CN115260627A - Boron nitride mixed modified polyethylene heat-conducting composite material and preparation method thereof - Google Patents
Boron nitride mixed modified polyethylene heat-conducting composite material and preparation method thereof Download PDFInfo
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- CN115260627A CN115260627A CN202210778577.XA CN202210778577A CN115260627A CN 115260627 A CN115260627 A CN 115260627A CN 202210778577 A CN202210778577 A CN 202210778577A CN 115260627 A CN115260627 A CN 115260627A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a boron nitride mixed modified polyethylene heat-conducting composite material which comprises the following components in parts by weight: 100 parts of polyethylene resin, 5-20 parts of boron nitride mixed filling particles, 0.05-0.10 part of composite antioxidant and 0.2-0.5 part of dispersant, wherein the boron nitride mixed filling particles are a mixture of one-dimensional boron nitride nanotubes and liquid-phase-stripped boron nitride two-dimensional nanosheets. The invention also discloses a preparation method of the boron nitride mixed modified polyethylene heat-conducting composite material, which comprises the steps of stirring and mixing the raw materials, adding the mixture into a double-roller open mill, and mixing, pressing and molding the mixture. The boron nitride mixed modified polyethylene heat-conducting composite material has good heat conductivity and excellent electrical insulation performance, and meets the requirements of industries such as electronics and electricity, high-temperature lubrication and the like on high-performance composite materials.
Description
Technical Field
The invention relates to a heat-conducting composite material and a preparation method thereof, in particular to a boron nitride mixed modified polyethylene heat-conducting composite material.
Background
The performance of electronic equipment is constantly improved, can release a large amount of heats in the use, and miniaturized equipment inside temperature constantly rises, may cause irreversible influence to equipment part, makes equipment life-span reduce, and the function is inefficacy. Most of the traditional heat conducting materials are metals and their compounds (such as Ag, au, cu, fe, etc.) and some non-metallic materials (such as graphite, siC, etc.). Metals, as good conductors of thermal energy, have the disadvantages of being heavy and susceptible to corrosion by chemical substances, and in particular, the metal materials have poor electrical insulation properties, which often limits their application in the industrial field. However, non-metallic materials such as graphite have high thermal conductivity, but have mechanical properties that are not satisfactory, so that they cannot be applied to most industrial scenes.
For high molecular polymers, heat conducting fillers are generally adopted for filling to achieve a certain heat conducting effect, but the high filling amount is required for forming a heat conducting network so as to achieve the improvement of the heat conducting effect. However, the high filling amount of the heat conductive filler affects both the mechanical properties and the electrical insulation properties of the material.
Disclosure of Invention
In view of the defects of the prior art, a task of the present invention is to provide a boron nitride mixed modified polyethylene heat-conducting composite material, which solves the problems that the heat-conducting property of the polyethylene material is poor, and the heat-conducting property is improved by the heat-conducting material with higher filling amount, and maintains good heat-conducting property and excellent electrical insulation property under the condition of less filler material. The invention also provides a preparation method of the boron nitride mixed modified polyethylene heat-conducting composite material.
The technical scheme of the invention is as follows: a boron nitride mixed modified polyethylene heat-conducting composite material comprises the following components in parts by weight: 100 parts of polyethylene resin, 5-20 parts of boron nitride mixed filler particles, 0.05-0.10 part of composite antioxidant and 0.2-0.5 part of dispersant, wherein the boron nitride mixed filler particles are a mixture of one-dimensional boron nitride nanotubes and liquid-phase-stripped boron nitride two-dimensional nanosheets.
Further, the mixing weight ratio of the one-dimensional boron nitride nanotube to the liquid-phase stripped boron nitride two-dimensional nanosheet is 1: 2-9.
Further, the one-dimensional boron nitride nanotube is modified by a silane coupling agent KH-550 or KH-570.
Further, the liquid-phase-stripped boron nitride two-dimensional nanosheet is obtained by liquid-phase stripping of h-BN with the particle size of 5-15 nm.
Further, the dispersant is polyvinylpyrrolidone.
Further, the compound antioxidant is formed by mixing an antioxidant 1010 and an antioxidant 168.
