CN112759797A - Heat-conducting insulating filler, heat-conducting insulating material and preparation method thereof - Google Patents

Heat-conducting insulating filler, heat-conducting insulating material and preparation method thereof Download PDF

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CN112759797A
CN112759797A CN202011597656.8A CN202011597656A CN112759797A CN 112759797 A CN112759797 A CN 112759797A CN 202011597656 A CN202011597656 A CN 202011597656A CN 112759797 A CN112759797 A CN 112759797A
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carbon fiber
polyurea resin
heat
conducting
conducting insulating
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CN112759797B (en
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毕曙光
冉建华
于洁
谢佑南
曹勇
孙爱祥
杨涛
黄行智
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Wuhan Kenda Kexun Technology Co ltd
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Abstract

The invention provides a heat-conducting insulating filler, a heat-conducting insulating material and a preparation method thereof. Above-mentioned heat conduction insulating filler adopts polyurea resin cladding carbon fiber as heat conduction insulating material, and the carbon fiber after the polyurea resin cladding has not only strengthened its and insulator interface bonding material between the compatibility, has improved its and insulator interface cohesion, can effectively avoid it to drop under exogenic action such as friction and become invalid, can also improve its insulating nature through polyurea resin cladding carbon fiber moreover, has overcome the electrically conductive drawback of traditional high heat conduction material, improves its application property as insulating heat conduction filler.

Description

Heat-conducting insulating filler, heat-conducting insulating material and preparation method thereof
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a heat conduction insulating filler, a heat conduction insulating material and a preparation method thereof.
Background
Conventional hard devices and electronic devices have wide application in fields such as wearable equipment, energy storage, implantation medical treatment and the like. Similar to the high thermal conductivity composite nano material, the preparation of the flexible electronic device is also mostly obtained by compounding the conductive material with the flexible polymer matrix. However, during the repeated deformation of the device, a large amount of heat may be accumulated inside the electronic device due to a large contact resistance between the conductive materials, a poor contact between the conductive materials and the polymer substrate, and the like. If not dissipated from the device in a timely manner, this heat will inevitably affect the performance and lifetime of the device and may even compromise the overall system. That is, for electronic devices, stable thermal properties are also important in addition to excellent mechanical and electrical properties.
Although the current heat-conducting insulating composite material has certain flexibility and is applied to the heat management of conventional hard electronic devices such as LEDs, the application research of the heat-conducting insulating composite material in the field of electronic devices is very little involved. The method is applied to the field of electronic devices, and the mechanism of the method is deeply researched, which is particularly important for the development of new generation electronic devices.
Disclosure of Invention
Based on this, it is necessary to provide a heat conducting insulating filler, a heat conducting insulating material and a preparation method thereof for solving the technical problem that a large amount of heat is accumulated inside a flexible electronic device due to poor contact between a conductive material and a polymer matrix and the like, and the application requirement of the flexible electronic device cannot be met by the conventional heat conducting material.
The invention provides a heat-conducting insulating filler which is a polyurea resin coated carbon fiber material.
In one embodiment, in the polyurea resin coated carbon fiber material, the weight ratio of the carbon fiber to the polyurea resin is 100: (1-50).
The invention also provides a heat-conducting insulating material which comprises an insulator and the heat-conducting insulating filler.
In one embodiment, the insulation is flexible insulation.
In one embodiment, the thermally conductive and insulating material is prepared by a mechanical extrusion orientation technique.
The invention also provides a preparation method of the heat-conducting insulating filler, which comprises the following steps:
a carbon fiber dispersion liquid preparation step, in which carbon fibers are dispersed in an organic solvent to prepare a carbon fiber dispersion liquid;
and a step of preparing the polyurea resin coated carbon fiber material, namely mixing a coating resin monomer with the carbon fiber dispersion liquid to perform polymerization coating reaction, and drying the obtained fixed material to constant weight to prepare the polyurea resin coated carbon fiber material.
