CN111925770A - Preparation method of epoxy resin and organic silicon composite pouring sealant - Google Patents
Preparation method of epoxy resin and organic silicon composite pouring sealant Download PDFInfo
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
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- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- 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
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C08L2312/00—Crosslinking
Abstract
The invention discloses a preparation method of an epoxy resin and organic silicon composite pouring sealant, which comprises the following steps: (1) preparation of component A: evacuating and stirring epoxy resin, alumina-coated graphene, epoxy siloxane coupling agent and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 70-90 minutes at the rotation speed of 1000-1200rpm and the vacuum degree of 0.15-0.25MPa to prepare a component A; (2) preparation of the component B: adding amino silicone oil, an aminosilane coupling agent and alumina-coated graphene into a high-speed dispersion machine at room temperature, evacuating, stirring, evacuating and stirring for 30-50 minutes at room temperature; the vacuum degree is 0.1-0.2MPa, and the rotation speed is 800-. The epoxy resin organic silicon composite pouring sealant prepared by the invention overcomes the defects of the traditional pouring sealant, has excellent mechanical property, insulation, sealing, water resistance, heat conductivity, flame retardance, chemical stability and bonding property, and is simple and easy to encapsulate.
Description
The invention relates to a divisional application of Chinese patent 'an epoxy resin and organic silicon composite pouring sealant and a preparation method thereof', wherein the application date is 11, 12 and 2017, and the application number is 201711110510.4.
Technical Field
The invention relates to the technical field of pouring sealant, in particular to an epoxy resin and organic silicon composite pouring sealant and a preparation method thereof.
Background
With the development of economic society, electronic materials and electronic products emerge like bamboo shoots in the spring after rain, and in order to match the development of electronic materials and electronic products, people put forward new requirements on potting adhesives for bonding, potting and packaging of electronic components, and the potting adhesives are required to have excellent mechanical properties, perfect appearance, insulation, sealing and water resistance, good thermal conductivity, flame retardancy and chemical stability, and convenient filling operation.
At present, the most used encapsulating materials mainly comprise three types, namely epoxy resin, polyurethane and organosilicon materials, and the room-temperature curing epoxy resin encapsulating adhesive is widely applied to bonding, encapsulating and packaging of electronic elements due to good mechanical property and cohesiveness, but the unmodified epoxy resin has high rigidity, poor toughness under high and low temperature impact, easy cracking of an adhesive layer and poor dimensional stability caused by thermal expansion and cold contraction under high and low temperatures; the organosilicon material has excellent high and low temperature resistance, weather resistance and electric insulation, but has the defects of low thermal conductivity, poor flame retardance and poor adhesive property; the polyurethane material has the best waterproof performance, acid resistance, flexibility and impact resistance, but when the polyurethane material is used as electronic packaging adhesive, more bubbles exist, the vacuum pumping and the adhesive filling are needed, and the operation is complex.
Therefore, there is a need for a more efficient method for synthesizing a potting adhesive which is excellent in mechanical properties, insulation, sealing, water resistance, thermal conductivity, flame retardancy, and chemical stability, and which is easy and simple to perform in potting operation.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the epoxy resin organosilicon composite pouring sealant and the preparation method thereof, the preparation method is simple and easy to implement, the requirement on equipment is not high, the cost is low, the epoxy resin organosilicon composite pouring sealant prepared by the preparation method has excellent mechanical property, insulation, sealing, water resistance, thermal conductivity, flame retardance, chemical stability and bonding property, and the pouring operation is simple and easy to implement.
In order to achieve the purpose, the invention adopts the technical scheme that the epoxy resin organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 1-2 of a component A and a component B;
the component A comprises the following raw materials in parts by weight: 45-65 parts of epoxy resin, 10-20 parts of alumina-coated graphene, 5-8 parts of epoxy siloxane coupling agent and 5-10 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 45-65 parts of amino silicone oil, 5-8 parts of amino silane coupling agent and 10-20 parts of aluminum oxide coated graphene;
the preparation method of the alumina-coated graphene comprises the following steps: adding distilled water and an emulsifier into the graphene treated at the temperature of 280-300 ℃, adding diluted hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion. After heating to the temperature of 200 ℃ and 250 ℃, slowly adding 10-20% of aluminum chloride solution in mass fraction into the suspension within 1-2 hours, and simultaneously dropwise adding ammonia water to keep the pH value of the suspension stable. And after the aluminum chloride solution is added, keeping the temperature for 4-5 hours. And then filtering the suspension, repeatedly washing with distilled water until no chloride ion is detected in the filtrate, finally washing with absolute ethyl alcohol, drying the washed graphene at 120 ℃ for 14h, and performing heat treatment at 500 ℃ for 6 h.
