CN112457632A - SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin and preparation method thereof - Google Patents

SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin and preparation method thereof Download PDF

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CN112457632A
CN112457632A CN202011292182.6A CN202011292182A CN112457632A CN 112457632 A CN112457632 A CN 112457632A CN 202011292182 A CN202011292182 A CN 202011292182A CN 112457632 A CN112457632 A CN 112457632A
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montmorillonite
epoxy resin
sio
high dielectric
dielectric property
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汪媛格
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Guangzhou Kaixie Technology Co ltd
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Priority to PCT/CN2021/092624 priority patent/WO2022105147A1/en
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    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/346—Clay
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

The invention relates to the technical field of epoxy resin, and discloses SiO with high dielectric property2The epoxy resin is synergistically modified by montmorillonite, and the mercapto nanometer SiO is treated under the action of a catalyst2Reacting the aminated montmorillonite with epoxy resin to obtain SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin, nano SiO2Has nanometer effect, unique microstructure of montmorillonite, strong binding force with macromolecular chain and chain segment of epoxy resin, synergistic inhibition of the macromolecular chain and chain segment movement of epoxy resin, and improved epoxy resin qualityThermal stability of the esters, SiO2The montmorillonite and the epoxy resin form an interface structure to capture free charges, so that space charges are accumulated to cause interface polarization and promote dipole polarization, and the two synergistically improve the relative dielectric constant of the epoxy resin to ensure SiO with high dielectric property2The montmorillonite synergistically modified epoxy resin has excellent thermal stability and dielectric property.