In one embodiment, in the step of preparing the carbon fiber dispersion, the step of dispersing the carbon fibers in the organic solvent is to mix the carbon fibers with the organic solvent, the dispersant and water, stir until the mixture is uniformly dispersed, and maintain the mixture at a temperature of 40 ℃ to 60 ℃ for 0.5h to 1.5 h.
In one embodiment, the coating resin monomer is toluene-2, 4-diisocyanate.
In one embodiment, the time of the polymerization coating reaction is 1-2 h, and the temperature of the polymerization coating reaction is 60-80 ℃.
In one embodiment, the drying temperature is 60 ℃ to 80 ℃.
Above-mentioned heat conduction insulating filler adopts polyurea resin cladding carbon fiber as heat conduction insulating material, and the carbon fiber after the polyurea resin cladding has not only strengthened its and insulator interface bonding material between the compatibility, has improved its and insulator interface cohesion, can effectively avoid it to drop under exogenic action such as friction and become invalid, can also improve its insulating nature through polyurea resin cladding carbon fiber moreover, has overcome the electrically conductive drawback of traditional high heat conduction material, improves its application property as insulating heat conduction filler.
According to the heat-conducting insulating material, the polyurea resin coated carbon fiber material is used as the heat-conducting filler, the interface bonding force between the insulator and the heat-conducting filler is effectively enhanced, the heat-conducting filler can be effectively prevented from falling off and losing efficacy under the action of external forces such as friction, and the heat-conducting insulating material is more suitable for being applied to flexible electronic devices with heat-conducting insulating requirements; furthermore, the heat-conducting insulating material utilizes a mechanical extrusion orientation technology to enable the prepared heat-conducting insulating material to be orderly arranged in an insulator, so that the prepared heat-conducting insulating material obtains high heat conductivity and high insulativity and meets the requirements of practical application.
According to the preparation method of the heat-conducting insulating filler, the polyurea resin is coated on the surface of the carbon fiber through an in-situ polymerization method to form the insulating layer, the coating structure formed through in-situ polymerization can enhance the interface compatibility of the polyurea resin coated carbon fiber and an insulator, and further enhance the binding force of the polyurea resin coated carbon fiber and the insulator, and is favorable for the ordered arrangement of the heat-conducting insulating filler in the insulator, so that the heat-conducting insulating material prepared from the polyurea resin coated carbon fiber has high heat conductivity and high insulating property, the defect of electric conduction of the traditional high heat-conducting material is overcome, and the requirements of practical application are better met.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention. In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is an infrared spectrum of a polyurea resin-coated carbon fiber material and CF prepared in examples 1 to 3 of the present invention;
FIG. 2 is an X-ray diffraction chart of the polyurea resin coated carbon fiber material and CF prepared in examples 1 to 3 of the present invention;
FIG. 3 is a thermogravimetric analysis chart of the polyurea resin coated carbon fiber material and CF prepared in examples 1 to 3 of the present invention;
fig. 4 is a scanning electron microscope image of different multiples of the thermally conductive and insulating material prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The reaction reagents used in the present invention are commercially available and are chemically pure or more.
The invention provides a heat-conducting insulating filler in a first large aspect, and the heat-conducting insulating filler is a polyurea resin coated carbon fiber material.
Above-mentioned heat conduction insulating filler adopts polyurea resin cladding carbon fiber as heat conduction insulating material, and the carbon fiber after the polyurea resin cladding has not only strengthened its and insulator interface bonding material between the compatibility, has improved its and insulator interface cohesion, can effectively avoid it to drop under exogenic action such as friction and become invalid, can also improve its insulating nature through polyurea resin cladding carbon fiber moreover, has overcome the electrically conductive drawback of traditional high heat conduction material, improves its application property as insulating heat conduction filler.
