CN108410416B - Encapsulating silica gel and preparation method and application thereof - Google Patents
Encapsulating silica gel and preparation method and application thereof Download PDFInfo
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- CN108410416B CN108410416B CN201810295063.2A CN201810295063A CN108410416B CN 108410416 B CN108410416 B CN 108410416B CN 201810295063 A CN201810295063 A CN 201810295063A CN 108410416 B CN108410416 B CN 108410416B
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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
- C09J11/08—Macromolecular additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/296—Organo-silicon compounds
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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
- C08K3/02—Elements
- C08K2003/023—Silicon
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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
- 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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- 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
Abstract
The invention provides encapsulating silica gel and a preparation method and application thereof. The encapsulating silica gel comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 20-45 parts of vinyl silicone oil, 2-7 parts of hydrogen-containing silicone oil, 40-80 parts of surface modified filler and 0.01-0.1 part of inhibitor; the component B comprises the following components in parts by weight: 20-45 parts of vinyl silicone oil, 30-70 parts of surface modified filler and 0.05-0.2 part of catalyst. The encapsulating silica gel prepared by the preparation method has low expansion coefficient, good leveling property during curing, flat and beautiful surface, can keep good encapsulating effect in cold and hot climatic environments, prevents the cracking or damage of components, and can be widely applied to encapsulating electronic components with higher requirements on temperature stability, such as LED power supplies and dry-type transformers.
Description
Technical Field
The invention belongs to the technical field of silicone rubber, relates to encapsulating silica gel and a preparation method thereof, and particularly relates to a preparation method and application of low-expansion high-leveling encapsulating silica gel.
Background
At present, in the fields of electronics, electricity, communication, aerospace and the like, in order to ensure that a product can stably work in an environment with large temperature change or can be reliably used in different areas with large temperature difference, a material with a low expansion coefficient is generally adopted to ensure that the product obtains excellent dimensional stability. The silicon rubber for encapsulating and protecting components also has the same requirement, otherwise, after being heated or cooled, the rubber expands or contracts to cause volume change to cause inconsistent thermal matching performance between the components, so that the invasion of moisture, dust and harmful gas to electronic components cannot be effectively prevented, and internal stress is possibly generated between the components and the rubber to cause the damage or failure of the electronic components. The existing common silicon rubber has a large thermal expansion coefficient, so that how to reduce the expansion coefficient is a key problem in silicon rubber application.
In order to effectively reduce the expansion rate of the silicone rubber, an inorganic filler with a low expansion coefficient can be used as a filler, and the inorganic filler can be graphite, silica powder, calcium carbonate, titanium dioxide, silica powder, alumina powder, magnesium oxide and the like, wherein the graphite and the silica powder have a remarkable reduction effect on the expansion coefficient. Meanwhile, the improvement effect on the expansion rate of the silicone rubber also depends on the using amount of the filler, and the expansion coefficient of the rubber can be reduced by increasing the proportion of the filler. However, when the amount of the filler is large, the viscosity of the gel becomes high, the leveling property becomes poor, the surface is uneven during potting, and the appearance is poor, so that the contradiction between the low expansion rate and the high leveling property is a problem to be solved urgently.
CN103242799A discloses a low-viscosity fast-curing high-flexibility two-component condensation type encapsulating silica gel and a preparation method thereof, the low-viscosity fast-curing high-flexibility two-component condensation type encapsulating silica gel consists of A, B two components, the mass ratio of A, B two components is 8-12: 1; wherein the component A comprises the following raw materials in parts by mass: 100 parts of hydroxyl-terminated polysiloxane, 20-100 parts of filler, 5-50 parts of plasticizer and 0.1-5 parts of pigment; the component B comprises the following raw materials in parts by mass: 1-5 parts of a cross-linking agent, 1-5 parts of a coupling agent, 0.01-0.5 part of a catalyst, 5-10 parts of a plasticizer and 0.5-5 parts of a chain extender. The two-component condensed type encapsulating silica gel prepared by the invention has the performances of low viscosity, fast curing and high flexibility, can meet the requirements of high luminous density and high production efficiency in the LED industry, and has improved leveling property, but the thermal expansion coefficient of the rubber material needs to be further improved.
CN105623593A discloses a two-component potting silica gel, which comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by mass: 100 parts of vinyl silicone oil, 0-100 parts of non-reactive silicone oil, 0.05-10 parts of hollow micro powder, 0.01-1.5 parts of transition metal complex catalyst and 0-3 parts of white slurry; the component B comprises the following raw materials in parts by mass: 100 parts of vinyl silicone oil, 0-100 parts of non-reactive silicone oil, 0.05-10 parts of hollow micro powder, 0.01-1 part of alkynol inhibitor, 10-40 parts of hydrogen-containing silicone oil and 0-3 parts of black paste. The encapsulating silica gel prepared by the invention is a closed-cell foaming material, and has excellent impact resistance, rebound elasticity, flexibility, sound insulation, water resistance and steam resistance, the volume of the encapsulating silica gel is not influenced by the environmental temperature, the thermal expansion coefficient is extremely small, but the rheological property and the aesthetic degree after encapsulation are further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the encapsulating silica gel which has low expansion coefficient, good leveling property during curing, smooth surface during encapsulating of the sizing material, good aesthetic property, more effective protection of components and parts and good service performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a potting silica gel, which is an addition type two-component potting adhesive and consists of a component A and a component B;
the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
20-45 parts of vinyl silicone oil
30-70 parts of surface modified filler
0.05-0.2 part of catalyst.