Description

SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin and preparation method thereof
Technical Field
The invention relates to the technical field of epoxy resin, in particular to SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin and a preparation method thereof.
Background
With the rapid increase of power consumption, the capacity and voltage level of electrical equipment are also higher and higher, so the requirement for safely operating electrical equipment is continuously increased, and the insulation material applied to the electrical equipment needs to have better electrical performance.
The epoxy resin has the advantages of stable chemical property, good mechanical property, good electrical insulation property and the like, has wide application prospect in the fields of electrical insulation, electronic industry and the like, but has poor thermal stability and dielectric property to be improved, the montmorillonite has unique microstructure and excellent electrical property and thermal stability, the nano-silica has unique nano-effect and can improve the dielectric property and the thermal stability of the epoxy resin, but the montmorillonite and the silica are easy to agglomerate in the epoxy resin to influence the addition effect of the epoxy resin, therefore, the SiO is adopted by people2The montmorillonite synergistically modifies the epoxy resin to solve the above problems.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides SiO with high dielectric property2The montmorillonite-modified epoxy resin and the preparation method thereof solve the problems of poor thermal stability and low dielectric property of the epoxy resin.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin, SiO with high dielectric properties2The preparation method of the-montmorillonite synergistically modified epoxy resin comprises the following steps:
(1) adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, stirring uniformly, adding montmorillonite at the temperature of 60-80 ℃, stirring at constant temperature for 1-3h with the mass ratio of the acrylamide to the montmorillonite being 10-20:100, carrying out vacuum filtration, washing with deionized water, and drying to obtain aminated montmorillonite;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, stirring for 2-4h at room temperature, placing the mixture into a reaction kettle, reacting for 4-8h at the temperature of 140 ℃ under the action of 100-;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into a reaction bottle, stirring uniformly, adding sulfhydrylated nano-silica-aminated montmorillonite, stirring uniformly, carrying out a reaction process, cooling to room temperature, adding curing agent methyltetrahydrophthalic anhydride and accelerator N, N-dimethylbenzylamine, stirring uniformly, defoaming in vacuum, pouring into a mold, heating and curing to form a film, and obtaining SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
Preferably, the water bath stirring instrument in the step (1) comprises a main body, a motor is movably connected to the bottom of the main body, a connecting block is movably connected to the top of the motor, a driving wheel is movably connected to the top of the connecting block, a driven wheel is movably connected to the left side of the driving wheel, a fixed wheel is movably connected to the top of the driving wheel, a magnetic wheel is movably connected to the left side of the fixed wheel, a partition board is movably connected to the middle of the main body, and a beaker is movably connected to the top of the partition board.
Preferably, the mass ratio of the aminated montmorillonite to the 3-mercaptopropyltrimethoxysilane in the step (2) is 100: 200-240.
Preferably, the mass ratio of the epoxy resin E44, the 1, 8-bis-dimethylamino naphthalene and the thiolated nano-silica-aminated montmorillonite in the step (3) is 100:0.4-1: 4-8.
Preferably, the reaction process in the step (3) is carried out at 200-240 ℃ for 30-90 min.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the SiO with high dielectric property2The epoxy resin is synergistically modified by the montmorillonite, acrylamide is intercalated into silicate sheets of the montmorillonite in a coordination compounding and hydrogen bond association mode to obtain aminated montmorillonite which is rich in amino and takes 3-mercaptopropyl trimethylOxysilane is a mercapto-containing silicon source precursor, aminated montmorillonite is used as a carrier, 3-mercaptopropyl trimethoxy silane is hydrolyzed through hydrothermal reaction to obtain nano-silica with mercapto on the surface, and the nano-silica is uniformly loaded on the surface and the lamellar structure of the aminated montmorillonite to reduce the agglomeration of the nano-silica, under the action of a catalyst 1, 8-bis-dimethylamino naphthalene, mercapto on the nano-silica is dehydrogenated to form mercapto anions, so that epoxy functional groups of epoxy resin are subjected to ring opening, hydrogen ions in the system are captured, the mercapto nano-silica is grafted to an epoxy resin matrix, meanwhile, amino on the aminated montmorillonite reacts with the epoxy groups, the aminated montmorillonite is subjected to covalent grafting with the epoxy resin, and the SiO with high dielectric property is obtained2-montmorillonite synergistically modifying epoxy resin.
The SiO with high dielectric property2The montmorillonite synergistically modified epoxy resin is characterized in that silica and montmorillonite are highly dispersed in an epoxy resin matrix through covalent grafting, the agglomeration phenomenon is reduced, a relatively stable region is formed, the structural stability and the thermal stability of the whole epoxy resin are improved, so that the glass transition temperature of the material is improved, nano-silica has a nano effect and inhibits the movement of a macromolecular chain and a chain segment of the epoxy resin, a unique microstructure of the montmorillonite has an ultrahigh specific surface area and strong binding force with the macromolecular chain and the chain segment of the epoxy resin, the interface stability is enhanced, the movement of the macromolecular chain and the chain segment of the epoxy resin is inhibited, and the glass transition temperature is further improved due to the synergistic effect of the silica and the montmorillonite, so that the thermal stability of the epoxy resin is improved.
