CN110903608A - High-thermal-conductivity epoxy composite material and preparation method thereof - Google Patents
High-thermal-conductivity epoxy composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-thermal-conductivity epoxy composite material and a preparation method thereof. The secondary modification method can effectively improve the dispersibility of the hexagonal boron nitride in the epoxy resin, so that the thermal conductivity and the mechanical property of the epoxy resin composite material taking the secondary modified particles as the filler are obviously improved.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a high-thermal-conductivity epoxy composite material and a preparation method thereof.
Background
Epoxy resin is widely used as thermosetting polymer in the fields of insulation and packaging of high and low voltage electric appliances, motors and electronic components due to the advantages of good electrical insulation, large structural density, good sealing performance and the like. However, the epoxy resin has the defects of poor heat conductivity, high crosslinking density, brittle quality and the like, so that the application of the epoxy resin is limited to a certain extent. Boron nitride has a high thermal conductivity (about 200W/(m · K)), has a graphene-like lamellar structure and excellent electrical insulation properties, and has a low thermal expansion coefficient, and thus is often used as a thermal conductive filler for increasing the thermal conductivity of a polymer matrix. However, due to the influence of polarity, surface chemical groups and the like, BN is difficult to disperse in a polymer matrix and is easy to agglomerate, and the interface compatibility of the composite material prepared from the inorganic filler and the organic epoxy matrix is poor, so that the continuous structure of the epoxy resin is damaged, the mechanical property of the composite material is obviously reduced, and the application of the epoxy resin composite material is limited.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity epoxy composite material and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-thermal-conductivity epoxy composite material comprises the following steps:
s1, adding 10 parts by mass of BN into a beaker, pouring ultrapure water into the beaker, and dispersing the ultrapure water at a high speed;
s2, adding 0.315 parts by mass of Tris-HCL into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH value to be alkaline, and performing centrifugal separation after full magnetic stirring reaction to obtain a precipitate;
s3, washing the precipitate obtained by centrifuging the S2 to obtain a final precipitate, drying the final precipitate, and grinding the dried final precipitate into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and fully stirring to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and fully stirring to obtain a mixture;
s5, centrifuging the mixture obtained in the S4 to obtain a precipitate; fully washing the precipitate with absolute ethyl alcohol to obtain a final precipitate, drying the final precipitate, and grinding the dried final precipitate into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, fully stirring the prepared epoxy resin in the S6; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution and preheating the mixed solution;
s8, preparing 20-80 parts by mass of k-DBN and 185 parts by mass of preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring to obtain mixed liquor;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and fully stirring to obtain a mixed liquid;
s10, injecting the mixed solution obtained in the step S9 into a mould, placing the mould in a vacuum drying oven for vacuum pumping and degassing until no obvious gas is separated out, and then curing; and finally, cooling and demolding at room temperature to obtain the final sample.
Further, in S1, the BN had a particle size of 15 μm and a purity of 99.5%.
Further, in S2, the pH was adjusted to 8.5 using 0.1mol/L NaOH solution.
Further, in S7, the epoxy resin was maintained at 60 ℃ by an oil bath during magnetic stirring.
Further, in S8, an oil bath environment at 60 ℃ was maintained during the stirring with the mechanical stirrer.