The component A comprises the following components in parts by weight:
20-45 parts of vinyl silicone oil, for example, the parts by weight of the vinyl silicone oil are 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts and 45 parts.
2-7 parts of hydrogen-containing silicone oil, for example, the weight parts of the hydrogen-containing silicone oil are 2 parts, 3 parts, 4 parts, 5 parts, 6 parts and 7 parts.
40-80 parts of surface modified filler, for example, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts and 80 parts of surface modified filler.
0.01 to 0.1 part of inhibitor, for example, 0.01 part, 0.02 part, 0.03 part, 0.04 part, 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, 0.1 part by weight of inhibitor.
The component B comprises the following components in parts by weight:
20-45 parts of vinyl silicone oil, for example, the parts by weight of the vinyl silicone oil are 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts and 45 parts.
30-70 parts of surface modified filler, for example, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts and 70 parts of surface modified filler.
0.05 to 0.2 part of catalyst, for example, 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, 0.1 part, 0.11 part, 0.12 part, 0.13 part, 0.14 part, 0.15 part, 0.16 part, 0.17 part, 0.18 part, 0.19 part, 0.2 part by weight of catalyst.
Aiming at the defects in the prior art, the low-expansion high-leveling encapsulation silica gel can overcome the defects of easiness in cracking and bulging, poor appearance attractiveness, low reliability and the like in the prior art, has low product viscosity, good leveling property, small thermal expansion, no crack and good appearance attractiveness, and also meets the requirements on processability, mechanical property and the like.
The low expansion rate of the invention means that the colloid has a length change caused by temperature change in one direction, namely the expansion rate is less than 15ppm/K, and the colloid does not expand obviously due to temperature rise in the using process.
The high leveling property means that the rubber material has good fluidity when being poured into the component after being uniformly mixed, and the rubber material is quickly filled in each gap to form a flat plane without obvious concave-convex feeling, and the flat plane is related to factors such as the viscosity of the rubber material, the surface tension and the like.
Preferably, the vinyl silicone oil has a vinyl content of 0.2 to 1.0 wt%, for example, the vinyl silicone oil has a vinyl content of 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, 0.9 wt%, 1 wt%, preferably 0.3 to 0.6 wt%.
Preferably, the vinyl silicone oil is terminal vinyl silicone oil or side chain vinyl silicone oil, preferably terminal vinyl silicone oil; the activity of the terminal vinyl is higher than that of the side chain vinyl, so that the crosslinking speed and the mechanical strength of the rubber material are improved more obviously.
Preferably, the viscosity of the vinyl silicone oil is 100 to 2000cp, for example, the viscosity of the vinyl silicone oil is 100cp, 200cp, 300cp, 400cp, 500cp, 600cp, 700cp, 800cp, 900cp, 1100cp, 1200cp, 1300cp, 1400cp, 1500cp, 1600cp, 1700cp, 1800cp, 1900cp, 2000cp, preferably 300 to 1000 cp. The vinyl content and the hydrogen content in the system must cooperate with each other to ensure proper viscosity and mechanical properties after curing, and further improve the stability of the properties.
The surface modified filler comprises a surface treatment auxiliary agent and powder, wherein the mass ratio of the surface treatment auxiliary agent to the powder is (0.1-1): 100, for example, the mass ratio of the surface treatment auxiliary agent to the powder is 0.1:100, 0.2:100, 0.3:100, 0.4:100, 0.5:100, 0.6:100, 0.7:100, 0.8:100, 0.9:100 and 1: 100. If the mass ratio of the surface treatment auxiliary agent to the powder is lower than 0.1:100, the effect of treating the powder is not obvious, and the effects of low expansion and high leveling property cannot be achieved; if the mass ratio of the surface treatment auxiliary agent to the powder is higher than 1:100, the viscosity of the component is obviously increased, and the leveling property is poor.
The powder is a mixture of at least two of graphite, silicon powder, silica micropowder, titanium dioxide, calcium carbonate, carbon black and alumina powder. For example, the combination of the mixture of powders is: the graphite and silicon micro powder mixture, the graphite and titanium dioxide mixture, the graphite and calcium carbonate mixture, the graphite and carbon black mixture and the graphite and alumina powder mixture; the mixture of silicon powder and silicon micropowder, the mixture of silicon powder and titanium dioxide, the mixture of silicon powder and calcium carbonate, the mixture of silicon powder and carbon black and the mixture of silicon powder and alumina powder; the silica powder and titanium dioxide mixture, the silica powder and calcium carbonate mixture, the silica powder and carbon black mixture, the silica powder and alumina powder mixture, the titanium dioxide and calcium carbonate mixture, the titanium dioxide and titanium dioxide mixture, the titanium dioxide and alumina powder mixture, the calcium carbonate and carbon black mixture, the calcium carbonate and alumina powder mixture, the carbon black and alumina powder mixture, the graphite, silica powder and titanium dioxide mixture, the graphite, silica powder and calcium carbonate mixture, the graphite, silica powder and carbon black mixture, the graphite, silica powder and alumina powder mixture, the graphite, calcium carbonate, carbon black, graphite, carbon black and alumina powder mixture, and similarly, the powder mixture can be four, five, six or seven mixtures, which are not listed herein.