The preparation method of the amino silicone oil comprises the following steps: adding octamethylcyclotetrasiloxane (D4) into a four-neck flask, stirring by a magnetic stirrer, heating by a methyl silicone oil bath, heating to 80-100 ℃ under the protection of nitrogen, adding N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane into the four-neck flask through a dropping funnel, stirring for 20-40 minutes, and then dropwise adding 1-3% by mass of tetramethylammonium hydroxide solution. Heating to 100 ℃ and 110 ℃, reacting for 6-8 hours, then dropwise adding hexamethyldisiloxane, cooling to 60 ℃, and reacting for l-2 hours. And carrying out reduced pressure distillation on the obtained crude product for 1-2 hours at the temperature of 60-70 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities, thus obtaining colorless and transparent viscous amino silicone oil.
The mass ratio of the graphene to the distilled water to the emulsifier to the aluminum chloride solution is 1: 10: 0.1-0.3: 5-10;
the emulsifier is one or more selected from sodium dodecyl benzene sulfonate, polyoxypropylene polyethylene glycerol ether and nonylphenol polyoxyethylene ether;
the mass ratio of the octamethylcyclotetrasiloxane (D4), the N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, the tetramethylammonium hydroxide solution and the hexamethyldisiloxane is 200: 4-1015-20: 2-3;
preferably, the epoxy resin is selected from any one or more of bisphenol A type epoxy resin and o-cresol formaldehyde epoxy resin;
preferably, the epoxy resin is sieved by a 200-mesh sieve before use;
preferably, the epoxysiloxane coupling agent is 3- (2, 3-glycidoxy) propyltrimethoxysilane; the amino silane coupling agent is selected from one or more of gamma-aminopropyl triethoxysilane, gamma-aminopropyl trimethoxysilane, N-beta (aminoethyl) -gamma-aminopropyl triethoxysilane, phenylaminomethyl trimethoxysilane and polyaminoalkyl trialkoxy silane;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring epoxy resin, alumina-coated graphene, epoxy siloxane coupling agent and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 70-90 minutes at the rotation speed of 1000-1200rpm and the vacuum degree of 0.15-0.25MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, an aminosilane coupling agent and alumina-coated graphene into a high-speed dispersion machine at room temperature, evacuating, stirring, evacuating and stirring for 30-50 minutes at room temperature; the vacuum degree is 0.1-0.2MPa, and the rotation speed is 800-.
A use method of an epoxy resin and organic silicon composite pouring sealant comprises the following steps: taking the component A and the component B according to the weight part of the designed epoxy resin organic silicon composite pouring sealant component, mixing and stirring the components uniformly, then stirring at 70-80 ℃, continuously stirring for 60-80 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an object to be poured, standing at room temperature for 3-5 hours for pre-curing, then placing in a vacuum drying oven, keeping the temperature at 120-150 ℃, and fully curing at constant temperature for 4-6 hours.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) compared with the pouring sealant in the prior art, the epoxy resin organic silicon composite pouring sealant has the advantages of simple and easy preparation method, low requirement on equipment, easily obtained raw materials and low cost.
(2) Compared with the pouring sealant in the prior art, the epoxy resin and organic silicon composite pouring sealant overcomes the defects of high rigidity, poor toughness at high and low temperature impact, easy cracking of a glue layer, poor dimensional stability caused by expansion with heat and contraction with cold at high and low temperatures, low heat conductivity of an organic silicon material, poor flame retardance and poor bonding performance of the epoxy resin, combines the excellent performance of the material, and has excellent mechanical property, insulation, sealing, water resistance, heat conductivity, flame retardance, chemical stability and bonding performance, and the pouring sealant is simple and easy to operate.
(3) The structure of the epoxy resin organic silicon composite potting adhesive contains the graphene filler wrapped by the alumina, so that the oxidation resistance, the heat conductivity and the mechanical property of the material are improved.