As an optional embodiment, in the polyurea resin coated carbon fiber material, the weight ratio of the carbon fiber to the polyurea resin is 100: (1-50); preferably, the weight ratio of the carbon fibers to the polyurea resin is 100: (5-15); more preferably, the weight ratio of carbon fibers to polyurea resin is 100: 10. according to the invention, researches show that the thermal conductivity coefficient of the polyurea resin coated carbon fiber material is positively correlated with the carbon fiber content of the polyurea resin coated carbon fiber material, and the volume resistivity is negatively correlated with the carbon fiber content of the polyurea resin coated carbon fiber material, namely, the higher the carbon fiber content of the polyurea resin coated carbon fiber material is, the higher the thermal conductivity coefficient is, the better the thermal conductivity is, and the smaller the volume resistivity is, the higher the electrical conductivity is, and the lower the insulation. In specific application, the weight ratio of the carbon fiber to the polyurea resin can be adjusted according to the application scene of the heat-conducting insulating material. The heat-conducting insulating material is mainly applied to flexible electronic devices, and researches show that the weight ratio of carbon fibers to polyurea resin is 100: (5-15), in particular, the weight ratio of the carbon fibers to the polyurea resin is 100: when 10, the heat-conducting property and the insulating property of the material can better meet the application requirements.
Wherein, the Carbon Fiber (CF) is a Fiber material of high-strength and high-modulus Fiber with the diameter of 5-10 μm and the Carbon content of more than 90 percent. In the invention, the Carbon Fiber is preferably short Carbon Fiber (Chopped Carbon Fiber), which is prepared by processing Carbon Fiber with high strength and high heat conductivity into a beam by selecting a bundling agent according to requirements and then cutting the beam according to a specified length, and has good heat conductivity.
The Polyurea resin (Polyurea) and the insulator have good compatibility, and the Polyurea resin coated carbon fiber material (CF @ Polyurea) and the insulator can be firmly bonded together, so that the heat-conducting insulating material prepared based on the Polyurea resin coated carbon fiber material has high heat conductivity and insulativity, and the defect of high heat-conducting gasket electric conduction is overcome.
The second aspect of the present invention provides a heat conducting insulating material, which includes an insulator and the above heat conducting insulating filler. In the heat-conducting insulating material, the heat-conducting insulating filler and the insulator can be independently used for preparation, and the heat-conducting insulating filler, other heat-conducting fillers and the insulator can also be used for preparation.
As an alternative, the insulation is a flexible insulation, which may be, for example, silicone.
As an alternative embodiment, the thermally conductive and insulating material is prepared by a mechanical extrusion orientation technique.
In a specific application, the heat-conducting and insulating material can be prepared into different structures according to an application scene, such as a gasket structure.
According to the heat-conducting insulating material, the polyurea resin coated carbon fiber material is used as the heat-conducting filler, the interface bonding force between the insulator and the heat-conducting filler is effectively enhanced, the heat-conducting filler can be effectively prevented from falling off and losing efficacy under the action of external forces such as friction, and the heat-conducting insulating material is more suitable for being applied to flexible electronic devices with heat-conducting insulating requirements; furthermore, the heat-conducting insulating material utilizes a mechanical extrusion orientation technology to enable the prepared heat-conducting insulating material to be orderly arranged in an insulator, so that the prepared heat-conducting insulating material obtains high heat conductivity and high insulativity and meets the requirements of practical application.
The third aspect of the present invention provides a preparation method of the above thermal conductive insulating filler, including the following steps:
a carbon fiber dispersion liquid preparation step, in which carbon fibers are dispersed in an organic solvent to prepare a carbon fiber dispersion liquid;
and a step of preparing the polyurea resin coated carbon fiber material, namely mixing a coating resin monomer with a carbon fiber dispersion liquid to perform polymerization coating reaction, and drying the obtained product to constant weight to prepare the polyurea resin coated carbon fiber material.
According to the preparation method of the heat-conducting insulating filler, the polyurea resin is coated on the surface of the carbon fiber through an in-situ polymerization method to form the insulating layer, the coating structure formed through in-situ polymerization can enhance the interface compatibility of the polyurea resin coated carbon fiber and an insulator, and further enhance the binding force of the polyurea resin coated carbon fiber and the insulator, and is favorable for the ordered arrangement of the heat-conducting insulating filler in the insulator, so that the heat-conducting insulating material prepared from the polyurea resin coated carbon fiber has high heat conductivity and high insulating property, the defect of electric conduction of the traditional high heat-conducting material is overcome, and the requirements of practical application are better met.