The listed powder has low expansion coefficient performance, wherein the reduction effect of graphite and silicon powder on the expansion coefficient is obvious. Meanwhile, the powder is modified by a surface treatment auxiliary agent, such as silane, silazane and siloxane with low polymerization degree, when the surface treatment auxiliary agent is mixed with the powder at high temperature, the surface treatment auxiliary agent reacts with silicon hydroxyl on the surface of the powder through active groups and polar bonds of the surface treatment auxiliary agent, so that the surface treatment auxiliary agent loses partial activity, the hydrophobicity of the surface of the powder is increased, the polarity is reduced, and the similar intermiscibility and the bonding force of the powder and a silicone oil component are improved. In the process of preparing the A, B component, the dispersion degree of the powder and the silicone oil can be effectively improved, the viscosity is reduced, and the leveling property is improved. Such surface-modified fillers have a positive effect on reducing the expansion coefficient of the rubber compound and at the same time improving its application processability.
Preferably, the mixture of at least two of the powders contains at least one of graphite and silicon powder. For example, the mixture of at least two kinds of powders contains only graphite and only graphite of silicon powders, the mixture of at least two kinds of powders contains only graphite and only silicon powders of silicon powders, and the mixture of at least two kinds of powders contains both graphite and silicon powders.
Preferably, the particle size of the powder is 1-20 μm, preferably 5-15 μm. The particle size of the filler is matched with the proportion of the filler in the system, so that the proper viscosity is ensured and the sedimentation is avoided. The mass fraction of the graphite and the silicon powder in the composite material can be regulated and controlled by adjusting the mass ratio of the graphite and the silicon powder.
The surface treating agent comprises one or a mixture of at least two of methacryloxypropyltrimethoxysilane, dimethyldimethoxysilane, hydroxyl-terminated polydimethylsiloxane and hexamethyldisilazane. For example, the combination of the mixture of surface-treating agents is methacryloxypropyltrimethoxysilane, a mixture of dimethyldimethoxysilane, methacryloxypropyltrimethoxysilane, a mixture of hydroxyl-terminated polydimethylsiloxanes, methacryloxypropyltrimethoxysilane, a mixture of hexamethyldisilazane, dimethyldimethoxysilane, a mixture of hydroxyl-terminated polydimethylsiloxanes, dimethyldimethoxysilane, a mixture of hexamethyldisilazane, a mixture of hydroxyl-terminated polydimethylsiloxanes and hexamethyldisilazane, methacryloxypropyltrimethoxysilane, dimethyldimethoxysilane, a mixture of hydroxyl-terminated polydimethylsiloxanes, methacryloxypropyltrimethoxysilane, dimethyldimethoxysilane, a mixture of hexamethyldisilazane, a mixture of dimethyldimethoxysilane, hydroxy-terminated polydimethylsiloxane and hexamethyldisilazane, a mixture of methacryloxypropyltrimethoxysilane, dimethyldimethoxysilane, hydroxy-terminated polydimethylsiloxane and hexamethyldisilazane.
Preferably, the hydrogen-containing silicone oil has a hydrogen content of 0.3 to 0.6 wt%, for example, the hydrogen-containing silicone oil has a hydrogen content of 0.3 wt%, 0.35 wt%, 0.4 wt%, 0.45 wt%, 0.5 wt%, 0.55 wt%, 0.6 wt%, preferably 0.35 to 0.45 wt%.
Preferably, the inhibitor is any one of ethynylcyclohexanol, methylbutynol and tetramethyltetravinylcyclotetrasiloxane or a combination of at least two thereof. For example, the combination of the mixture of inhibitors is a mixture of ethynylcyclohexanol, methylbutinol, tetramethyltetravinylcyclotetrasiloxane, methylbutinol and tetramethyltetravinylcyclotetrasiloxane, or a mixture of ethynylcyclohexanol, methylbutinol and tetramethyltetravinylcyclotetrasiloxane.
Preferably, the catalyst is a platinum catalyst.
Preferably, the platinum catalyst is a platinum complex and/or a mixture of a platinum chelate and an organosiloxane, such as one or a mixture of at least two of chloroplatinic acid, chloroplatinic acid-isopropanol complex, chloroplatinic acid-divinyltetramethyldisiloxane complex. Preferably chloroplatinic acid-divinyltetramethyldisiloxane complex, the content of the active ingredient thereof being 3000-5000 ppm.
The invention also aims to provide a preparation method of the encapsulating silica gel, which comprises the following steps:
1) uniformly mixing the surface treatment auxiliary agent and the powder according to the mass ratio of (0.1-1) to 100, and heating and stirring to obtain a surface modified filler;
2) adding 20-45 parts by weight of vinyl silicone oil, 40-70 parts by weight of surface modified filler and 2-7 parts by weight of hydrogen-containing silicone oil into a stirrer, heating and stirring, adding 0.05-0.1 part by weight of inhibitor, and continuously stirring to obtain a component A;
adding 20-45 parts by weight of vinyl silicone oil and 30-70 parts by weight of surface modified filler into a stirrer, heating and stirring, adding 0.01-0.2 part by weight of catalyst, and continuously stirring to obtain a component B.