(4) According to the epoxy resin organic silicon composite pouring sealant, a chemical crosslinking reaction is generated between epoxy groups in the component A and amino groups in the component B to form a three-dimensional network structure through curing, so that the mechanical property and the chemical stability of the material can be improved while the processing fluidity is ensured.
(5) The epoxy resin organic silicon composite pouring sealant has moderate curing conditions, does not need overhigh temperature, does not need to add a catalyst into a rubber material, and is convenient and easy to operate.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
The raw material used in the following examples of the present invention was obtained from Shanghai spring Xin import & export trade company, Inc.
Example 1
An epoxy resin and organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 1, component A and component B;
the component A comprises the following raw materials in parts by weight: 45 parts of bisphenol A epoxy resin, 10 parts of alumina-coated graphene, 5 parts of epoxy siloxane coupling agent and 5 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 45 parts of amino silicone oil, 5 parts of amino silane coupling agent and 10 parts of alumina-coated graphene;
the preparation method of the alumina-coated graphene comprises the following steps: adding 1000g of distilled water and 10g of sodium dodecyl benzene sulfonate serving as an emulsifier into 100g of graphene treated at 280 ℃, adding dilute hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion. After heating to 200 ℃, 500g of a 10% aluminum chloride solution was slowly added to the suspension over 1 hour while ammonia was added dropwise to keep the pH of the suspension stable. After the addition of the aluminum chloride solution, the temperature is maintained for 4 hours. And then filtering the suspension, repeatedly washing with distilled water until no chloride ion is detected in the filtrate, finally washing with absolute ethyl alcohol, drying the washed graphene at 120 ℃ for 14h, and performing heat treatment at 500 ℃ for 6 h.
The preparation method of the amino silicone oil comprises the following steps: 200g of octamethylcyclotetrasiloxane (D4) is added into a four-neck flask, stirred by a magnetic stirrer, heated by methyl silicone oil bath, heated to 80 ℃ under the protection of nitrogen, 4g of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane is added into the four-neck flask through a dropping funnel, stirred for 20 minutes and then 20g of tetramethylammonium hydroxide solution with the mass fraction of 1% is added dropwise. Heating to 100 ℃, reacting for 6 hours, dropwise adding 2g of hexamethyldisiloxane, cooling to 60 ℃, and reacting for l hours. And carrying out reduced pressure distillation on the obtained crude product for 1 hour at the temperature of 60 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities so as to obtain colorless and transparent viscous amino silicone oil.
Preferably, the epoxy resin is sieved by a 200-mesh sieve before use;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring bisphenol A type epoxy resin, alumina-coated graphene, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 70 minutes at the rotating speed of 1000rpm and the vacuum degree of 0.15MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, gamma-aminopropyl triethoxysilane and alumina coated graphene into a high-speed dispersion machine at room temperature, and vacuumizing and stirring for 30 minutes at room temperature; the vacuum degree is 0.1MPa, the rotating speed is 800rpm, and the component B is prepared.
A use method of an epoxy resin and organic silicon composite pouring sealant comprises the following steps: taking the component A and the component B according to the designed weight parts of the components of the epoxy resin organic silicon composite pouring sealant, mixing and stirring the components uniformly, then stirring at 70 ℃, continuously stirring for 60 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an encapsulated object, standing for 3 hours at room temperature for precuring, placing the object in a vacuum drying oven, keeping the temperature at 120 ℃ for 4 hours, and fully curing.
Example 2
An epoxy resin and organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 1.2 of component A and component B;
the component A comprises the following raw materials in parts by weight: 48 parts of o-cresol formaldehyde epoxy resin, 13 parts of alumina-coated graphene, 7 parts of epoxy siloxane coupling agent and 7 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 48 parts of amino silicone oil, 7 parts of amino silane coupling agent and 13 parts of alumina-coated graphene;
the preparation method of the alumina-coated graphene comprises the following steps: adding 1000g of distilled water and 20g of emulsifier polyoxypropylene polyethylene glycerol ether into 100g of graphene treated at 290 ℃, adding dilute hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion. After heating to 220 ℃, 600g of aluminum chloride solution with the mass fraction of 13% is slowly added into the suspension within 1.5 hours, and ammonia water is dropwise added to keep the pH value of the suspension stable; after the addition of the aluminum chloride solution, the temperature was maintained for 4.3 hours. And then filtering the suspension, repeatedly washing with distilled water until no chloride ion is detected in the filtrate, finally washing with absolute ethyl alcohol, drying the washed graphene at 120 ℃ for 14h, and performing heat treatment at 500 ℃ for 6 h.