As an optional embodiment, in the step of preparing the carbon fiber dispersion liquid, the step of dispersing the carbon fibers into the organic solvent is to mix the carbon fibers with the organic solvent, the dispersant and water, stir until the mixture is uniformly dispersed, and maintain the mixture for 0.5 to 1.5 hours at the temperature of between 40 and 60 ℃; preferably, after stirring to disperse uniformly, the mixture is maintained at a temperature of 40 ℃ to 60 ℃ for 1.0 h.
Wherein the organic solvent may be selected from petroleum ether. The petroleum ether can well disperse the carbon fiber and has no adverse effect on the polymerization coating reaction.
In the preparation step of the polyurea resin coated carbon fiber material, a small amount of water is added into a carbon fiber dispersion liquid, the water can infiltrate the surface of the carbon fiber, then a coating resin monomer is added, and the water and the coating resin monomer react to generate polyurea resin coated on the surface of the carbon fiber.
Further alternatively, the volume of the dispersant used for dispersing 10g to 20g of the carbon fibers is 1mL to 3mL, the volume of the organic solvent is 100mL to 200mL, and the volume of the water is 2mL to 5 mL. Among them, the dispersant may be selected from those which do not affect the properties of the raw material used in the present invention, and preferably a nonionic surfactant such as sorbitan fatty acid ester (Span-80).
In the step of preparing the polyurea resin-coated carbon fiber material, the coating resin monomer is preferably Toluene-2,4-diisocyanate (TDI). After the coating resin monomer toluene-2,4-diisocyanate is added into the carbon fiber dispersion liquid, water and the coating resin monomer toluene-2,4-diisocyanate are subjected to polymerization reaction on the surface of the carbon fiber to generate polyurea resin.
As an alternative embodiment, the time of the polymerization coating reaction is 1-2 h, and the temperature of the polymerization coating reaction is 60-80 ℃.
As an optional implementation mode, the drying temperature is 60-80 ℃.
Example 1
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
And adding 0.5g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting at the temperature of 60 ℃ for 1h, and drying the obtained solid at the temperature of 60-80 ℃ to constant weight to obtain the polyurea resin coated carbon fiber material. From the section of example 1 of the infrared spectrum of FIG. 1, it can be shown that 3398cm-1Is a vibration absorption peak of O-H, N-H bond; 2927 and 2850cm-1C-H shock absorption peaks for methyl and methylene; 2275cm-1Is the N-C shock absorption peak; 1600-1500cm-1The absorption peaks of the expansion vibration of the amide C ═ O and the deformation vibration of C-N and N-H are shown; 1218cm-1Polyurea resins have been successfully coated on the CF surface for C-H bond bending vibration absorption peaks. From the example 1 portion of the X-ray diffraction spectrum of FIG. 2, it can be shown that the peak of the crystal peak of CF is weakened after coating the polyurea resin. From the example 1 portion of the thermogravimetric plot of fig. 3, it can be shown that the coating mass percentage of polyurea resin in the polyurea resin coated carbon fiber material is 7.6%, i.e., 7.6g of polyurea-containing resin per 100g of polyurea resin coated carbon fiber material.
The prepared polyurea resin coated carbon fiber material is mixed with the insulator silica gel, so that the mass percent of the carbon fiber in the mixture is 4.8 percent, namely the mass percent of the polyurea resin coated carbon fiber is 5.2 percent. And preparing the heat-conducting insulating material by using a mechanical extrusion orientation technology. Fig. 4 is a scanning electron microscope image of different multiples of the thermally conductive and insulating material obtained in example 1 of the present invention. As can be seen from the figure, the carbon fibers are uniformly and tightly bonded to the insulator after being coated with the polyurea resin.
Example 2
Dispersing 10g of CF in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the CF is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form uniform CF dispersion.
