CN112552643A - Epoxy resin-based heat insulation material and preparation method thereof - Google Patents
Epoxy resin-based heat insulation material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an epoxy resin-based heat-insulating material and a preparation method thereof, and relates to the technical field of heat-insulating material preparation. An epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and anhydride moderate-temperature curing agent; the adding mass of the hexagonal boron nitride is 1-25% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 1-10% of that of the epoxy resin. The epoxy resin-based heat insulation material is of a stacked structure, the preparation method of the material is simple, the obtained material has good heat insulation performance under a certain proportion, the temperature rise time of the top surface can be delayed, local high-temperature hot spots can be effectively avoided, the capability of quickly dissipating heat and cooling in all directions is realized, and the application prospect of protecting electronic devices is realized.
Description
Technical Field
The invention relates to the technical field of heat insulation material preparation, in particular to an epoxy resin-based heat insulation material and a preparation method thereof.
Background
Insulation refers to materials that retard the transmission of heat flow. In recent years, as the electronic industry and the energy industry become important pivots for economic development, energy conservation, consumption reduction and heat insulation have been more emphasized. With the rapid development of heat insulation materials, the heat insulation materials are widely applied in the industries of aerospace, electronics, buildings and the like.
At present, the development of heat insulation materials mainly plays a role in heat preservation and heat insulation through means of reducing the heat conductivity of the heat insulation materials (such as aerogel, ceramic and the like). For some electronic device industries, the phenomenon of heat accumulation exists, which easily causes the problem of local high-temperature hot spots, thereby limiting the application.
The invention provides an epoxy resin-based thermal insulation material and a preparation method thereof through macroscopic anisotropy of the material, achieves the effects of edge heat dissipation and top thermal insulation, and overcomes the common problems of local high-temperature hot spots and short-term high-temperature impact of the thermal insulation material.
Disclosure of Invention
Aiming at the problems, the invention provides an epoxy resin-based heat-insulating material and a preparation method thereof.
The technical scheme of the invention is as follows:
an epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and anhydride moderate-temperature curing agent; the adding mass of the hexagonal boron nitride is 1-25% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 1-10% of that of the epoxy resin.
Further, the pretreatment of the expanded vermiculite comprises the following steps: and (3) placing the expanded vermiculite in deionized water for ultrasonic treatment for 2-3 h to remove lower-layer impurities, then drying, placing at 850-1000 ℃ for treatment for 1-2 h, naturally cooling, and then grinding into powder.
Further, the pretreatment of the hexagonal boron nitride: placing hexagonal boron nitride in isopropanol for ultrasonic treatment for 3-6 h, centrifuging, drying, and then grinding into powder.
Further, the mass ratio of the epoxy resin, the anhydride moderate-temperature curing agent, DMP-30 and n-butyl glycidyl ether is as follows: 0.40-0.58: 0.30-0.41: 0.01: 0.2 to 0.5.
Further, the acid anhydride medium-temperature curing agent is one of methyl nadic anhydride or phthalic anhydride.
In addition, the invention also provides a preparation method of the epoxy resin-based heat-insulating material, which comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, an anhydride moderate-temperature curing agent, DMP-30, n-butyl glycidyl ether and hexagonal boron nitride at 60 ℃ for 30-60 min to obtain a hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, the anhydride moderate-temperature curing agent, DMP-30, n-butyl glycidyl ether and expanded vermiculite at 60 ℃ for 30-60 min to obtain an expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 50-80 min at 60 ℃; then, deflating, and heating to 110-130 ℃ for curing for 1.5-2.5 h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60-90 min at 60 ℃; then, deflating, heating to 110-130 ℃, curing for 2-2.5 h, continuing to heat to 140 ℃, curing for 1.5-2.5 h, and finally heating to 180 ℃, curing for 1.5-2.5 h to obtain a unit heat insulation material;
and S4, repeating the operations of S2-S3 on the basis of the unit heat insulation material to obtain the epoxy resin-based heat insulation material with the stacked structure.