The SiO with high dielectric property2Montmorillonite synergistically modified epoxy resin, nano silicon dioxide grafted to epoxy resin matrix, the nano effect of the epoxy resin enables molecular chains of silicon dioxide and epoxy resin to be adhered together, the polarity of the epoxy resin is enhanced, dipole polarization is increased, meanwhile, the interface structure of the silicon dioxide and the epoxy resin captures free charges in a medium, space charges are accumulated, interface polarization is caused, the relative dielectric constant of the epoxy resin is improved, the interlayer spacing of aminated montmorillonite is large, and covalent bonding is facilitatedEpoxy resin molecular chains are branched to form a good interface structure, so that free charges in a captured medium are promoted to be accumulated, interface polarization is caused, dipole polarization is promoted, the relative dielectric constant of the epoxy resin is further improved, and SiO with high dielectric property is enabled to be2The montmorillonite synergistically modified epoxy resin has excellent thermal stability and dielectric property.
Drawings
FIG. 1 is a schematic diagram of a water bath stirrer;
FIG. 2 is a schematic view of the gear in a bottom view;
fig. 3 is a schematic top view of the gear.
1. A main body; 2. a motor; 3. connecting blocks; 4. a driving wheel; 5. a driven wheel; 6. a fixed wheel; 7. a magnetic wheel; 8. a partition plate; 9. and (4) a beaker.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin, SiO with high dielectric property2The preparation method of the-montmorillonite synergistically modified epoxy resin comprises the following steps:
(1) adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, wherein the water bath stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, the left side of the driving wheel is movably connected with a driven wheel, the top of the driving wheel is movably connected with a fixed wheel, the left side of the fixed wheel is movably connected with a magnetic wheel, the middle of the main body is movably connected with a partition plate, the top of the partition plate is movably connected with a beaker, stirring is uniform, montmorillonite is added at 60-80 ℃, the mass ratio of the acrylamide to the montmorillonite is 10-20:100, stirring and reacting at constant temperature for 1-3 hours, carrying out reduced pressure suction;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, wherein the mass ratio of the deionized water to the ethanol to the diluted hydrochloric acid to the aminated montmorillonite is 100: 200-;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino naphthalene into a reaction bottle, stirring uniformly, adding thiolated nano-silica-aminated montmorillonite, wherein the mass ratio of the epoxy resin E44 to the 1, 8-bis-dimethylamino naphthalene to the thiolated nano-silica-aminated montmorillonite is 100:0.4-1:4-8, stirring uniformly, carrying out a reaction process, reacting at 200-240 ℃ for 30-90min, cooling to room temperature, adding curing agent methyltetrahydrophthalic anhydride and accelerant N, N-dimethylbenzylamine, stirring uniformly, defoaming in vacuum, pouring into a mold, heating and curing to form a film, and obtaining SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
Example 1
(1) Adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, wherein the water bath stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, the left side of the driving wheel is movably connected with a driven wheel, the top of the driving wheel is movably connected with a fixed wheel, the left side of the fixed wheel is movably connected with a magnetic wheel, the middle of the main body is movably connected with a partition plate, the top of the partition plate is movably connected with a beaker, stirring uniformly, adding montmorillonite at 60 ℃, wherein the mass ratio of the acrylamide to the montmorillonite is 10:100, stirring at constant temperature for 1h, carrying out reduced pressure suction filtration, washing;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, wherein the mass ratio of the deionized water to the ethanol to the diluted hydrochloric acid to the aminated montmorillonite is 100:200, stirring the mixture at room temperature for 2 hours, placing the mixture into a reaction kettle, reacting the mixture at 100 ℃ for 4 hours, cooling the mixture to room temperature, centrifuging the mixture, washing the mixture with deionized water and absolute ethyl alcohol, and drying the mixture to obtain thiolated nano silicon dioxide-aminated montmorillonite;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into a reaction bottle,stirring uniformly, adding sulfhydrylation nano-silica-amination montmorillonite, wherein the mass ratio of epoxy resin E44, 1, 8-bis-dimethylamino-naphthalene to sulfhydrylation nano-silica-amination montmorillonite is 100:0.4:4, stirring uniformly, carrying out a reaction process, reacting at 200 ℃ for 30min, cooling to room temperature, adding curing agent methyltetrahydrophthalic anhydride and accelerant N, N-dimethylbenzylamine, stirring uniformly, defoaming in vacuum, pouring into a mold, heating and curing to form a film, and obtaining SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
Example 2
(1) Adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, wherein the water bath stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, the left side of the driving wheel is movably connected with a driven wheel, the top of the driving wheel is movably connected with a fixed wheel, the left side of the fixed wheel is movably connected with a magnetic wheel, the middle of the main body is movably connected with a partition plate, the top of the partition plate is movably connected with a beaker, stirring is uniform, montmorillonite is added at 65 ℃, the mass ratio of the acrylamide to the montmorillonite is 13:100, stirring and reacting at constant temperature for 1.5 hours, carrying out vacuum filtration;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, wherein the mass ratio of the deionized water to the ethanol to the aminated montmorillonite is 100:210, stirring for 2.5h at room temperature, placing the mixture into a reaction kettle, reacting for 5h at 110 ℃, cooling to room temperature, centrifuging, washing with deionized water and absolute ethyl alcohol, and drying to obtain thiolated nano silicon dioxide-aminated montmorillonite;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into a reaction bottle, stirring uniformly, adding thiolated nano-silica-aminated montmorillonite, wherein the mass ratio of the epoxy resin E44 to the epoxy resin E44 to the 1, 8-bis-dimethylamino-naphthalene to the thiolated nano-silica-aminated montmorillonite is 100:0.6:5.3, stirring uniformly, carrying out a reaction process, wherein the reaction process is carried out at 210 ℃ for 50min, cooling to room temperature, addingAdding curing agent methyltetrahydrophthalic anhydride and accelerator N, N-dimethylbenzylamine, stirring uniformly, defoaming in vacuum, pouring into a mould, heating and curing to form a film, and obtaining SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
Example 3