The preparation method of the amino silicone oil comprises the following steps: 200g of octamethylcyclotetrasiloxane (D4) is added into a four-neck flask, stirred by a magnetic stirrer, heated by methyl silicone oil bath, heated to 90 ℃ under the protection of nitrogen, 6g of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane is added into the four-neck flask through a dropping funnel, stirred for 30 minutes and then 18g of tetramethylammonium hydroxide solution with the mass fraction of 2% is added dropwise. The temperature is increased to 105 ℃, 2.5g of hexamethyldisiloxane is added dropwise after the reaction is carried out for 7 hours, the temperature is reduced to 60 ℃, and then the reaction is carried out for l.5 hours. And carrying out reduced pressure distillation on the obtained crude product for 1.5 hours at 65 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities so as to obtain colorless and transparent viscous amino silicone oil.
Preferably, the epoxy resin is sieved by a 200-mesh sieve before use;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring o-cresol formaldehyde epoxy resin, alumina-coated graphene, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 80 minutes, wherein the rotating speed is 1050rpm, and the vacuum degree is 0.2MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and alumina coated graphene into a high-speed dispersion machine at room temperature, and vacuumizing and stirring for 40 minutes at room temperature; the vacuum degree is 0.15MPa, the rotating speed is 900rpm, and the component B is prepared.
A use method of an epoxy resin and organic silicon composite pouring sealant comprises the following steps: taking the component A and the component B according to the designed weight parts of the components of the epoxy resin organic silicon composite pouring sealant, mixing and stirring the components uniformly, then stirring at 75 ℃, continuously stirring for 70 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an encapsulated object, standing at room temperature for 4 hours for precuring, placing in a vacuum drying oven, keeping the temperature for 5 hours at 130 ℃, and fully curing.
Example 3
An epoxy resin and organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 1.7 of component A and component B;
the component A comprises the following raw materials in parts by weight: 55 parts of epoxy resin, 17 parts of alumina-coated graphene, 7 parts of epoxy siloxane coupling agent and 8 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 55 parts of amino silicone oil, 7 parts of amino silane coupling agent and 16 parts of alumina-coated graphene;
the preparation method of the alumina-coated graphene comprises the following steps: adding 1000g of distilled water and 22g of nonylphenol polyoxyethylene ether serving as an emulsifier into 100g of graphene treated at 285 ℃, adding dilute hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion. After heating to 240 ℃, 700g of an aluminum chloride solution with a mass fraction of 16% was slowly added to the suspension over 1.8 hours, while ammonia was added dropwise to keep the pH of the suspension stable. After the addition of the aluminum chloride solution, the temperature is maintained for 4.8 hours. And then filtering the suspension, repeatedly washing with distilled water until no chloride ion is detected in the filtrate, finally washing with absolute ethyl alcohol, drying the washed graphene at 120 ℃ for 14h, and performing heat treatment at 500 ℃ for 6 h.
The preparation method of the amino silicone oil comprises the following steps: 200g of octamethylcyclotetrasiloxane (D4) is added into a four-neck flask, stirred by a magnetic stirrer, heated by methyl silicone oil bath, heated to 95 ℃ under the protection of nitrogen, 8g of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane is added into the four-neck flask through a dropping funnel, stirred for 35 minutes and then 17g of tetramethylammonium hydroxide solution with the mass fraction of 3% is added dropwise. Raising the temperature to 108 ℃, reacting for 7.8 hours, then dropwise adding hexamethyldisiloxane, reducing the temperature to 60 ℃, and reacting for l.9 hours. And carrying out reduced pressure distillation on the obtained crude product for 1.8 hours at 68 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities, thus obtaining colorless and transparent viscous amino silicone oil.
The epoxy resin is a mixture formed by mixing bisphenol A epoxy resin and o-cresol formaldehyde epoxy resin according to the mass ratio of 2: 5;
preferably, the epoxy resin is sieved by a 200-mesh sieve before use;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring epoxy resin, alumina-coated graphene, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 83 minutes at the rotating speed of 1100rpm and the vacuum degree of 0.22MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, phenylaminomethyl triethoxysilane and alumina-coated graphene into a high-speed dispersion machine at room temperature, and vacuumizing and stirring for 42 minutes at room temperature; the vacuum degree is 0.16MPa, the rotating speed is 920rpm, and the component B is prepared.