Adding 1.0g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. From the section of example 2 of the infrared spectrum of FIG. 1, it can be shown that 3398cm-1Is a vibration absorption peak of O-H, N-H bond; 2927 and 2850cm-1C-H shock absorption peaks for methyl and methylene; 2275cm-1Is the N-C shock absorption peak; 1600-1500cm-1The absorption peaks of the expansion vibration of the amide C ═ O and the deformation vibration of C-N and N-H are shown; 1218cm-1For C-H bond bending vibrationsDynamic absorption peaks, polyurea resins have been successfully coated on CF surfaces. From the example 2 portion of the X-ray diffraction spectrum of FIG. 2, it can be shown that the peak of the crystal peak of CF is weakened after coating the polyurea resin. From the example 2 portion of the thermogravimetric plot of fig. 3, it can be shown that the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material is 11.1%, i.e., 11.1g of the polyurea-containing resin per 100g of the polyurea resin coated carbon fiber material.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percent of carbon fibers in the mixture is 4.8 percent, namely the mass percent of the polyurea resin coated carbon fibers is 5.4 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 3
Dispersing 10g of CF in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the CF is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form uniform CF dispersion.
Adding 1.5g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. From the section of example 3 of the infrared spectrum of FIG. 1, it can be shown that 3398cm-1Is a vibration absorption peak of O-H, N-H bond; 2927 and 2850cm-1C-H shock absorption peaks for methyl and methylene; 2275cm-1Is the N-C shock absorption peak; 1600-1500cm-1The absorption peaks of the expansion vibration of the amide C ═ O and the deformation vibration of C-N and N-H are shown; 1218cm-1Polyurea resins have been successfully coated on the CF surface for C-H bond bending vibration absorption peaks. From the example 3 portion of the X-ray diffraction spectrum of FIG. 2, it can be shown that the peak of the crystal peak of CF is weakened after coating the polyurea resin. From the example 3 portion of the thermogravimetric plot of fig. 3, it can be shown that the coating mass percentage of polyurea resin in the polyurea resin coated carbon fiber material is 15.3%, i.e. 15.3g of polyurea-containing resin per 100g of polyurea resin coated carbon fiber material.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percent of carbon fibers in the mixture is 4.8 percent, namely the mass percent of the polyurea resin coated carbon fibers is 5.7 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Comparative example 1
The uncoated carbon fiber and the insulator silica gel are mixed according to the weight ratio, so that the mass percent of the carbon fiber in the mixture is 4.8%, and the heat-conducting insulating material is prepared by utilizing a mechanical extrusion orientation technology.
Further, the polyurea resin coated carbon fiber materials prepared in examples 1 to 3 and the powder resistance value of the carbon fiber were tested using a conventional apparatus in the art, and the thermal conductivity, volume resistivity and breakdown voltage resistance tests of the thermal conductive insulation materials prepared in examples 1 to 3 and comparative example 1 were tested, and the test results are shown in tables 1 and 2.
TABLE 1 test results of resistance values of polyurea resin-coated carbon fiber materials prepared in examples 1 to 3, carbon fibers
Figure BDA0002867026020000081
Table 2 heat conductive and insulating property test of heat conductive and insulating materials prepared in examples 1 to 3 and comparative example 1
Figure BDA0002867026020000091
Example 4
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
And adding 0.1g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting at the temperature of 60 ℃ for 1h, and drying the obtained solid at the temperature of 60-80 ℃ to constant weight to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 1.21%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 5
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
Adding 2.0g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 20.2%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 6
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
Adding 2.5g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 25.4%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 7
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
Adding 3.0g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 30.8%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 8
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
Adding 3.5g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 35.7%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 9
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
Adding 4.0g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 41.1%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
Example 10
Dispersing 10g of short Carbon Fiber (CF) in 100mL of petroleum ether, simultaneously dripping 1mL of Span-80, magnetically stirring until the mixture is uniformly dispersed, dripping 2mL of deionized water, and heating the obtained dispersion solution to 60 ℃ for 1.0h to form a uniform CF dispersion liquid.