(1) Adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, wherein the water bath stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, the left side of the driving wheel is movably connected with a driven wheel, the top of the driving wheel is movably connected with a fixed wheel, the left side of the fixed wheel is movably connected with a magnetic wheel, the middle of the main body is movably connected with a partition plate, the top of the partition plate is movably connected with a beaker, stirring uniformly, adding montmorillonite at 70 ℃, wherein the mass ratio of the acrylamide to the montmorillonite is 16:100, stirring at constant temperature for 2 hours, carrying out reduced pressure suction filtration, washing;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, wherein the mass ratio of the deionized water to the ethanol to the diluted hydrochloric acid to the aminated montmorillonite is 100:225, stirring the mixture at room temperature for 3 hours, placing the mixture into a reaction kettle, reacting the mixture at 120 ℃ for 6 hours, cooling the mixture to room temperature, centrifuging the mixture, washing the mixture with deionized water and absolute ethyl alcohol, and drying the mixture to obtain thiolated nano silicon dioxide-aminated montmorillonite;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into a reaction bottle, stirring uniformly, adding thiolated nano-silica-aminated montmorillonite, wherein the mass ratio of the epoxy resin E44 to the 1, 8-bis-dimethylamino-naphthalene to the thiolated nano-silica-aminated montmorillonite is 100:0.8:6.6, stirring uniformly, carrying out a reaction process, wherein the reaction process is to react at 225 ℃ for 70min, cooling to room temperature, adding curing agent methyltetrahydrophthalic anhydride and accelerant N, N-dimethylbenzylamine, stirring uniformly, carrying out vacuum deaeration, pouring into a mold, heating and curing to form a film, and obtaining SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
Example 4
(1) Adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, wherein the water bath stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, the left side of the driving wheel is movably connected with a driven wheel, the top of the driving wheel is movably connected with a fixed wheel, the left side of the fixed wheel is movably connected with a magnetic wheel, the middle of the main body is movably connected with a partition plate, the top of the partition plate is movably connected with a beaker, stirring uniformly, adding montmorillonite at 80 ℃, wherein the mass ratio of the acrylamide to the montmorillonite is 20:100, stirring at constant temperature for 3 hours, carrying out reduced pressure suction filtration, washing;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, wherein the mass ratio of the deionized water to the ethanol to the diluted hydrochloric acid to the aminated montmorillonite is 100:240, stirring at room temperature for 4 hours, placing the mixture into a reaction kettle, reacting at 140 ℃ for 8 hours, cooling to room temperature, centrifuging, washing with deionized water and absolute ethyl alcohol, and drying to obtain thiolated nano-silica-aminated montmorillonite;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into a reaction bottle, stirring uniformly, adding thiolated nano-silica-aminated montmorillonite, wherein the mass ratio of the epoxy resin E44 to the 1, 8-bis-dimethylamino-naphthalene to the thiolated nano-silica-aminated montmorillonite is 100:1:8, stirring uniformly, carrying out a reaction process, reacting at 240 ℃ for 90min, cooling to room temperature, adding curing agent methyltetrahydrophthalic anhydride and accelerator N, N-dimethylbenzylamine, stirring uniformly, carrying out vacuum deaeration, pouring into a mold, heating and curing to form a film, and obtaining the SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
Comparative example 1
(1) Adding deionized water and acrylamide into a reaction bottle, placing the reaction bottle in a water bath stirrer, wherein the water bath stirrer comprises a main body, the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, the left side of the driving wheel is movably connected with a driven wheel, the top of the driving wheel is movably connected with a fixed wheel, the left side of the fixed wheel is movably connected with a magnetic wheel, the middle of the main body is movably connected with a partition plate, the top of the partition plate is movably connected with a beaker, stirring uniformly, adding montmorillonite at 7 ℃, wherein the mass ratio of the acrylamide to the montmorillonite is 5:100, stirring at constant temperature for 2 hours, carrying out reduced pressure suction filtration, washing;
(2) adding deionized water, ethanol, diluted hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into a reaction bottle, wherein the mass ratio of the deionized water to the ethanol to the diluted hydrochloric acid to the aminated montmorillonite is 100:160, stirring for 3 hours at room temperature, placing the mixture into a reaction kettle, reacting for 6 hours at 120 ℃, cooling to room temperature, centrifuging, washing with deionized water and absolute ethyl alcohol, and drying to obtain thiolated nano-silica-aminated montmorillonite;
(3) adding deionized water, epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into a reaction bottle, stirring uniformly, adding thiolated nano-silica-aminated montmorillonite, wherein the mass ratio of the epoxy resin E44 to the 1, 8-bis-dimethylamino-naphthalene to the thiolated nano-silica-aminated montmorillonite is 100:0.2:2, stirring uniformly, carrying out a reaction process, wherein the reaction process is to react for 60min at 220 ℃, cooling to room temperature, adding curing agent methyltetrahydrophthalic anhydride and accelerator N, N-dimethylbenzylamine, stirring uniformly, carrying out vacuum deaeration, pouring into a mold, heating and curing to form a film, and obtaining the SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
SiO having high dielectric properties obtained in examples and comparative examples was tested using a differential scanning calorimeter of PT-DSC type2The glass transition temperature of the montmorillonite synergistically modified epoxy resin is GB/T22567-2008.
Figure BDA0002784219680000091
With the high dielectric properties of SiO obtained in the examples and comparative examples2Montmorillonite synergistically modifying epoxy resin to give a sample of 20mm by 20mm specification and coating conductive carbon of approximately 1um thickness on both sides with screen-printed platesAnd (3) testing the relative dielectric constant and the dielectric loss factor of the sample by using a DMS-2000 type broadband dielectric spectrometer, wherein the testing standard is GB/T31838.1-2015.
Figure BDA0002784219680000092