The beneficial effects of the invention are as follows: the epoxy resin-based heat insulation material is in an anisotropic stacked structure, the preparation method of the material is simple, the obtained material has good heat insulation performance under a certain proportion, the temperature rise time of the top surface can be delayed, local high-temperature hot spots can be effectively avoided, the capability of quickly dissipating heat and cooling in all directions is realized, and the application prospect of protecting electronic devices is realized.
Drawings
FIG. 1 is a graph showing the temperature variation trend of the center of the top of a sample after the bottom of the sample is heated by a 120 ℃ point heat source; wherein, Epon: pure epoxy resin material, i.e. pure sample obtained in comparative example 3; e-ver: sample obtained in comparative example 1; APCs-5: the sample obtained in example 1; APCs-15: example 2 sample obtained; APCs-25: the sample obtained in example 3;
FIG. 2 is a thermal infrared imaging change diagram of the temperature change at the top of a sample after the bottom of the sample is heated by a 120 ℃ surface heat source according to the present invention; wherein the stacked structure is the epoxy resin-based heat insulating material of the stacked structure obtained in embodiment 3;
FIG. 3 is a thermal infrared imaging change diagram of the temperature change at the top of a sample after the bottom of the sample is heated by a 120 ℃ point heat source; wherein the stacked structure is the epoxy resin-based heat insulating material of the stacked structure obtained in embodiment 3; shown in the figure are 9 a temperature change curve of a pure sample, 10 a temperature change curve of a comparative sample 2, 11 a temperature change curve of a stacked structure, and 12 a temperature change curve of the comparative sample 1;
FIG. 4 is a graph showing the temperature variation trend of the center of the top of a sample after the bottom of the sample is heated by a surface heat source at 80 ℃ according to the present invention; wherein the stacked structure is the epoxy resin-based heat insulating material of the stacked structure obtained in embodiment 3;
FIG. 5 is a graph showing the natural cooling temperature change at 80 ℃ in the sample chamber of the present invention; in the figure, (a) shows a top temperature profile and (b) shows a side temperature profile;
fig. 6 shows a testing table for testing heat insulation performance according to the present invention.
In the figure: 1. a transformer; 2. fixing a workbench; 3. heating a tube; 4. a data acquisition instrument; 5. measuring points; 6. a sample; 7. a fixing clip; 8. provided is a thermal infrared imager.
Detailed Description
The embodiments of the present invention can be obtained by different substitutions in specific ranges based on the above technical solutions, and therefore, the following embodiments are only preferred embodiments of the embodiments, and any technical substitutions made by the above technical solutions are within the protection scope of the present invention.
The invention also provides a heat insulation performance test bench for testing the material as shown in fig. 6, the heat insulation performance test bench is composed of a transformer 1, a fixed workbench 2, a heating pipe 3, a data acquisition instrument 4, measurement points 5, a sample 6, a fixing clamp 7 and a thermal infrared imager 8, the transformer 1 is connected with the heating pipe 3 and used for supplying power to the heating pipe 3, the heating pipe 3 is positioned at the top of the fixed workbench 2, the sample 6 is placed at the top of the heating pipe 3, five measurement points 5 are arranged on the surface of the sample 6, the data acquisition instrument 4 is used for measuring the measurement points 5, and the thermal infrared imager 8 is used for acquiring heat distribution data of the sample 6 and clamping the sample 6 by the fixing clamp 7.