Preferably, the specific process in the step 1) is to dilute the surface treatment auxiliary agent into a 5% solution with methyl silicone oil, then mix the solution with the powder at a high speed in a kneader according to a mass ratio of (0.1-1): 100, the rotation speed of blades of the kneader is 30-60 rpm, heat the mixture to 60-90 ℃, stir the mixture for 20-40 min, stop stirring and heating the mixture, stand the mixture at room temperature for 8-12 h, vacuumize the mixture again, the vacuum degree of the vacuumize is less than or equal to-0.095 MPa, heat the mixture to 60-90 ℃ and dry the mixture for 0.5-2 h to obtain the surface modified filler.
In the invention, the mixing of the raw material components in the step 1) needs larger shearing force, and the ordinary stirring is difficult to realize, so the mixing needs to be carried out in a kneader; and in the vacuum kneading process, the temperature needs to be raised to 60-90 ℃ so that the processing aid reacts with the filler.
Preferably, in the step 1), the rotating speed of the blade of the kneader is 30-60 rpm, for example, the rotating speed of the blade is 30rpm, 35rpm, 40rpm, 45rpm, 50rpm, 55rpm, 60rpm, and the vacuum degree of the vacuum is less than or equal to-0.095 MPa. It should be noted that, in the present invention, the vacuum degree is represented by negative pressure (a value that the system pressure is lower than the atmospheric pressure), and the smaller the value of the negative pressure, the higher the vacuum degree is.
As a preferable scheme, the specific process of the step 2) comprises the steps of heating 20-45 parts by weight of vinyl silicone oil, 40-70 parts by weight of surface modified composite filler and 2-7 parts by weight of hydrogen-containing silicone oil in a planetary stirrer to 60-90 ℃, stirring for 1-2 hours, vacuumizing for 0.5-2 hours, adding 0.05-0.1 part by weight of inhibitor, and stirring for 5-20 min to obtain a component A;
according to the weight portion, 20-45 portions of vinyl silicone oil and 30-70 portions of surface modified filler are heated to 60-90 ℃ in a planetary mixer, stirred for 1-2 hours, vacuumized for 0.5-2 hours, added with 0.01-0.2 portion of catalyst and stirred for 5-20 min, and the component B is obtained.
Preferably, the mixing in step 2) is performed in a planetary mixer, wherein the stirring speed of the planetary mixer is 40-100 rpm, for example, the stirring speed of the planetary mixer is 40rpm, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100 rpm; the vacuum degree of the vacuum is less than or equal to-0.095 MPa.
The invention also aims to provide a using method of the encapsulating silica gel, wherein the component A and the component B are mixed according to the mass ratio of (0.95-1.05): 1, and the encapsulating silica gel is used after being placed and cured at room temperature. For example, the mass ratio of the component A to the component B is 0.95:1, 0.96:1, 0.97:1, 0.98:1, 0.99:1, 1:1, 1.01:1, 1.02:1, 1.03:1, 1.04:1 and 1.05: 1.
The fourth purpose of the invention is to provide application of the potting silica gel, wherein the potting silica gel is used for potting an LED power supply or a dry-type transformer.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the potting silica gel, the surface modified filler is selected as a raw material, the surface modified filler is combined with a silicone oil system and an inhibitor to prepare the component A, the surface modified filler is combined with silicone oil and a catalyst to prepare the component B, and the A, B component is matched for use, so that the balance between the expansion coefficient and the leveling property of a sizing material can be effectively realized, the thermal expansion coefficient of a composite material is reduced, the potting surface is flat and attractive, the thermal expansion coefficient is 6-15 ppm/K, the leveling property is good, components can be more effectively protected, and good use performance is achieved.
(2) The encapsulating silica gel prepared by the preparation method of the encapsulating silica gel has low expansion coefficient, good leveling property during curing, flat and beautiful surface, can keep good encapsulating effect in cold and hot climatic environments, and prevents components from cracking or damaging.
(3) The encapsulating silica gel can be widely applied to encapsulating electronic components with higher requirements on temperature stability, such as LED power supplies and dry-type transformers.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Unless otherwise specified, the viscosity values in the present invention are all measured at 25 ℃.
Example 1
1) Diluting methacryloxypropyl trimethoxysilane into a 5% solution by using methyl silicone oil, then uniformly mixing the solution and the powder in a kneader at a high speed, wherein the temperature is 80 ℃, the stirring speed is 50rpm, the stirring is carried out for 30min, then the stirring and the heating are stopped, the mixture is placed at room temperature for 10 hours, and then the mixture is vacuumized and dried at 80 ℃ for 1 hour to obtain the surface modified composite filler. The mass ratio of the surface treatment auxiliary agent to the powder is 0.3: 100. The powder is a composition of graphite powder, silicon powder and silicon micropowder, the mass ratio of the powder to the silicon micropowder is 1:1:8, and the particle sizes of the powder and the silicon micropowder are all 10 micrometers.