Further, in the above-mentioned case,
s1, adding 10 parts by mass of BN into a beaker, then pouring ultrapure water into the beaker, and dispersing the mixture at a high speed for 30min by using a high-speed dispersion machine;
s2, adding 0.315 part by mass of Tris-HCL into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH to 8.5, carrying out magnetic stirring reaction for 6 hours at the temperature of 25 ℃, and then carrying out centrifugal separation at the rotating speed of 3000r/min to obtain a precipitate;
s3, washing the precipitate obtained by centrifuging the S2 by using ultrapure water for 5 times to obtain a final precipitate, drying the final precipitate by using a blast dryer at 50 ℃ for 24 hours, and finally grinding the final precipitate into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and stirring for 10min at 60 ℃ by using a magnetic stirrer to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and stirring for 3 hours at the temperature of 60 ℃ by using a magnetic stirrer to obtain a mixture;
s5, performing centrifugal separation on the mixture obtained in the step S4 at the rotating speed of 3000r/min to obtain a precipitate; washing the precipitate with anhydrous ethanol for 5 times to obtain final precipitate, drying the final precipitate with forced air drier at 50 deg.C for 24 hr, and grinding into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, adding the prepared epoxy resin in the S6 into a beaker, and stirring for 20min by using a magnetic stirrer; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution, and preheating the mixed solution for 20 minutes at the temperature of 80 ℃;
s8, preparing 20-80 parts by mass of k-DBN and 185 parts by mass of preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring for 60min by using a mechanical stirrer to obtain mixed liquor;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and mechanically stirring for 15 minutes at the temperature of 80 ℃ to obtain a mixed liquid;
s10, coating a mold with a release agent, placing the mold into a drying oven, preheating to 118 ℃, injecting the mixed solution obtained in the step S9 into the mold, placing the mold into a vacuum drying oven, keeping the temperature of the mold at 80 ℃, and performing vacuum degassing treatment for 1 hour until no obvious gas is separated out; then keeping the temperature at 100 ℃ for 4h, and then keeping the temperature at 150 ℃ for 10h for curing; and finally, cooling and demolding at room temperature to obtain the final sample.
The high-thermal-conductivity epoxy composite material obtained by the preparation method comprises 20-80 parts by mass of k-BN, 100 parts by mass of epoxy resin, 85 parts by mass of curing agent and 1 part by mass of accelerator.
The invention has the following beneficial effects:
1. according to the method, hexagonal boron nitride particles are modified for the second time, dopamine is firstly accessed, then a coupling agent is added, the coupling agent is reacted with the dopamine to be introduced onto the surface of BN, Si-O-C groups capable of being combined with epoxy resin are grafted onto the surface of the hexagonal boron nitride, and the interface combination capacity between the filler and the matrix is improved; BN is subjected to secondary modification by dopamine and a coupling agent and then is added into the epoxy composite material prepared by epoxy, so that the thermal stability and the mechanical property of the composite material are improved;
2. the method effectively improves the dispersibility of the hexagonal boron nitride in the epoxy resin, and obviously improves the heat-conducting property and the mechanical property of the epoxy resin composite material taking the secondary modified particles as the filler.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram comparing thermal conductivities of three composite materials;
FIG. 2 is a graph showing a comparison of tensile strengths of three composites;
FIG. 3 is a graph comparing elongation at break for three composites.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is exemplary in nature and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
A preparation method of a high-thermal-conductivity epoxy composite material comprises the following steps:
s1, adding 10 parts by mass of BN into a beaker, pouring ultrapure water into the beaker, and dispersing the ultrapure water for 30min at a high speed by using a high-speed dispersion machine; the BN particle size is 15 mu m, and the purity is 99.5%;
s2, adding 0.315 part by mass of Tris-HCl into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH to 8.5 by using 0.1mol/L NaOH solution, carrying out magnetic stirring reaction for 6 hours at the temperature of 25 ℃, and then carrying out centrifugal separation at the rotating speed of 3000r/min to obtain a precipitate;
s3, adding ultrapure water into the precipitate obtained by centrifuging the S2, washing for 5 times to obtain a final precipitate, drying the final precipitate for 24 hours at 50 ℃ by using a blast dryer, and finally grinding into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and stirring for 10min at 60 ℃ by using a magnetic stirrer to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and stirring for 3 hours at the temperature of 60 ℃ by using a magnetic stirrer to obtain a mixture;
s5, performing centrifugal separation on the mixture obtained in the step S4 at the rotating speed of 3000r/min to obtain a precipitate; adding absolute ethyl alcohol into the precipitate, fully stirring, washing for 5 times to obtain a final precipitate, drying the final precipitate for 24 hours at 50 ℃ by using a blast drier, and finally grinding into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, adding the prepared epoxy resin in the S6 into a beaker, and stirring for 20min by using a magnetic stirrer; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution, and preheating the mixed solution for 20 minutes at the temperature of 80 ℃; in the magnetic stirring process, the epoxy resin is kept at 60 ℃ by using an oil bath method;
s8, preparing 20 parts by mass of k-DBN and 185 parts by mass of the preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring for 60min by using a mechanical stirrer to obtain mixed liquor; keeping the oil bath environment at 60 ℃ in the stirring process of the mechanical stirrer;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and mechanically stirring for 15 minutes at the temperature of 80 ℃ to obtain a mixed liquid;
s10, coating a mold with a release agent, placing the mold into a drying oven, preheating to 118 ℃, injecting the mixed solution obtained in the step S9 into the mold, placing the mold into a vacuum drying oven, keeping the temperature of the mold at 80 ℃, and performing vacuum degassing treatment for 1 hour until no obvious gas is separated out; then keeping the temperature at 100 ℃ for 4h, and then keeping the temperature at 150 ℃ for 10h for curing; and finally, cooling and demolding at room temperature to obtain the final sample.