Example 1
An epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and methyl nadic anhydride; the adding mass of the hexagonal boron nitride is 5% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 1% of that of the epoxy resin. The pretreatment of the expanded vermiculite comprises the following steps: placing expanded vermiculite in deionized water for ultrasonic treatment for 2h to remove lower-layer impurities, then drying, placing at 850 ℃ for treatment for 1h, naturally cooling, and grinding into powder; the pretreatment of the hexagonal boron nitride: putting the hexagonal boron nitride into isopropanol for ultrasonic treatment for 3h, centrifuging, drying and then grinding into powder. The mass ratio of the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether is as follows: 0.40: 0.30: 0.01: 0.2.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the hexagonal boron nitride at 60 ℃ for 30min to obtain a hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the expanded vermiculite at 60 ℃ for 30min to obtain an expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 50min at 60 ℃; then, deflating, heating to 110 ℃, and curing for 1.5h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 110 ℃ for curing for 2h, continuing to heat to 140 ℃ for curing for 1.5h, and finally heating to 180 ℃ for curing for 1.5h to obtain a unit heat-insulating material;
and S4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining the epoxy resin-based heat insulation material with the stacked structure.
Example 2
An epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and methyl nadic anhydride; the adding mass of the hexagonal boron nitride is 15% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 1% of that of the epoxy resin. The pretreatment of the expanded vermiculite comprises the following steps: placing the expanded vermiculite in deionized water for ultrasonic treatment for 2.5h to remove lower-layer impurities, then drying, placing in a temperature of 950 ℃ for treatment for 1.5h, naturally cooling, and grinding into powder; the pretreatment of the hexagonal boron nitride: putting the hexagonal boron nitride into isopropanol, carrying out ultrasonic treatment for 4.5h, centrifuging, drying, and then grinding into powder. The mass ratio of the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether is as follows: 0.48: 0.35: 0.01: 0.4.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the hexagonal boron nitride at 60 ℃ for 45min to obtain a hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the expanded vermiculite at 60 ℃ for 45min to obtain an expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃, and curing for 2h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃ for curing for 2.2h, continuing to heat to 140 ℃ for curing for 2h, and finally heating to 180 ℃ for curing for 2h to obtain a unit heat-insulating material;
and S4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining the epoxy resin-based heat insulation material with the stacked structure.
Example 3
An epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and methyl nadic anhydride; the adding mass of the hexagonal boron nitride is 25% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 1% of that of the epoxy resin. The pretreatment of the expanded vermiculite comprises the following steps: placing expanded vermiculite in deionized water for ultrasonic treatment for 3h to remove lower-layer impurities, then drying, placing at 1000 ℃ for treatment for 2h, naturally cooling, and grinding into powder; the pretreatment of the hexagonal boron nitride: placing hexagonal boron nitride in isopropanol for ultrasonic treatment for 6h, centrifuging, drying, and grinding into powder. The mass ratio of the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether is as follows: 0.58: 0.41: 0.01: 0.5.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the hexagonal boron nitride at 60 ℃ for 60min to obtain a hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the expanded vermiculite at 60 ℃ for 60min to obtain an expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 80min at 60 ℃; then, deflating, heating to 130 ℃, and curing for 2.5h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 90min at 60 ℃; then deflating, heating to 130 ℃ for curing for 2.5h, continuing to heat to 140 ℃ for curing for 2.5h, and finally heating to 180 ℃ for curing for 2.5h to obtain a unit heat-insulating material;
and S4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining the epoxy resin-based heat insulation material with the stacked structure.
Example 4
An epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and phthalic anhydride; the adding mass of the hexagonal boron nitride is 15% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 5% of that of the epoxy resin. The pretreatment of the expanded vermiculite comprises the following steps: placing expanded vermiculite in deionized water for ultrasonic treatment for 2h to remove lower-layer impurities, then drying, placing at 850 ℃ for treatment for 1h, naturally cooling, and grinding into powder; the pretreatment of the hexagonal boron nitride: putting the hexagonal boron nitride into isopropanol for ultrasonic treatment for 3h, centrifuging, drying and then grinding into powder. The mass ratio of the epoxy resin, phthalic anhydride, DMP-30 to n-butyl glycidyl ether is as follows: 0.40: 0.30: 0.01: 0.2.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, phthalic anhydride, DMP-30, n-butyl glycidyl ether and hexagonal boron nitride at 60 ℃ for 30min to obtain hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, phthalic anhydride, DMP-30, n-butyl glycidyl ether and expanded vermiculite at 60 ℃ for 30min to obtain expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 50min at 60 ℃; then, deflating, heating to 110 ℃, and curing for 1.5h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 110 ℃ for curing for 2h, continuing to heat to 140 ℃ for curing for 1.5h, and finally heating to 180 ℃ for curing for 1.5h to obtain a unit heat-insulating material;
and S4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining the epoxy resin-based heat insulation material with the stacked structure.