2) Heating 20 parts by weight of vinyl-terminated silicone oil and 75 parts by weight of surface modified composite filler, and 5 parts by weight of hydrogen-containing silicone oil in a planetary mixer to 80 ℃, stirring for 1.5h, vacuumizing for 1h, adding 0.05 part by weight of inhibitor, and stirring for 10min to obtain a component A;
heating 25 parts by weight of vinyl-terminated silicone oil and 75 parts by weight of surface modified filler to 80 ℃ in a planetary stirrer, stirring for 1.5h, vacuumizing for 1h, adding 0.01 part by weight of catalyst, and stirring for 10min to obtain the component B.
Wherein the vinyl-terminated silicone oil has a vinyl content of 1.0 wt% and a viscosity of 100 cp. The hydrogen content of the hydrogen-containing silicone oil is 0.3 wt%, and the viscosity is 100 cp; the inhibitor is ethynyl cyclohexanol; the catalyst was 3000ppm of chloroplatinic acid-divinyltetramethyldisiloxane complex catalyst.
Example 2
1) Diluting methacryloxypropyl trimethoxysilane into a 5% solution by using methyl silicone oil, then uniformly mixing the solution and the powder in a kneader at a high speed, wherein the temperature is 60 ℃, the stirring speed is 60rpm, the stirring is carried out for 25min, then the stirring and the heating are stopped, the mixture is placed at room temperature for 11 hours, and then the mixture is vacuumized and dried at 60 ℃ for 2 hours to obtain the surface modified composite filler. The mass ratio of the surface treatment auxiliary agent to the powder is 0.5: 100. The powder is a composition of graphite powder, silicon powder and silicon micropowder, the mass ratio of the powder to the silicon micropowder is 1:1:8, and the particle sizes of the powder and the silicon micropowder are all 12 micrometers.
2) Heating 30 parts by weight of terminal vinyl silicone oil, 65 parts by weight of surface modified composite filler and 5 parts by weight of hydrogen-containing silicone oil in a planetary mixer to 70 ℃, stirring for 2 hours, vacuumizing for 1.5 hours, adding 0.08 part by weight of inhibitor, and stirring for 10 minutes to obtain a component A;
heating 30 parts by weight of vinyl-terminated silicone oil and 70 parts by weight of surface modified filler to 80 ℃ in a planetary stirrer, stirring for 1.5h, vacuumizing for 1h, adding 0.1 part by weight of catalyst, and stirring for 10min to obtain the component B.
Wherein the vinyl-terminated silicone oil has a vinyl content of 1.0 wt% and a viscosity of 100 cp. The hydrogen content of the hydrogen-containing silicone oil is 0.3 wt%, and the viscosity is 100 cp; the inhibitor is methyl butynol; the catalyst was 3000ppm of chloroplatinic acid-divinyltetramethyldisiloxane complex catalyst.
Example 3
1) Respectively diluting methacryloxypropyltrimethoxysilane and hydroxyl-terminated polydimethylsiloxane into 5% solution by using methyl silicone oil, then uniformly mixing the solution and the powder in a kneader at a high speed at the temperature of 80 ℃, the stirring speed of 50rpm, stirring for 30min, stopping stirring and heating, standing at room temperature for 10 hours, vacuumizing at the temperature of 80 ℃, and drying for 1 hour to obtain the surface-modified composite filler. The mass ratio of the surface treatment auxiliary agent methacryloxypropyltrimethoxysilane to the hydroxyl-terminated polydimethylsiloxane to the powder is 0.2:0.2: 100. The powder is a composition of graphite powder, silicon powder and silicon micropowder, the mass ratio of the powder to the silicon micropowder is 1:1:8, and the particle sizes of the powder and the silicon micropowder are all 10 micrometers. The hydroxyl-terminated polydimethylsiloxane had a viscosity of 100 cp.
2) Heating 30 parts of vinyl-terminated silicone oil, 63 parts of surface modified composite filler and 7 parts of hydrogen-containing silicone oil in a planetary mixer to 80 ℃, stirring for 1.5h, vacuumizing for 1h, adding 0.05 part by weight of inhibitor, and stirring for 10min to obtain a component A;
heating 30 parts of vinyl-terminated silicone oil and 70 parts of surface modified filler to 80 ℃ in a planetary mixer, stirring for 1.5h, vacuumizing for 1h, adding 0.01 part by weight of catalyst, and stirring for 10min to obtain the component B.
Wherein the vinyl-terminated silicone oil has a vinyl content of 1.0 wt% and a viscosity of 100 cp. The hydrogen content of the hydrogen-containing silicone oil is 0.3 wt%, and the viscosity is 100 cp; the inhibitor is a mixture of methyl butynol and tetramethyl tetravinylcyclotetrasiloxane; the catalyst was 3000ppm of chloroplatinic acid-divinyltetramethyldisiloxane complex catalyst.
Example 4
1) Respectively diluting methacryloxypropyltrimethoxysilane and hydroxyl-terminated polydimethylsiloxane into 5% solution by using methyl silicone oil, then uniformly mixing the solution and the powder in a kneader at a high speed at 90 ℃, stirring at a speed of 30rpm for 40min, stopping stirring and heating, standing at room temperature for 8 hours, vacuumizing at 90 ℃, and drying for 0.5 hour to obtain the surface-modified composite filler. The mass ratio of the surface treatment auxiliary agent methacryloxypropyltrimethoxysilane to the hydroxyl-terminated polydimethylsiloxane to the powder is 0.2:0.2: 100. The powder is a composition of graphite powder, silicon micropowder and alumina powder, the mass ratio of the powder is 1:1:4:4, and the particle diameters of the powder are all 10 micrometers. The hydroxyl-terminated polydimethylsiloxane had a viscosity of 100 cp.