Example 2
A preparation method of a high-thermal-conductivity epoxy composite material comprises the following steps:
s1, adding 10 parts by mass of BN into a beaker, pouring ultrapure water into the beaker, and dispersing the ultrapure water for 30min at a high speed by using a high-speed dispersion machine; the BN particle size is 15 mu m, and the purity is 99.5%;
s2, adding 0.315 part by mass of Tris-HCl into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH to 8.5 by using 0.1mol/L NaOH solution, carrying out magnetic stirring reaction for 6 hours at the temperature of 25 ℃, and then carrying out centrifugal separation at the rotating speed of 3000r/min to obtain a precipitate;
s3, adding ultrapure water into the precipitate obtained by centrifuging the S2, washing for 5 times to obtain a final precipitate, drying the final precipitate for 24 hours at 50 ℃ by using a blast dryer, and finally grinding into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and stirring for 10min at 60 ℃ by using a magnetic stirrer to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and stirring for 3 hours at the temperature of 60 ℃ by using a magnetic stirrer to obtain a mixture;
s5, performing centrifugal separation on the mixture obtained in the step S4 at the rotating speed of 3000r/min to obtain a precipitate; adding absolute ethyl alcohol into the precipitate, fully stirring, washing for 5 times to obtain a final precipitate, drying the final precipitate for 24 hours at 50 ℃ by using a blast drier, and finally grinding into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, adding the prepared epoxy resin in the S6 into a beaker, and stirring for 20min by using a magnetic stirrer; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution, and preheating the mixed solution for 20 minutes at the temperature of 80 ℃; in the magnetic stirring process, the epoxy resin is kept at 60 ℃ by using an oil bath method;
s8, preparing 50 parts by mass of k-DBN and 185 parts by mass of preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring for 60min by using a mechanical stirrer to obtain mixed liquor; keeping the oil bath environment at 60 ℃ in the stirring process of the mechanical stirrer;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and mechanically stirring for 15 minutes at the temperature of 80 ℃ to obtain a mixed liquid;
s10, coating a mold with a release agent, placing the mold into a drying oven, preheating to 118 ℃, injecting the mixed solution obtained in the step S9 into the mold, placing the mold into a vacuum drying oven, keeping the temperature of the mold at 80 ℃, and performing vacuum degassing treatment for 1 hour until no obvious gas is separated out; then keeping the temperature at 100 ℃ for 4h, and then keeping the temperature at 150 ℃ for 10h for curing; and finally, cooling and demolding at room temperature to obtain the final sample.