100 parts of polyethylene resin, 5-20 parts of boron nitride mixed filler particles, 0.05-0.10 part of composite antioxidant and 0.2-0.5 part of dispersant are poured into a high-speed mixer for mixing, then the mixture is added into a double-roll open mill for further mixing, and finally the mixture is pressed and molded to obtain the boron nitride mixed modified polyethylene heat-conducting composite material, wherein the boron nitride mixed filler particles are a mixture of one-dimensional boron nitride nanotubes and liquid-phase stripped boron nitride two-dimensional nanosheets.
Further, the mixing weight ratio of the one-dimensional boron nitride nanotube to the liquid-phase stripped boron nitride two-dimensional nanosheet is 1: 2-9.
Further, the one-dimensional boron nitride nanotube is modified by the following steps: adding the boron nitride nanotube into an absolute ethyl alcohol solution of a silane coupling agent, stirring and centrifuging, washing with absolute ethyl alcohol, and finally carrying out vacuum drying, wherein the silane coupling agent is KH-550 or KH-570, and the using amount of the silane coupling agent is 0.2-0.5% of the weight of the boron nitride nanotube.
Further, the liquid phase exfoliated boron nitride two-dimensional nanosheet is prepared by the following steps: and (2) adding metal sodium after h-BN drying treatment, adding nitrogen for protection and sealing, keeping the temperature of 115-125 ℃ for more than 35h under a stirring state in an anhydrous and oxygen-free environment, naturally cooling, then sequentially dropwise adding n-hexane and dimethylformamide, washing with distilled water for multiple times, and carrying out suction filtration and sedimentation to obtain the boron nitride two-dimensional nanosheet.
The technical scheme provided by the invention has the advantages that:
1) According to the invention, by adding the boron nitride heat-conducting fillers with different dimensions, a hybrid heat-conducting network can be formed, the filling density of the boron nitride nanoparticles can be optimized, a synergistic effect is formed, the using amount of the fillers is reduced, and the heat-conducting property of the matrix resin is effectively improved. Meanwhile, the boron nitride has good high-temperature insulating property, and the intrinsic advantages of the composite material matrix, such as good electrical insulating property, good processing property and the like, can be maintained by adding the mixed heat-conducting filler.
2) According to the invention, the surface modification treatment is carried out on the one-dimensional boron nitride nanotube, so that the crosslinking between the one-dimensional boron nitride nanotube and a matrix material can be improved, and on one hand, a heat conduction network chain can be formed more effectively in the system; on the other hand, the irregular surface can weaken Van der Waals force to the maximum extent, avoid the agglomeration of nano materials and influence the dispersibility; meanwhile, the polarity of the B-N bond enables the boron nitride nanotube and the matrix material to have strong interface interaction, thereby enhancing the mechanical property of the composite material.
3) The invention uses the nonionic dispersant polyvinylpyrrolidone, which is adsorbed on the gap wall of the heat-conducting filler by Van der Waals force, and realizes the dispersion effect on solid particles by virtue of the steric hindrance effect, thereby effectively improving the heat conductivity of the material.
4) The invention adopts double-roller open milling and tabletting molding to prepare the heat-conducting composite material, and realizes the orientation of the two-dimensional filler boron nitride nanosheet under the action of external force when the matrix resin and the heat-conducting filler are mixed, thereby further improving the filling effect of the filler and achieving the purpose of effectively improving the heat-conducting property of the matrix resin.
5) The invention relates to a boron nitride mixed filling modified polyethylene heat-conducting composite material with different dimensions. The filling amount of the heat-conducting filler is low, the heat-conducting efficiency is high, and meanwhile, the insulating property of the composite material is good.
Detailed Description
The present invention is further described in the following examples, which are intended to be illustrative only and not to be limiting as to the scope of the invention, which is to be given the full breadth of the appended claims and any and all modifications within the scope of the following claims.
Example 1
The boron nitride mixed modified polyethylene heat-conducting composite material comprises the following components in parts by weight: 100kg of low-density polyethylene resin, 0.5kg of one-dimensional boron nitride nanotube, 4.5kg of liquid-phase peeled boron nitride two-dimensional nanosheet, 0.02kg of antioxidant 1010, 0.04kg of antioxidant 168 and 0.2kg of polyvinylpyrrolidone.
Example 2
The boron nitride mixed modified polyethylene heat-conducting composite material comprises the following components in parts by weight: 100kg of low-density polyethylene resin, 2kg of one-dimensional boron nitride nanotubes, 4.5kg of liquid-phase stripped boron nitride two-dimensional nanosheets, 0.02kg of antioxidant 1010, 0.04kg of antioxidant 168 and 0.2kg of polyvinylpyrrolidone.