A use method of an epoxy resin and organic silicon composite pouring sealant comprises the following steps: taking the component A and the component B according to the designed weight parts of the epoxy resin organic silicon composite pouring sealant component, mixing and stirring the components uniformly, then stirring at 77 ℃, continuously stirring for 73 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an encapsulated object, standing at room temperature for 4 hours for precuring, placing in a vacuum drying oven, keeping the temperature at 135 ℃ for 6 hours, and fully curing.
Example 4
An epoxy resin and organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 1.9 of a component A and a component B;
the component A comprises the following raw materials in parts by weight: 62 parts of epoxy resin, 19 parts of alumina-coated graphene, 8 parts of epoxy siloxane coupling agent and 6 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 60 parts of amino silicone oil, 8 parts of amino silane coupling agent and 19 parts of alumina-coated graphene;
the preparation method of the alumina-coated graphene comprises the following steps: adding 1000g of distilled water and 23g of sodium dodecyl benzene sulfonate serving as an emulsifier into 100g of graphene treated at 290 ℃, adding dilute hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion. After heating to 240 ℃, 850g of a 20% aluminum chloride solution was slowly added to the suspension over 2 hours while ammonia was added dropwise to keep the pH of the suspension stable. After the addition of the aluminum chloride solution, the temperature is maintained for 5 hours. And then filtering the suspension, repeatedly washing with distilled water until no chloride ion is detected in the filtrate, finally washing with absolute ethyl alcohol, drying the washed graphene at 120 ℃ for 14h, and performing heat treatment at 500 ℃ for 6 h.
The preparation method of the amino silicone oil comprises the following steps: 200g of octamethylcyclotetrasiloxane (D4) is added into a four-neck flask, stirred by a magnetic stirrer, heated by methyl silicone oil bath, heated to 97 ℃ under the protection of nitrogen, 8g of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane is added into the four-neck flask through a dropping funnel, stirred for 37 minutes, and then 18g of tetramethylammonium hydroxide solution with the mass fraction of 2.5% is added dropwise. The temperature is increased to 106 ℃, 2.5g of hexamethyldisiloxane is dripped after 8 hours of reaction, and the reaction is carried out for l hours after the temperature is reduced to 60 ℃. And carrying out reduced pressure distillation on the obtained crude product for 1 hour at 66 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities so as to obtain colorless and transparent viscous amino silicone oil.
The epoxy resin is a mixture formed by mixing bisphenol A epoxy resin and o-cresol formaldehyde epoxy resin according to the mass ratio of 3: 8;
preferably, the epoxy resin is sieved by a 200-mesh sieve before use;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring epoxy resin, alumina-coated graphene, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 90 minutes at the rotating speed of 1200rpm and the vacuum degree of 0.24MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, polyamino alkyl trialkoxysilane and alumina coated graphene into a high-speed dispersion machine at room temperature, evacuating, stirring, evacuating and stirring for 47 minutes at room temperature; the vacuum degree is 0.2MPa, the rotating speed is 1000rpm, and the component B is prepared.
A use method of an epoxy resin and organic silicon composite pouring sealant comprises the following steps: taking the component A and the component B according to the designed weight parts of the components of the epoxy resin organic silicon composite pouring sealant, mixing and stirring the components uniformly, then stirring the components at 80 ℃, continuously stirring the mixture for 77 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an encapsulated object, standing the mixture at room temperature for 5 hours for precuring, placing the mixture in a vacuum drying oven, keeping the temperature constant for 6 hours, and fully curing the mixture.
Example 5
An epoxy resin and organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 2, component A and component B;
the component A comprises the following raw materials in parts by weight: 65 parts of epoxy resin, 20 parts of alumina-coated graphene, 8 parts of epoxy siloxane coupling agent and 10 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 65 parts of amino silicone oil, 8 parts of amino silane coupling agent and 20 parts of alumina-coated graphene;
the preparation method of the alumina-coated graphene comprises the following steps: adding 1000g of distilled water and 30g of emulsifier polyoxypropylene polyethylene glycerol ether into 100g of graphene treated at 300 ℃, adding diluted hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion. After heating to 250 ℃, 1000g of a 20% aluminum chloride solution was slowly added to the suspension over 2 hours while ammonia was added dropwise to keep the pH of the suspension stable. After the addition of the aluminum chloride solution, the temperature is maintained for 5 hours. And then filtering the suspension, repeatedly washing with distilled water until no chloride ion is detected in the filtrate, finally washing with absolute ethyl alcohol, drying the washed graphene at 120 ℃ for 14h, and performing heat treatment at 500 ℃ for 6 h.