Example 5
An epoxy resin-based heat insulating material in a stacked structure comprises the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and phthalic anhydride; the adding mass of the hexagonal boron nitride is 25% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 10% of that of the epoxy resin. The pretreatment of the expanded vermiculite comprises the following steps: placing expanded vermiculite in deionized water for ultrasonic treatment for 2h to remove lower-layer impurities, then drying, placing at 850 ℃ for treatment for 1h, naturally cooling, and grinding into powder; the pretreatment of the hexagonal boron nitride: putting the hexagonal boron nitride into isopropanol for ultrasonic treatment for 3h, centrifuging, drying and then grinding into powder. The mass ratio of the epoxy resin, phthalic anhydride, DMP-30 to n-butyl glycidyl ether is as follows: 0.40: 0.30: 0.01: 0.2.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, phthalic anhydride, DMP-30, n-butyl glycidyl ether and hexagonal boron nitride at 60 ℃ for 30min to obtain hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, phthalic anhydride, DMP-30, n-butyl glycidyl ether and expanded vermiculite at 60 ℃ for 30min to obtain expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 50min at 60 ℃; then, deflating, heating to 110 ℃, and curing for 1.5h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 110 ℃ for curing for 2h, continuing to heat to 140 ℃ for curing for 1.5h, and finally heating to 180 ℃ for curing for 1.5h to obtain a unit heat-insulating material;
and S4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining the epoxy resin-based heat insulation material with the stacked structure.
Comparative example 1
An epoxy resin-based heat insulating material comprises the following raw materials: epoxy resin, expanded vermiculite, DMP-30, n-butyl glycidyl ether and methyl nadic anhydride; the adding mass of the expanded vermiculite is 1% of that of the epoxy resin. The pretreatment of the expanded vermiculite comprises the following steps: placing the expanded vermiculite in deionized water for ultrasonic treatment for 2.5h to remove lower-layer impurities, then drying, placing in a temperature of 950 ℃ for treatment for 1.5h, naturally cooling, and grinding into powder; the mass ratio of the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether is as follows: 0.48: 0.35: 0.01: 0.4.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the expanded vermiculite at 60 ℃ for 45min to obtain an expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the expanded vermiculite-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃ and curing for 2h to obtain expanded vermiculite-epoxy sheets;
s3, taking a molding layer: taking down the die, pouring the expanded vermiculite-epoxy preparation solution on the surface of the expanded vermiculite-epoxy sheet, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃ for curing for 2.2h, continuing to heat to 140 ℃ for curing for 2h, and finally heating to 180 ℃ for curing for 2h to obtain a unit heat-insulating material;
s4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material to obtain a comparison sample 1.
Comparative example 2
An epoxy resin-based heat insulating material comprises the following raw materials: epoxy resin, hexagonal boron nitride, DMP-30, n-butyl glycidyl ether and methyl nadic anhydride; the adding mass of the hexagonal boron nitride is 15% of that of the epoxy resin. The pretreatment of the hexagonal boron nitride: putting the hexagonal boron nitride into isopropanol, carrying out ultrasonic treatment for 4.5h, centrifuging, drying, and then grinding into powder. The mass ratio of the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether is as follows: 0.48: 0.35: 0.01: 0.4.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30, the n-butyl glycidyl ether and the hexagonal boron nitride at 60 ℃ for 45min to obtain a hexagonal boron nitride-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃, and curing for 2h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring the hexagonal boron nitride-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃ for curing for 2.2h, continuing to heat to 140 ℃ for curing for 2h, and finally heating to 180 ℃ for curing for 2h to obtain a unit heat-insulating material;
s4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining a comparison sample 2.