Example 3
The boron nitride mixed modified polyethylene heat-conducting composite material comprises the following components in parts by weight: 100kg of low-density polyethylene resin, 2kg of one-dimensional boron nitride nanotubes, 18kg of liquid-phase-stripped boron nitride two-dimensional nanosheets, 0.02kg of antioxidant 1010, 0.04kg of antioxidant 168 and 0.2kg of polyvinylpyrrolidone.
Example 4
The boron nitride mixed modified polyethylene heat-conducting composite material comprises the following components in parts by weight: 100kg of low-density polyethylene resin, 2kg of one-dimensional boron nitride nanotubes, 18kg of liquid-phase-stripped boron nitride two-dimensional nanosheets, 0.02kg of antioxidant 1010, 0.05kg of antioxidant 168 and 0.3kg of polyvinylpyrrolidone.
Example 5
The boron nitride mixed modified polyethylene heat-conducting composite material comprises the following components in parts by weight: 100kg of low-density polyethylene resin, 2kg of one-dimensional boron nitride nanotubes, 18kg of liquid-phase stripped boron nitride two-dimensional nanosheets, 0.03kg of antioxidant 1010, 0.06kg of antioxidant 168 and 0.5kg of polyvinylpyrrolidone.
The boron nitride mixed modified polyethylene heat-conducting composite material obtained in the embodiment is prepared by the following method:
firstly preparing boron nitride two-dimensional nanosheets, putting h-BN with the particle size of 5-15 nm in a conical flask for drying treatment for 24h, then putting metal sodium in the conical flask for sealing, adding nitrogen for protection, and keeping the temperature of 120 ℃ for 40h under the magnetic stirring state in an anhydrous and oxygen-free environment. And (3) naturally cooling, then sequentially dropwise adding n-hexane and dimethylformamide, washing with distilled water for multiple times, and carrying out suction filtration and sedimentation to obtain the boron nitride two-dimensional nanosheet.
Weighing the raw materials according to a formula, wherein the one-dimensional boron nitride nanotube and the liquid-phase stripped boron nitride two-dimensional nanosheet are dried in a vacuum oven at 80 ℃ for 6 hours for later use; and then pouring the raw materials into a high-speed mixer for mixing, adding the mixed materials into a double-roll open mill for further mixing at the stirring paddle rotating speed of 900 revolutions per minute, and finally performing compression molding to obtain the boron nitride mixed modified polyethylene heat-conducting composite material. Wherein the temperature of the double-roller open mill is as follows: the temperature of the front roller is 110 ℃, the temperature of the rear roller is 115 ℃, and the distance between the rollers is controlled to be 4-6 mm; the temperature of the tablet press is 175 ℃ at the upper plate and 175 ℃ at the lower plate, the low pressure is 5min, the high pressure is 6min, and the cooling is 3min.
The thermally conductive composite materials prepared in examples 1 to 5 were subjected to performance tests, and the test results are shown in the following table (/ not tested).
| Thermally conductive material | Thermal conductivity/W/(m. K) | Volume resistance/. About.108Ω | Breakdown voltage/kV |
| Example 1 | 0.51 | 2.32 | 7.74 |
| Example 2 | 0.65 | 0.45 | 7.65 |
| Example 3 | 0.82 | 1.07 | 7.72 |
| Example 4 | 0.82 | / | / |
| Example 5 | 0.82 | / | / |
The surface modification of the one-dimensional boron nitride nanotube adopted in the above embodiment is specifically performed by the following steps: adding the boron nitride nanotube into an absolute ethyl alcohol solution of a silane coupling agent, controlling the temperature to be 50 ℃, stirring for 6h on a magnetic stirrer, performing ultrasonic treatment for 30min, centrifuging by using a high-speed core machine, washing for 3 times by using absolute ethyl alcohol, finally, putting the modified material into a vacuum drying oven for drying, sealing and storing for later use.
Example 6
The same as example 1 except that the silane coupling agent was KH550 in an amount of 0.2% by mass based on the boron nitride nanotubes.
Example 7
The silane coupling agent was KH570, added in an amount of 0.2% by mass based on the boron nitride nanotubes, as in example 2.
