
7. The fluorosilicone pouring sealant according to claim 1, wherein the fluorosilicone a component has a density of 1.40-2.0g/cm 3 The viscosity is 3000-10000 mPa.s; the density of the fluorosilicone B component is 1.40-2.0g/cm 3 The viscosity is 3000-10000 mPa.s.
8. The fluorosilicone pouring sealant according to any one of claims 1 to 7, wherein the mass ratio of the fluorosilicone a component to the fluorosilicone B component is 1: (0.5-1.5).
9. The method for preparing the heat-conducting oil-resistant fluorosilicone pouring sealant according to claim 1, which is characterized by comprising the following steps:
step 1: uniformly dispersing a certain amount of vinyl fluorosilicone oil and a hydrophobic heat-conducting filler F1, then adding a platinum catalyst, and uniformly mixing to obtain a fluorosilicone A component;
step 2: uniformly dispersing a certain amount of hydrogen-containing fluorosilicone oil and hydrophobic heat-conducting filler F2 to obtain a fluorosilicone B component;
step 3: uniformly mixing the fluorosilicone A component prepared in the step 1 and the fluorosilicone B component prepared in the step 2 according to the mass ratio of 1:0.5-1.5, and curing at room temperature for 2-24 hours to obtain the curing adhesive.
10. The preparation method of claim 9, wherein the thermal conductivity of the cured adhesive prepared in the step 3 is 0.6-1.5W/(m.k), and the volume expansion rate of the cured adhesive in gasoline is not higher than 50%.
CN202310690287.4A 2023-06-12 2023-06-12 Heat-conducting oil-resistant fluorosilicone pouring sealant and preparation method thereof Pending CN116694298A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310690287.4A CN116694298A (en) 2023-06-12 2023-06-12 Heat-conducting oil-resistant fluorosilicone pouring sealant and preparation method thereof

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Application Number Priority Date Filing Date Title
CN202310690287.4A CN116694298A (en) 2023-06-12 2023-06-12 Heat-conducting oil-resistant fluorosilicone pouring sealant and preparation method thereof

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CN116694298A true CN116694298A (en) 2023-09-05

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