Example 3
A preparation method of a high-thermal-conductivity epoxy composite material comprises the following steps:
s1, adding 10 parts by mass of BN into a beaker, pouring ultrapure water into the beaker, and dispersing the ultrapure water for 30min at a high speed by using a high-speed dispersion machine; the BN particle size is 15 mu m, and the purity is 99.5%;
s2, adding 0.315 part by mass of Tris-HCl into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH to 8.5 by using 0.1mol/L NaOH solution, carrying out magnetic stirring reaction for 6 hours at the temperature of 25 ℃, and then carrying out centrifugal separation at the rotating speed of 3000r/min to obtain a precipitate;
s3, adding ultrapure water into the precipitate obtained by centrifuging the S2, washing for 5 times to obtain a final precipitate, drying the final precipitate for 24 hours at 50 ℃ by using a blast dryer, and finally grinding into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and stirring for 10min at 60 ℃ by using a magnetic stirrer to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and stirring for 3 hours at the temperature of 60 ℃ by using a magnetic stirrer to obtain a mixture;
s5, performing centrifugal separation on the mixture obtained in the step S4 at the rotating speed of 3000r/min to obtain a precipitate; adding absolute ethyl alcohol into the precipitate, fully stirring, washing for 5 times to obtain a final precipitate, drying the final precipitate for 24 hours at 50 ℃ by using a blast drier, and finally grinding into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, adding the prepared epoxy resin in the S6 into a beaker, and stirring for 20min by using a magnetic stirrer; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution, and preheating the mixed solution for 20 minutes at the temperature of 80 ℃; in the magnetic stirring process, the epoxy resin is kept at 60 ℃ by using an oil bath method;
s8, preparing 80 parts by mass of k-DBN and 185 parts by mass of preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring for 60min by using a mechanical stirrer to obtain mixed liquor; keeping the oil bath environment at 60 ℃ in the stirring process of the mechanical stirrer;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and mechanically stirring for 15 minutes at the temperature of 80 ℃ to obtain a mixed liquid;
s10, coating a mold with a release agent, placing the mold into a drying oven, preheating to 118 ℃, injecting the mixed solution obtained in the step S9 into the mold, placing the mold into a vacuum drying oven, keeping the temperature of the mold at 80 ℃, and performing vacuum degassing treatment for 1 hour until no obvious gas is separated out; then keeping the temperature at 100 ℃ for 4h, and then keeping the temperature at 150 ℃ for 10h for curing; and finally, cooling and demolding at room temperature to obtain the final sample.
The high-thermal-conductivity epoxy composite material obtained by the preparation method comprises 20-80 parts by mass of k-BN, 100 parts by mass of epoxy resin, 85 parts by mass of curing agent and 1 part by mass of accelerator.
DBN is BN modified by a coupling agent dopamine, and k-DBN is BN secondarily modified by the coupling agent dopamine.
As shown in fig. 1, as the loading of BN increases, the thermal conductivity of the composite material increases, and at the same loading, the thermal conductivity of the modified composite material is higher than that of the unmodified composite material. At a low filling amount, the lifting rate of the modified composite material is not obvious, because the viscosity of a mixed system is low and the dispersion of BN is good when the content of BN is low, the improvement of the thermal conductivity of the composite material by modification is not particularly obvious, and when the filling amount of BN is 30 wt%, the thermal conductivity of the k-DBN/EP composite material is 0.892W/(m.k), is improved by 20.05 percent compared with the BN/EP composite material (0.743W/(m.k)) and is improved by 355 percent compared with pure epoxy (0.196W/(m.k)). The existence of the gaps in the composite material can improve the interface thermal resistance, and has great influence on the improvement of the thermal conductivity, and after the surface modification, the compatibility of BN and epoxy resin is increased, and the gaps are reduced, so that the thermal conductivity is obviously improved. Meanwhile, the k-DBN/EP composite material has higher thermal conductivity than the DBN/EP composite material, which shows that the k-DBN and the epoxy resin have better bonding property and lower interface thermal resistance, and are more beneficial to heat conduction.