The preparation method of the amino silicone oil comprises the following steps: 200g of octamethylcyclotetrasiloxane (D4) is added into a four-neck flask, stirred by a magnetic stirrer, heated by methyl silicone oil bath, heated to 100 ℃ under the protection of nitrogen, 10g of N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane is added into the four-neck flask through a dropping funnel, stirred for 40 minutes and then 20g of tetramethylammonium hydroxide solution with the mass fraction of 3% is added dropwise. The temperature is increased to 110 ℃, 3g of hexamethyldisiloxane is dripped after the reaction is carried out for 8 hours, and the reaction is carried out for 2 hours after the temperature is reduced to 60 ℃. And carrying out reduced pressure distillation on the obtained crude product for 2 hours at 70 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities so as to obtain colorless and transparent viscous amino silicone oil.
Preferably, the epoxy resin is selected from bisphenol A type epoxy resin and o-cresol formaldehyde epoxy resin which are mixed according to the mass ratio of 3: 7;
preferably, the epoxy resin is sieved by a 200-mesh sieve before use;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring epoxy resin, alumina-coated graphene, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 90 minutes at the rotating speed of 1200rpm and the vacuum degree of 0.25MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, gamma-aminopropyltrimethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane and alumina coated graphene into a high-speed dispersion machine at room temperature, evacuating, stirring, evacuating and stirring for 50 minutes at room temperature; the vacuum degree is 0.2MPa, the rotating speed is 1000rpm, and the component B is prepared.
A use method of an epoxy resin and organic silicon composite pouring sealant comprises the following steps: taking the component A and the component B according to the designed weight parts of the components of the epoxy resin organic silicon composite pouring sealant, mixing and stirring the components uniformly, then stirring the components at 80 ℃, continuously stirring the components for 80 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an encapsulated object, standing the mixture at room temperature for 5 hours for precuring, placing the mixture in a vacuum drying oven, keeping the temperature at 150 ℃ for 6 hours, and fully curing the mixture.
Comparative example
The epoxy resin pouring sealant is traditionally sold in the market.
Product performance testing of the above examples and comparative examples:
(1) viscosity: according to the standard GB/T10247-2008;
(2) tensile strength, elongation at break: (ii) a A. Uniformly mixing the component B, performing vacuum defoaming, uniformly coating on a mold with the thickness of 2mm, and performing ultraviolet curing for 40 minutes, and then testing according to GB/T528-2009;
(3) hardness: testing the Shore A hardness according to GB/T531-2008;
(4) dielectric strength: testing the dielectric strength according to GB/T1695-2005;
(5) volume resistivity: testing the volume resistivity according to GB/T1692-2008;
(6) thermal conductivity: testing the thermal conductivity according to GB/T11205-2009;
(7) flame retardancy: testing the flame retardant rating according to UL 94;
(8) heat resistance: testing the heat distortion temperature according to GB/T1634-79; the test results are shown in table 1:
TABLE 1 results of Performance test of examples and comparative examples
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Viscosity (mPa.s) | 2550 | 2600 | 2500 | 2340 | 2220 | 5000 |
| Hardness (ShoreA) | 83 | 81 | 83 | 83 | 84 | 80 |
| Tensile Strength (MPa) | 4.6 | 4.6 | 4.5 | 4.7 | 4.6 | 2.2 |
| Elongation at Break (%) | 344 | 350 | 346 | 356 | 360 | 182 |
| Dielectric strength (KV/mm) | 36 | 35 | 36 | 38 | 40 | 25 |
| Volume resistivity (. times.10)15Q.cm) | 5.3 | 5.2 | 5.4 | 5.6 | 5.4 | 2.3 |
| Coefficient of thermal conductivity (W/m.K) | 2.3 | 2.4 | 2.6 | 2.8 | 2.6 | 1.5 |
| Flame retardant rating (UL94) | V-0 | V-0 | V-0 | V-0 | V-0 | V-1 |
| Heat resistance (0.45 MPa/. degree.C.) | 105 | 110 | 104 | 115 | 110 | 87 |