Comparative example 3
An epoxy resin-based heat insulating material comprises the following raw materials: epoxy resin, DMP-30, n-butyl glycidyl ether and methyl nadic anhydride; the mass ratio of the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether is as follows: 0.48: 0.35: 0.01: 0.4.
a preparation method of an epoxy resin-based heat insulation material comprises the following steps:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, the methyl nadic anhydride, the DMP-30 and the n-butyl glycidyl ether at 60 ℃ for 45min to obtain epoxy preparation liquid;
s2, molding and curing: pouring the epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 60min at 60 ℃; then deflating, heating to 120 ℃ and curing for 2h to obtain epoxy sheets;
s3, taking a molding layer: taking down the mold, pouring epoxy preparation liquid on the surface of the epoxy sheet, and vacuumizing for 60min at 60 ℃; then, deflating, heating to 120 ℃ for curing for 2.2h, continuing to heat to 140 ℃ for curing for 2h, and finally heating to 180 ℃ for curing for 2h to obtain a unit heat-insulating material;
and S4, repeating the operations of S2-S3 for 1 time on the basis of the unit heat insulation material, and obtaining the pure sample.
The above examples and comparative examples were subjected to the associated heating and the change in the top temperature thereof was measured. The heat pipe is used as a point heat source, the silicon rubber heating plate is used as a surface heat source, the regulator is used as constant voltage, continuous and stable temperature is provided at the bottom of the sample, a top temperature curve is recorded through a data acquisition instrument, the top temperature is acquired through an infrared imager, and the results are shown in table 1 and fig. 1-6.
TABLE 1 thermal insulation Properties on the Top of epoxy resin-based insulation Material
The insulation ratio refers to the percentage of temperature reduction of the sample compared to the top of the pure sample at different measurement times and temperatures. As can be seen from Table 1, the samples obtained in the examples have lower top temperatures than the pure samples at different measurement times and different temperatures, regardless of the point heat source or the surface heat source; the reduction amplitude of the sample obtained in the comparative example is far lower than that of the sample obtained in the example, and the sample obtained in the example has good heat insulation effect.
FIG. 1 is a graph showing the temperature change at the top of different samples with the bottom of the inventive sample heated by a point heat source at 120 ℃. It can be seen that the top temperature of the samples of examples 1-3 is reduced by 10-15 ℃ compared with that of comparative samples 1 and 3, which indicates that the samples obtained in examples 1-3 can have good heat insulation effect, and further indicates that the service life of the electronic device can be prolonged.
FIG. 2 is a graph of thermal infrared imaging of temperature change at the top of different samples with the bottom of the inventive sample heated by a 120 ℃ surface heat source. It can be seen that white high-temperature hot spots appear in the comparative examples 1-3, the example sample does not appear, and the temperature rise time is well prolonged, so that the sample obtained in the embodiment can effectively avoid the high-temperature local hot spots.
FIG. 3 is a thermal infrared imaging graph showing the temperature change of the top of different samples after the bottom of the sample of the invention is heated by a point heat source at 120 ℃. It can be seen that white high-temperature hot spots appear in the comparative examples 1-3, the example sample does not appear, and the temperature rise time is well prolonged, so that the sample obtained in the embodiment can effectively avoid the high-temperature local hot spots.
Therefore, as can be seen from fig. 2 and 3, the sample obtained by the embodiment can effectively avoid the high-temperature local hot spot regardless of whether the point heat source or the surface heat source heats the bottom of the sample.