2) Heating 30 parts of side chain vinyl silicone oil, 63 parts of surface modified composite filler and 7 parts of hydrogen-containing silicone oil in a planetary mixer to 90 ℃, stirring for 1 hour, vacuumizing for 1 hour, adding 0.05 part by weight of inhibitor, and stirring for 10min to obtain a component A;
heating 30 parts of side chain vinyl silicone oil and 70 parts of surface modified filler to 80 ℃ in a planetary stirrer, stirring for 1.5h, vacuumizing for 1h, adding 0.01 part by weight of catalyst, and stirring for 10min to obtain the component B.
Wherein the vinyl content of the side chain vinyl silicone oil is 0.5 wt%, and the viscosity is 200 cp. The hydrogen content of the hydrogen-containing silicone oil is 0.3 wt%, and the viscosity is 100 cp; the inhibitor is a mixture of methyl butynol and tetramethyl tetravinylcyclotetrasiloxane; the catalyst was 3000ppm of chloroplatinic acid-divinyltetramethyldisiloxane complex catalyst.
Example 5
1) Respectively diluting methacryloxypropyl trimethoxysilane and dimethyl dimethoxysilane into 5% solution by using methyl silicone oil, then uniformly mixing the solution and the powder in a kneader at a high speed, wherein the temperature is 80 ℃, the stirring speed is 50rpm, the stirring is carried out for 30min, then the stirring and the heating are stopped, the mixture is placed at room temperature for 10 hours, and then the mixture is vacuumized and dried at 80 ℃ for 1 hour to obtain the surface modified composite filler. The mass ratio of the surface treatment auxiliary agents of methacryloxypropyltrimethoxysilane and dimethyldimethoxysilane to the powder is 0.2:0.2: 100. The powder is a composition of graphite powder, silicon micropowder and alumina powder, the mass ratio of the powder is 1:1:4:4, and the particle diameters of the powder are all 10 micrometers. The hydroxyl-terminated polydimethylsiloxane had a viscosity of 100 cp.
2) Heating 30 parts of vinyl-terminated silicone oil, 63 parts of surface modified composite filler and 7 parts of hydrogen-containing silicone oil in a planetary mixer to 80 ℃, stirring for 1.5h, vacuumizing for 1h, adding 0.05 part by weight of inhibitor, and stirring for 10min to obtain a component A;
heating 30 parts of vinyl-terminated silicone oil and 70 parts of surface modified filler to 80 ℃ in a planetary mixer, stirring for 1.5h, vacuumizing for 1h, adding 0.01 part by weight of catalyst, and stirring for 10min to obtain the component B.
Wherein the vinyl-terminated silicone oil has a vinyl content of 1.0 wt% and a viscosity of 100 cp. The hydrogen content of the hydrogen-containing silicone oil is 0.3 wt%, and the viscosity is 100 cp; the inhibitor is tetramethyl tetravinylcyclotetrasiloxane; the catalyst was 3000ppm of chloroplatinic acid-divinyltetramethyldisiloxane complex catalyst.
Comparative example 1
The difference from example 5 is that the amount of the treating agent used was 0, i.e., the powder was treated without the surface treating agent.
Comparative example 2
The difference from example 5 is that the graphite amount is 0, i.e. the powder ratio is silicon powder: silicon micropowder: the ratio of alumina to alumina is 1:4: 4.
Comparative example 3
The difference from example 5 is that the amount of silicon powder is 0, i.e. the powder ratio is graphite: silicon micropowder: the ratio of alumina to alumina is 1:4: 4.
Comparative example 4
The difference from example 5 is that the surface-treating assistants were methacryloxypropyltrimethoxysilane and hexamethyldisilazane, i.e.the hydroxy-terminated polydimethylsiloxane was changed to hexamethyldisilazane, the others were unchanged.
Comparative example 5
The difference from example 5 is that the amount of the surface treatment assistant used was increased, that is, the mass ratio of the surface treatment assistants methacryloxypropyltrimethoxysilane and dimethyldimethoxysilane to the powder was 0.6:0.6:100, and the others were unchanged.
Comparative example 6
The difference from example 5 is that the vinyl silicone oil is a side chain vinyl silicone oil having a vinyl group content of 1.0 wt% and a viscosity of 100 cp.
Comparative example 7
The difference from the example 5 is that the surface treatment auxiliary agent is vinyl trimethoxy silane and methyl trimethoxy silane, the ratio of the vinyl trimethoxy silane to the methyl trimethoxy silane to the powder is 0.2:0.2:100, and the rest is unchanged.
Comparative example 8
The difference from the embodiment 5 is that the powder is white carbon black, aluminum hydroxide and quartz powder, and the proportion is 1:1:8, the rest is unchanged.