From the above table, it can be seen that, compared with the conventional epoxy resin pouring sealant sold in the market, the electronic pouring sealant disclosed in the embodiment of the invention has better flame retardancy, thermal conductivity, electrical insulation property, mechanical property, fluidity and heat resistance, and meets the use requirements of the electronic pouring sealant.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those of ordinary skill in the art can readily practice the present invention as described herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (9)
1. The preparation method of the epoxy resin and organic silicon composite pouring sealant is characterized in that the epoxy resin and organic silicon composite pouring sealant is prepared from the following components in parts by weight of 1: 1-2 of a component A and a component B:
the component A comprises the following raw materials in parts by weight: 45-65 parts of epoxy resin, 10-20 parts of alumina-coated graphene, 5-8 parts of epoxy siloxane coupling agent and 5-10 parts of dibenzyl phosphate;
the component B comprises the following raw materials in parts by weight: 45-65 parts of amino silicone oil, 5-8 parts of amino silane coupling agent and 10-20 parts of aluminum oxide coated graphene;
the preparation method of the epoxy resin organic silicon composite pouring sealant comprises the following steps:
(1) preparation of component A: evacuating and stirring epoxy resin, alumina-coated graphene, epoxy siloxane coupling agent and dibenzyl phosphate in a high-speed dispersion machine at normal temperature for 70-90 minutes at the rotation speed of 1000-1200rpm and the vacuum degree of 0.15-0.25MPa to prepare a component A;
(2) preparation of the component B: adding amino silicone oil, an aminosilane coupling agent and alumina-coated graphene into a high-speed dispersion machine at room temperature, evacuating, stirring, evacuating and stirring for 30-50 minutes at room temperature; the vacuum degree is 0.1-0.2MPa, and the rotation speed is 800-.
2. The preparation method of the epoxy resin organosilicon composite pouring sealant according to claim 1, wherein the preparation method of the alumina-coated graphene comprises the following steps:
(1) adding distilled water and an emulsifier into the graphene treated at the temperature of 280 plus 300 ℃, adding dilute hydrochloric acid to adjust the pH value of the suspension to be neutral, and performing ultrasonic dispersion;
(2) after heating to the temperature of 200 ℃ and 250 ℃, slowly adding 10-20% of aluminum chloride solution in mass fraction into the suspension within 1-2 hours, and simultaneously dropwise adding ammonia water to keep the pH value of the suspension stable;
(3) and after the aluminum chloride solution is added, preserving heat for 4-5 hours, filtering the suspension, repeatedly cleaning the suspension with distilled water until no chloride ion is detected in the filtrate, finally cleaning the suspension with absolute alcohol, drying the cleaned graphene at 120 ℃ for 14 hours, and performing heat treatment at 500 ℃ for 6 hours.
3. The preparation method of the epoxy resin organosilicon composite pouring sealant according to claim 2, wherein the mass ratio of the graphene, the distilled water, the emulsifier and the aluminum chloride solution is 1: 10: 0.1-0.3: 5 to 10.
4. The preparation method of the epoxy resin organosilicon composite pouring sealant as claimed in claim 2, wherein the emulsifier is selected from one or more of sodium dodecyl benzene sulfonate, polyoxypropylene polyethylene glycerol ether and nonylphenol polyoxyethylene ether.
5. The preparation method of the epoxy resin organosilicon composite pouring sealant according to claim 1, wherein the preparation method of the amino silicone oil comprises the following steps:
(1) adding octamethylcyclotetrasiloxane (D4) into a four-neck flask, stirring by a magnetic stirrer, heating by a methyl silicone oil bath, heating to 80-100 ℃ under the protection of nitrogen, adding N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane into the four-neck flask through a dropping funnel, stirring for 20-40 minutes, and then dropwise adding 1-3% by mass of tetramethylammonium hydroxide solution;
(2) heating to 100 ℃ and 110 ℃, reacting for 6-8 hours, dropwise adding hexamethyldisiloxane, cooling to 60 ℃, and reacting for l-2 hours;
(3) and carrying out reduced pressure distillation on the obtained crude product for 1-2 hours at the temperature of 60-70 ℃ by using a rotary evaporator to remove low-boiling-point micromolecule impurities, thus obtaining colorless and transparent viscous amino silicone oil.