FIG. 4 is a graph showing the temperature change at the top of different samples with the bottom of the inventive sample heated by a surface heat source at 80 ℃. It can be seen that the top temperature of the sample of example 3 is reduced compared to the sample of comparative example, which is 22.37% lower than the top temperature of the sample of comparative example 2 or the pure sample of example 3 and 6.12% lower than the top temperature of the sample of comparative example 1 at 400s, indicating that the sample of example has a good thermal insulating effect, further indicating that it can improve the lifetime of the electronic device.
Fig. 5 is a graph showing the temperature change of the sample of the present invention, which is simultaneously heated to 80 ℃ and then naturally cooled at room temperature, wherein (a) shows the top temperature change and (b) shows the side temperature change. As can be seen from the figure, the sample of the embodiment has the capability of rapidly dissipating heat and reducing temperature in all directions.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (6)
1. An epoxy resin-based heat insulating material is characterized by being of a stacked structure and comprising the following raw materials: epoxy resin, hexagonal boron nitride, expanded vermiculite, DMP-30, n-butyl glycidyl ether and anhydride moderate-temperature curing agent; the adding mass of the hexagonal boron nitride is 1-25% of that of the epoxy resin, and the adding mass of the expanded vermiculite is 1-10% of that of the epoxy resin.
2. The epoxy resin-based heat insulating material according to claim 1, wherein the pre-treatment of the expanded vermiculite is: and (3) placing the expanded vermiculite in deionized water for ultrasonic treatment for 2-3 h to remove lower-layer impurities, then drying, placing at 850-1000 ℃ for treatment for 1-2 h, naturally cooling, and then grinding into powder.
3. The epoxy resin-based heat insulating material according to claim 1, wherein the hexagonal boron nitride pretreatment: placing hexagonal boron nitride in isopropanol for ultrasonic treatment for 3-6 h, centrifuging, drying, and then grinding into powder.
4. The epoxy resin-based heat insulating material according to claim 1, wherein the mass ratio of the epoxy resin, the anhydride moderate-temperature curing agent, DMP-30 and n-butyl glycidyl ether is: 0.40-0.58: 0.30-0.41: 0.01: 0.2 to 0.5.
5. The epoxy resin-based heat insulating material according to claim 1, wherein the acid anhydride mid-temperature curing agent is one of methylnadic anhydride or phthalic anhydride.
6. The method for preparing an epoxy resin-based heat insulating material according to any one of claims 1 to 5, comprising the steps of:
s1, preparation of a preparation solution: mixing and stirring the epoxy resin, an anhydride moderate-temperature curing agent, DMP-30, n-butyl glycidyl ether and hexagonal boron nitride at 60 ℃ for 30-60 min to obtain a hexagonal boron nitride-epoxy preparation solution; mixing and stirring the epoxy resin, the anhydride moderate-temperature curing agent, DMP-30, n-butyl glycidyl ether and expanded vermiculite at 60 ℃ for 30-60 min to obtain an expanded vermiculite-epoxy preparation solution;
s2, molding and curing: pouring the hexagonal boron nitride-epoxy preparation solution into a polytetrafluoroethylene mold, and vacuumizing for 50-80 min at 60 ℃; then, deflating, and heating to 110-130 ℃ for curing for 1.5-2.5 h to obtain a semi-cured hexagonal boron nitride-epoxy layer;
s3, taking a molding layer: taking down the mold, pouring expanded vermiculite-epoxy preparation solution on the surface of the semi-solidified hexagonal boron nitride-epoxy layer, and vacuumizing for 60-90 min at 60 ℃; then, deflating, heating to 110-130 ℃, curing for 2-2.5 h, continuing to heat to 140 ℃, curing for 1.5-2.5 h, and finally heating to 180 ℃, curing for 1.5-2.5 h to obtain a unit heat insulation material;
and S4, repeating the operations of S2-S3 on the basis of the unit heat insulation material to obtain the epoxy resin-based heat insulation material with the stacked structure.
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