After the components of the rubber material A, B of the examples 1-5 and the comparative examples 1-8 are respectively finished, the components are mixed according to the mass ratio of 0.95-1.05: 1 and then cured at room temperature for use.
Comparative example 9
The difference from the embodiment 5 is that the A, B components are mixed according to the mass ratio of 2:1 and then are cured at room temperature for use.
In the invention, the test method of the performance of the potting adhesive comprises the following steps:
coefficient of expansion: the compound was cured to a coupon having dimensions Φ 5 × 25mm and then measured using a NETZSCH DIL 402C thermal expansion instrument. The test temperature range is RT-150 ℃, and the heating rate is 5 ℃/min. The expansion coefficient was obtained by analyzing the rate of change of the size of the sample with temperature.
And (3) viscosity testing: testing by using a rotary viscometer at the test temperature of 25 ℃;
and (3) testing mechanical properties: the tensile properties of the samples were tested according to the standard determination of tensile stress strain properties of GBT 528-2009 vulcanisates or thermoplastic rubbers.
The performance data for the potting gels provided in examples 1-5 and comparative examples 1-9 above are shown in table 1 below.
TABLE 1
From the comparison of examples 1 to 5, when the amount of the processing aid used is small or used alone, the compound viscosity is high and the product flowability is poor. The matching use of the powder in example 5 also leads to a more obvious reduction of the viscosity of the rubber compound and a more obvious reduction of the expansion coefficient. Therefore, the processing aid is selected to be matched for use, and the formula matched with the powder has better comprehensive performance.
As can be seen from the performance data provided in example 5 and comparative examples 1-3, the absence of a processing aid in the filler group composition results in a high tack, poor leveling, and a high coefficient of expansion; when the amount of the graphite or the silicon powder is small, the reduction of the expansion coefficient is not obvious. Only with the selection of specific processing aids, the silica gels prepared under specific conditions have the properties of low swelling and high leveling.
From the data of example 5 and comparative example 4, it is clear that the use of hexamethyldisilazane leads to a decrease in strength after curing, an increase in viscosity and poor leveling.
From the data of example 5 and comparative example 5, it is understood that the use of a large amount of the surface treatment assistant increases the colloidal viscosity and deteriorates leveling property. The amount of the filler surface treatment aid is preferably within a suitable range.
From the data of example 5 and comparative example 6, it can be seen that the thermal expansion coefficient of the side-chain vinyl silicone oil is improved relative to that of the terminal vinyl silicone oil, and it can be seen that the balance between the thermal expansion coefficient and the leveling property of the rubber compound is better when the terminal vinyl silicone oil is selected as the vinyl silicone oil.
From the data of example 5 and comparative example 7, it is clear that the use of vinyltrimethoxysilane and methyltrimethoxysilane as treating agents results in a marked increase in the viscosity of the compound and a deterioration in the leveling properties.
From the data of example 5 and comparative example 8, it is clear that the use of white carbon black, aluminum hydroxide, and quartz powder as fillers significantly increases the viscosity of the rubber compound and increases the strength reduction expansion ratio.
As can be seen from the data of example 5 and comparative example 9, when A, B components are used and not mixed according to the corresponding proportion, the curing time of the compound is shortened or prolonged, the strength of the compound is reduced, the hardness deviates from the standard range, and the expansion rate is increased.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (18)
1. The encapsulating silica gel is characterized by consisting of a component A and a component B, wherein the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
20-45 parts of vinyl silicone oil
30-70 parts of surface modified filler
0.05-0.2 part of a catalyst;
the vinyl silicone oil is terminal vinyl silicone oil;
the surface modified filler comprises a surface treatment auxiliary agent and powder, and the mass ratio of the surface treatment auxiliary agent to the powder is (0.1-1): 100;
the powder is a mixture of at least two of graphite, silicon powder, silica micropowder, titanium dioxide, calcium carbonate, carbon black and alumina powder;
the mixture of at least two of the powders at least contains silicon powder;
the surface treatment auxiliary agent is methacryloxypropyltrimethoxysilane and dimethyldimethoxysilane;
the inhibitor is one or a mixture of at least two of ethynyl cyclohexanol, methyl butynol and tetramethyl tetravinylcyclotetrasiloxane;
the mass ratio of the component A to the component B is (0.95-1.05): 1.
2. The potting silica gel of claim 1, wherein the vinyl silicone oil in the component a and the component B has a vinyl content of 0.2 to 1.0 wt%.
3. The potting silica gel of claim 1, wherein the vinyl silicone oil in the component a and the component B has a vinyl content of 0.3 to 0.6 wt%.
4. The silicone potting compound of claim 1, wherein the vinyl silicone oil has a viscosity of 100-2000 cp.
5. The potting silicone rubber of claim 1, wherein the vinyl silicone oil has a viscosity of 300-1000 cp.
6. The potting silica gel of claim 1, wherein the powder has a particle size of 1 to 20 μm.
7. The potting silica gel of claim 1, wherein the powder has a particle size of 5 to 15 μm.
8. The potting silicone rubber according to claim 1, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.3 to 0.6 wt%.
9. The potting silicone rubber according to claim 1, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.35 to 0.45 wt%.
10. The potting silica gel of claim 1, wherein the catalyst is a platinum catalyst.
11. The potting silica gel of claim 10, wherein the platinum catalyst is a mixture of a platinum complex and/or a platinum chelate and an organosiloxane.