As shown in fig. 2, as the content of BN filler increases, the tensile strength and elongation at break of the composite gradually decrease because BN has poor compatibility with epoxy resin, and the addition of micron-sized BN is equivalent to the introduction of defects into the matrix, which makes cracks more easily extend inside the resin, resulting in a decrease in the tensile strength and elongation at break of the composite. After the surface of BN is modified, the bonding force of BN and epoxy resin is increased, the tensile strength is improved, and the improvement of the tensile strength of the composite material prepared from the k-DBN filling resin is most obvious. However, the binding force between the modified filler and the resin is increased, so that the movement of the resin chain segment is difficult, and therefore, the elongation at break of the composite material is reduced after modification, but when the filler content is 30 wt%, the viscosity of the composite material is too high, the dispersibility of the filler is poor, and when the filler is not modified, the internal voids of the prepared composite material are large, so that the mechanical property is reduced, and the dispersibility of the modified filler is improved, so that the elongation at break shows a tendency of increasing.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (7)
1. The preparation method of the high-thermal-conductivity epoxy composite material is characterized by comprising the following steps of:
s1, adding 10 parts by mass of BN into a beaker, pouring ultrapure water into the beaker, and dispersing the ultrapure water at a high speed;
s2, adding 0.315 parts by mass of Tris-HCL into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH value to be alkaline, and performing centrifugal separation after full magnetic stirring reaction to obtain a precipitate;
s3, washing the precipitate obtained by centrifuging the S2 to obtain a final precipitate, drying the final precipitate, and grinding the dried final precipitate into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and fully stirring to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and fully stirring to obtain a mixture;
s5, centrifuging the mixture obtained in the S4 to obtain a precipitate; fully washing the precipitate with absolute ethyl alcohol to obtain a final precipitate, drying the final precipitate, and grinding the dried final precipitate into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, fully stirring the prepared epoxy resin in the S6; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution and preheating the mixed solution;
s8, preparing 20-80 parts by mass of k-DBN and 185 parts by mass of preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring to obtain mixed liquor;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and fully stirring to obtain a mixed liquid;
s10, injecting the mixed solution obtained in the step S9 into a mould, placing the mould in a vacuum drying oven for vacuum pumping and degassing until no obvious gas is separated out, and then curing; and finally, cooling and demolding at room temperature to obtain the final sample.
2. The method according to claim 1, wherein the BN in S1 has a particle size of 15 μm and a purity of 99.5%.
3. The method according to claim 1, wherein the pH of S2 is adjusted to 8.5 with 0.1mol/L NaOH solution.
4. The production method according to claim 1, wherein in S7, the epoxy resin is maintained at 60 ℃ by an oil bath method during magnetic stirring.
5. The production method according to claim 1, wherein in S8, an oil bath environment of 60 ℃ is maintained during the stirring with the mechanical stirrer.
6. The production method according to claim 1,
s1, adding 10 parts by mass of BN into a beaker, then pouring ultrapure water into the beaker, and dispersing the mixture at a high speed for 30min by using a high-speed dispersion machine;
s2, adding 0.315 part by mass of Tris-HCL into the BN mixed solution obtained in the S1, adding 1 part by mass of dopamine hydrochloride, adjusting the pH to 8.5, carrying out magnetic stirring reaction for 6 hours at the temperature of 25 ℃, and then carrying out centrifugal separation at the rotating speed of 3000r/min to obtain a precipitate;
s3, washing the precipitate obtained by centrifuging the S2 by using ultrapure water for 5 times to obtain a final precipitate, drying the final precipitate by using a blast dryer at 50 ℃ for 24 hours, and finally grinding the final precipitate into powder to obtain DBN;