Claims (5)

1. SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin characterized by: the SiO with high dielectric property2The preparation method of the-montmorillonite synergistically modified epoxy resin comprises the following steps:
(1) adding acrylamide into deionized water, placing the mixture into a water bath stirrer, stirring uniformly, adding montmorillonite at the temperature of 60-80 ℃, stirring and reacting for 1-3h at constant temperature, decompressing, filtering, washing and drying to obtain aminated montmorillonite, wherein the mass ratio of the acrylamide to the montmorillonite is 10-20: 100;
(2) adding ethanol, dilute hydrochloric acid, aminated montmorillonite and 3-mercaptopropyl trimethoxy silane into deionized water, stirring for 2-4h at room temperature, placing in a reaction kettle, reacting for 4-8h at the temperature of 140 ℃ under the temperature of 100-;
(3) adding epoxy resin E44 and catalyst 1, 8-bis-dimethylamino-naphthalene into deionized water, stirring uniformly, adding sulfhydrylated nano-silica-aminated montmorillonite, stirring uniformly, carrying out a reaction process, cooling, adding curing agent methyltetrahydrophthalic anhydride and accelerator N, N-dimethylbenzylamine, stirring uniformly, defoaming in vacuum, pouring into a mold, heating and curing to form a film, and obtaining SiO with high dielectric property2-montmorillonite synergistically modifying epoxy resin.
2. The SiO with high dielectric property as claimed in claim 12-montmorillonite synergistically modified epoxy resin characterized by: the water bath stirring instrument in the step (1) comprises a main body, wherein the bottom of the main body is movably connected with a motor, the top of the motor is movably connected with a connecting block, the top of the connecting block is movably connected with a driving wheel, and the left side of the driving wheelThe movable connection has the follower, and the top swing joint of action wheel has the tight pulley, and the left side swing joint of tight pulley has the magnetic force wheel, and the centre swing joint of main part has the baffle, and the top swing joint of baffle has the beaker.
3. The SiO with high dielectric property as claimed in claim 12-montmorillonite synergistically modified epoxy resin characterized by: the mass ratio of the aminated montmorillonite to the 3-mercaptopropyltrimethoxysilane in the step (2) is 100: 200-240.
4. The SiO with high dielectric property as claimed in claim 12-montmorillonite synergistically modified epoxy resin characterized by: the mass ratio of the epoxy resin E44, the 1, 8-bis-dimethylamino naphthalene and the sulfhydrylation nano silicon dioxide-amination montmorillonite in the step (3) is 100:0.4-1: 4-8.
5. The SiO with high dielectric property as claimed in claim 12-montmorillonite synergistically modified epoxy resin characterized by: the reaction process in the step (3) is carried out at 200-240 ℃ for 30-90 min.
CN202011292182.6A 2020-11-18 2020-11-18 SiO with high dielectric property2-montmorillonite synergistically modified epoxy resin and preparation method thereof Withdrawn CN112457632A (en)

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WO2022105147A1 (en) * 2020-11-18 2022-05-27 广州凯协科技有限公司 High-dielectric-performance epoxy resin synergistically modified with sio2-montmorillonite and preparation method therefor
CN118308053A (en) * 2024-04-01 2024-07-09 惠东县合成化工实业有限公司 Preparation method of modified epoxy resin adhesive

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