12. The potting silica gel of claim 10, wherein the platinum catalyst is one or a mixture of at least two of chloroplatinic acid, chloroplatinic acid-isopropanol complex, chloroplatinic acid-divinyltetramethyldisiloxane complex.
13. A method for preparing the potting silica gel of any of claims 1 to 12, comprising the steps of:
1) uniformly mixing the surface treatment auxiliary agent and the powder according to the mass ratio of (0.1-1) to 100, and heating and stirring to obtain a surface modified filler;
2) adding 20-45 parts by weight of vinyl silicone oil, 40-70 parts by weight of surface modified filler and 2-7 parts by weight of hydrogen-containing silicone oil into a stirrer, heating and stirring, adding 0.05-0.1 part by weight of inhibitor, and continuously stirring to obtain a component A;
adding 20-45 parts by weight of vinyl silicone oil and 30-70 parts by weight of surface modified filler into a stirrer, heating and stirring, adding 0.01-0.2 part by weight of catalyst, and continuously stirring to obtain a component B.
14. The preparation method of claim 13, wherein the specific process of the step 1) is to dilute the surface treatment auxiliary agent with methyl silicone oil into a 5% solution, then mix the solution with the powder at a mass ratio of (0.1-1): 100 in a kneader at a high speed, the rotation speed of a blade of the kneader is 30-60 rpm, heat the mixture to 60-90 ℃, stir the mixture for 20-40 min, then stop stirring and heating, stand the mixture at room temperature for 8-12 h, vacuumize the mixture again, the degree of vacuum of the vacuumization is less than or equal to-0.095 MPa, heat the mixture to 60-90 ℃ and dry the mixture for 0.5-2 h to obtain the surface modified filler.
15. The preparation method of claim 13, wherein the specific process of step 2) comprises heating 20-45 parts by weight of vinyl silicone oil, 40-70 parts by weight of the surface-modified composite filler, and 2-7 parts by weight of hydrogen-containing silicone oil in a planetary mixer to 60-90 ℃, stirring for 1-2 hours, vacuumizing for 0.5-2 hours, adding 0.05-0.1 part by weight of an inhibitor, and stirring for 5-20 min to obtain component A;
according to the weight portion, 20-45 portions of vinyl silicone oil and 30-70 portions of surface modified filler are heated to 60-90 ℃ in a planetary mixer, stirred for 1-2 hours, vacuumized for 0.5-2 hours, added with 0.01-0.2 portion of catalyst and stirred for 5-20 min, and the component B is obtained.
16. The method according to claim 15, wherein in the step 2), the stirring speed of the planetary stirrer is 40 to 100 rpm; the vacuum degree of the vacuumizing is less than or equal to-0.095 MPa.
17. The method for using the potting silica gel according to any one of claims 1 to 12, wherein the component a and the component B are mixed at a mass ratio of (0.95 to 1.05):1 and used after being left to cure at room temperature.
18. Use of the potting silica gel of any of claims 1 to 12 in potting of an LED power supply or a dry transformer.
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| CN109762515A (en) * | 2019-01-28 | 2019-05-17 | 东莞兆舜有机硅科技股份有限公司 | A kind of bonding Embedding Material and preparation method thereof and the application in dry-type transformer |
| CN110964327B (en) * | 2019-12-16 | 2021-09-17 | 杭州之江新材料有限公司 | High-refractive-index transparent silica gel and preparation method and application thereof |
| CN111228897A (en) * | 2020-02-17 | 2020-06-05 | 苏州桐力光电股份有限公司 | Organosilicon porous breathable sterilizing nano filter material for mask and preparation method thereof |
| CN111534276A (en) * | 2020-05-26 | 2020-08-14 | 唐山三友硅业有限责任公司 | Low-density adhesive type flame-retardant silicone rubber and preparation method thereof |
| CN112300754B (en) * | 2020-10-27 | 2021-09-28 | 复旦大学 | Heat-cured enclosure dam organic silicon adhesive and preparation method and application thereof |
| CN115141223A (en) * | 2021-03-31 | 2022-10-04 | 比亚迪股份有限公司 | Surface modifier, modified filler, preparation method of modified filler and pouring sealant |
| CN113563851A (en) * | 2021-07-20 | 2021-10-29 | 深圳先进电子材料国际创新研究院 | In-situ modified low-viscosity high-performance heat-conducting gel and preparation method and application thereof |
| CN115109562B (en) * | 2022-08-09 | 2024-03-12 | 广州白云科技股份有限公司 | Double-component high-heat-dissipation high-conductivity organic silicon pouring sealant and preparation method thereof |
| CN115895277B (en) * | 2022-12-22 | 2023-10-20 | 广州市白云化工实业有限公司 | Pre-cured single-component heat-conducting gel and preparation method thereof |
| CN116063854A (en) * | 2023-03-09 | 2023-05-05 | 深圳天鼎新材料有限公司 | Double-component flame-retardant ceramic silica gel and preparation method and application thereof |
| CN117683511A (en) * | 2023-12-27 | 2024-03-12 | 广东鼎立森新材料有限公司 | Double-component high-heat-conductivity self-leveling pouring sealant and preparation method thereof |
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