6. The preparation method of the epoxy resin organosilicon composite pouring sealant as claimed in claim 5, wherein the mass ratio of the octamethylcyclotetrasiloxane (D4), the N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, the tetramethylammonium hydroxide solution and the hexamethyldisiloxane is 200: 4-10: 15-20: 2 to 3.
7. The preparation method of the epoxy resin organosilicon composite pouring sealant according to claim 1, wherein the epoxy resin is selected from any one or more of bisphenol A type epoxy resin and o-cresol formaldehyde epoxy resin.
8. The preparation method of the epoxy resin organosilicon composite pouring sealant according to claim 1, wherein the epoxy siloxane coupling agent is 3- (2, 3-epoxypropoxy) propyltrimethoxysilane; the amino silane coupling agent is selected from one or more of gamma-aminopropyl triethoxysilane, gamma-aminopropyl trimethoxysilane, N-beta (aminoethyl) -gamma-aminopropyl triethoxysilane, phenylaminomethyl trimethoxysilane and polyaminoalkyl trialkoxy silane.
9. The use method of the epoxy resin organic silicon composite pouring sealant prepared by the preparation method of any one of claims 1 to 8 is characterized by comprising the following steps: taking the component A and the component B according to the weight part of the designed epoxy resin organic silicon composite pouring sealant component, mixing and stirring the components uniformly, then stirring at 70-80 ℃, continuously stirring for 60-80 minutes after the mixture is dissolved into a liquid state, then coating the mixture on the surface of an object to be poured, standing at room temperature for 3-5 hours for pre-curing, then placing in a vacuum drying oven, keeping the temperature at 120-150 ℃, and fully curing at constant temperature for 4-6 hours.
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| CN116903861A (en) * | 2023-09-12 | 2023-10-20 | 哈尔滨工业大学 | Synthesis method of high ammonia value silicone oil, organic silicon/epoxy adhesive film, preparation method of organic silicon/epoxy adhesive film and bendable laminated board |
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| CN108441153A (en) * | 2018-04-08 | 2018-08-24 | 湖州丘天电子科技有限公司 | A kind of high-performance epoxy resin base electron pouring sealant and its preparation process |
| CN111690345B (en) * | 2020-06-22 | 2021-12-07 | 江西优宝新材料科技有限公司 | Modified graphene oxide, modified graphene oxide composite epoxy binder and preparation method |
| CN112358846A (en) * | 2020-11-04 | 2021-02-12 | 碳元科技股份有限公司 | Two-component pouring sealant with low thermal expansion coefficient and preparation method thereof |
| CN114196211A (en) * | 2021-12-28 | 2022-03-18 | 佛山金戈新材料股份有限公司 | Preparation method of low-specific-gravity high-heat-conductivity gasket |
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| CN101805996B (en) * | 2010-03-18 | 2012-09-05 | 佛山市顺德区德美瓦克有机硅有限公司 | Hydrophilic amino-polysiloxane softener and preparation method thereof |
| CN105623592A (en) * | 2014-11-05 | 2016-06-01 | 南京艾鲁新能源科技有限公司 | Flexible insulation pouring sealant based on modified epoxy resin |
| CN105524469B (en) * | 2014-11-27 | 2017-02-22 | 比亚迪股份有限公司 | Heat-conducting glue and its preparation method and use |
| CN104877612A (en) * | 2015-06-15 | 2015-09-02 | 南京工业大学 | Heat-conducting insulating adhesive and preparation method thereof |
| CN105524225B (en) * | 2016-01-06 | 2018-06-15 | 上海保立佳新材料有限公司 | A kind of hud typed polyacrylate dispersion printing adhesive |
| CN107057322B (en) * | 2017-05-09 | 2019-06-18 | 东莞市亚仑塑料原料有限公司 | A kind of PC alloy material and preparation method thereof |
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| CN116903861A (en) * | 2023-09-12 | 2023-10-20 | 哈尔滨工业大学 | Synthesis method of high ammonia value silicone oil, organic silicon/epoxy adhesive film, preparation method of organic silicon/epoxy adhesive film and bendable laminated board |
| CN116903861B (en) * | 2023-09-12 | 2023-12-12 | 哈尔滨工业大学 | Synthesis method of high ammonia value silicone oil, organic silicon/epoxy adhesive film, preparation method of organic silicon/epoxy adhesive film and bendable laminated board |
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