Adding 4.5g of toluene-2,4-diisocyanate into the CF dispersion liquid, mixing, reacting for 1h at the temperature of 60 ℃, and drying the obtained solid to constant weight at the temperature of 60-80 ℃ to obtain the polyurea resin coated carbon fiber material. Infrared spectrum detection proves that the polyurea resin is successfully coated on the surface of the CF; the X-ray diffraction spectrum confirmed that the peak of the crystalline peak of CF was reduced after coating the polyurea resin relative to the uncoated CF; as can be seen from the thermal weight loss test curve, the coating mass percentage of the polyurea resin in the polyurea resin coated carbon fiber material prepared in example 4 is 46.3%.
Mixing the prepared polyurea resin coated carbon fiber material with an insulator silica gel to ensure that the mass percentages of the carbon fibers in the mixture are respectively 4.8 percent and 10 percent, and preparing the heat-conducting insulating material by utilizing a mechanical extrusion orientation technology.
The polyurea resin coated carbon fiber materials prepared in examples 4 to 10 and the powder resistance value of the carbon fiber were tested by using a conventional instrument in the art, and the thermal conductivity, volume resistivity and breakdown voltage resistance tests of the thermal conductive insulation materials prepared in examples 4 to 10 were tested, and the test results are shown in tables 3 and 4.
TABLE 3 test results of resistance values of polyurea resin-coated carbon fiber materials prepared in examples 4 to 10
Figure BDA0002867026020000121
Table 4 test of heat conductive and insulating properties of heat conductive and insulating materials prepared in examples 4 to 10
Figure BDA0002867026020000131
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The heat-conducting insulating filler is characterized in that the heat-conducting insulating filler is a polyurea resin coated carbon fiber material.
2. The thermally conductive insulating filler according to claim 1, wherein the polyurea resin coating carbon fiber material has a weight ratio of carbon fiber to polyurea resin of 100: (1-50).
3. A thermally conductive and insulating material comprising an insulator and the thermally conductive and insulating filler of claim 1 or 2.
4. The thermally conductive insulation of claim 3 wherein said insulation is flexible insulation.
5. The thermally conductive insulation material according to claim 3 or 4, wherein the thermally conductive insulation material is prepared by a mechanical extrusion orientation technique.
6. A method for preparing a thermally conductive insulating filler according to claim 1 or 2, characterized in that the method comprises the steps of:
a carbon fiber dispersion liquid preparation step, in which carbon fibers are dispersed in an organic solvent to prepare a carbon fiber dispersion liquid;
and a step of preparing the polyurea resin coated carbon fiber material, namely mixing a coating resin monomer with the carbon fiber dispersion liquid to perform polymerization coating reaction, and drying the obtained fixed material to constant weight to prepare the polyurea resin coated carbon fiber material.
7. The method of claim 6, wherein in the step of preparing the carbon fiber dispersion, the step of dispersing the carbon fibers in the organic solvent is to mix the carbon fibers with the organic solvent, the dispersant and water, stir the mixture until the mixture is uniformly dispersed, and maintain the mixture at a temperature of 40 ℃ to 60 ℃ for 0.5h to 1.5 h.
8. The method of claim 6, wherein the coating resin monomer is toluene-2, 4-diisocyanate.
9. The method for preparing the heat-conducting insulating filler according to claim 8, wherein the polymerization coating reaction time is 1-2 h, and the temperature of the polymerization coating reaction is 60-80 ℃.
10. The method of preparing a thermally conductive insulating filler according to any one of claims 6 to 9, wherein the drying temperature is 60 ℃ to 80 ℃.
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CN109486204A (en) * 2018-11-08 2019-03-19 南方科技大学 A kind of heat conductive insulating composite material and preparation method
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WO1994026815A1 (en) * 1993-05-07 1994-11-24 Metalleido S.R.L. Composite material comprising a treated reinforcing filler and a polymer matrix formed by polycondensation with aldehyde, and relative production method
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