s4, according to the mass ratio of DBN: weighing DBN and KH550 silane coupling agent at a ratio of 100: 5; adding absolute ethyl alcohol into a KH550 silane coupling agent, and stirring for 10min at 60 ℃ by using a magnetic stirrer to obtain a coupling agent absolute ethyl alcohol mixed solution; adding DBN into the anhydrous ethanol mixed solution of the coupling agent, and stirring for 3 hours at the temperature of 60 ℃ by using a magnetic stirrer to obtain a mixture;
s5, performing centrifugal separation on the mixture obtained in the step S4 at the rotating speed of 3000r/min to obtain a precipitate; washing the precipitate with anhydrous ethanol for 5 times to obtain final precipitate, drying the final precipitate with forced air drier at 50 deg.C for 24 hr, and grinding into powder to obtain k-DBN;
s6, preparing epoxy resin: curing agent: accelerator 100: 85: 1, curing agent and accelerator;
s7, adding the prepared epoxy resin in the S6 into a beaker, and stirring for 20min by using a magnetic stirrer; adding the curing agent prepared in the step S6 into the stirred epoxy resin to obtain a mixed solution, and preheating the mixed solution for 20 minutes at the temperature of 80 ℃;
s8, preparing 20-80 parts by mass of k-DBN and 185 parts by mass of preheated mixed liquor in S7, adding k-DBN particles into the preheated mixed liquor in S7, and stirring for 60min by using a mechanical stirrer to obtain mixed liquor;
s9, adding the accelerant prepared in the S6 into the mixed liquid obtained in the S8, and mechanically stirring for 15 minutes at the temperature of 80 ℃ to obtain a mixed liquid;
s10, coating a mold with a release agent, placing the mold into a drying oven, preheating to 118 ℃, injecting the mixed solution obtained in the step S9 into the mold, placing the mold into a vacuum drying oven, keeping the temperature of the mold at 80 ℃, and performing vacuum degassing treatment for 1 hour until no obvious gas is separated out; then keeping the temperature at 100 ℃ for 4h, and then keeping the temperature at 150 ℃ for 10h for curing; and finally, cooling and demolding at room temperature to obtain the final sample.
7. The high-thermal-conductivity epoxy composite material obtained by the preparation method of any one of claims 1 to 6 is characterized by comprising 20 to 80 parts by mass of k-BN, 100 parts by mass of epoxy resin, 85 parts by mass of curing agent and 1 part by mass of accelerator.
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| CN111607839A (en) * | 2020-06-23 | 2020-09-01 | 南通强生石墨烯科技有限公司 | Method for preparing modified white graphene polyester composite fiber and fiber prepared by method |
| CN113354919A (en) * | 2021-06-13 | 2021-09-07 | 西北工业大学 | Soft metal-friendly resin-based friction material and preparation method thereof |
| CN113698736A (en) * | 2021-10-09 | 2021-11-26 | 深圳市鑫奕龙达电子有限公司 | Halogen-free flame-retardant heat-conducting wire insulating layer and preparation method thereof |
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| CN116622283A (en) * | 2023-07-24 | 2023-08-22 | 广东优冠生物科技有限公司 | Fireproof flame-retardant shell substrate coating and preparation method thereof |
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| CN111560660A (en) * | 2020-06-23 | 2020-08-21 | 南通强生石墨烯科技有限公司 | Method for preparing white graphene regenerated cellulose composite fiber and fiber prepared by method |
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| CN113354919A (en) * | 2021-06-13 | 2021-09-07 | 西北工业大学 | Soft metal-friendly resin-based friction material and preparation method thereof |
| CN113698736A (en) * | 2021-10-09 | 2021-11-26 | 深圳市鑫奕龙达电子有限公司 | Halogen-free flame-retardant heat-conducting wire insulating layer and preparation method thereof |
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| CN114025472A (en) * | 2021-11-12 | 2022-02-08 | 百强电子（深圳）有限公司 | High-heat-dissipation metal-based printed circuit board and manufacturing method thereof |
| CN114213882A (en) * | 2021-12-31 | 2022-03-22 | 东莞市安宿泰电子科技有限公司 | High-temperature-resistant heat-dissipation coating and preparation method thereof |
| CN115819845A (en) * | 2022-12-23 | 2023-03-21 | 国网浙江省电力有限公司金华供电公司 | Filler modification method, modified filler and filled heat-conducting epoxy resin |
| CN116622283A (en) * | 2023-07-24 | 2023-08-22 | 广东优冠生物科技有限公司 | Fireproof flame-retardant shell substrate coating and preparation method thereof |
| CN116622283B (en) * | 2023-07-24 | 2023-11-07 | 广东优冠生物科技有限公司 | Fireproof flame-retardant shell substrate coating and preparation method thereof |
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