Example 8
The silane coupling agent was KH570, added in an amount of 0.2% by mass based on the boron nitride nanotubes, as in example 3.
Example 9
The silane coupling agent was KH570, added in an amount of 0.4% by mass based on the boron nitride nanotubes, as in example 3.
Example 10
The silane coupling agent was KH570, added in an amount of 0.5% by mass based on the boron nitride nanotubes, as in example 3.
The thermally conductive composite materials prepared in examples 6 to 10 were subjected to performance tests, and the test results are shown in the following table.
| Thermally conductive material | Thermal conductivity/W/(m.K) | Volume resistance/' 108Ω | Breakdown voltage/kV |
| Example 6 | 0.63 | 1.15 | 7.68 |
| Example 7 | 0.76 | 1.50 | 7.74 |
| Example 8 | 1.08 | 1.46 | 7.72 |
| Example 9 | 1.01 | 1.47 | 7.74 |
| Example 10 | 0.98 | 1.53 | 7.78 |
A comparative example was prepared on the basis of example 1, using SDS as the dispersant instead of polyvinylpyrrolidone, and was subjected to a performance test, resulting in a thermal conductivity of 0.47W/(m.K), a volume resistance of 0.17X 108Ω, breakdown voltage 7.67kV.
Claims (10)
1. The boron nitride mixed modified polyethylene heat-conducting composite material is characterized by comprising the following components in parts by weight: 100 parts of polyethylene resin, 5-20 parts of boron nitride mixed filler particles, 0.05-0.10 part of composite antioxidant and 0.2-0.5 part of dispersant, wherein the boron nitride mixed filler particles are a mixture of one-dimensional boron nitride nanotubes and liquid-phase-stripped boron nitride two-dimensional nanosheets.
2. The boron nitride mixed modified polyethylene heat-conducting composite material according to claim 1, wherein the mixing weight ratio of the one-dimensional boron nitride nanotubes to the liquid-phase exfoliated boron nitride two-dimensional nanosheets is 1: 2-9.
3. The boron nitride mixed modified polyethylene heat-conducting composite material according to claim 1, wherein the one-dimensional boron nitride nanotubes are modified with a silane coupling agent KH-550 or KH-570.
4. The boron nitride mixed modified polyethylene heat-conducting composite material according to claim 1, wherein the liquid-phase-peeled boron nitride two-dimensional nanosheet is obtained by liquid-phase peeling of h-BN with the particle size of 5-15 nm.
5. The boron nitride mixed modified polyethylene heat conduction composite material according to claim 1, wherein the dispersant is polyvinylpyrrolidone.
6. The boron nitride mixed modified polyethylene heat conduction composite material according to claim 1, wherein the composite antioxidant is formed by mixing an antioxidant 1010 and an antioxidant 168.
7. The preparation method of the boron nitride mixed and modified polyethylene heat-conducting composite material is characterized by pouring 100 parts of polyethylene resin, 5-20 parts of boron nitride mixed and filled particles, 0.05-0.10 part of composite antioxidant and 0.2-0.5 part of dispersant into a high-speed mixer for mixing, then adding the mixture into a double-roll open mill for further mixing, and finally performing compression molding to obtain the boron nitride mixed and modified polyethylene heat-conducting composite material, wherein the boron nitride mixed and filled particles are a mixture of one-dimensional boron nitride nanotubes and liquid-phase peeled boron nitride two-dimensional nanosheets.
8. The preparation method of the boron nitride mixed modified polyethylene heat conduction composite material according to claim 7, wherein the mixing weight ratio of the one-dimensional boron nitride nanotubes to the liquid-phase exfoliated boron nitride two-dimensional nanosheets is 1: 2-9.
9. The method for preparing the boron nitride mixed modified polyethylene heat-conducting composite material according to claim 7, wherein the one-dimensional boron nitride nanotubes are modified by the following steps: adding the boron nitride nanotube into an absolute ethyl alcohol solution of a silane coupling agent, stirring and centrifuging, washing with absolute ethyl alcohol, and finally performing vacuum drying, wherein the silane coupling agent is KH-550 or KH-570, and the using amount of the silane coupling agent is 0.2-0.5% of the weight of the boron nitride nanotube.
10. The preparation method of the boron nitride mixed modified polyethylene heat conduction composite material according to claim 7, wherein the liquid-phase exfoliated boron nitride two-dimensional nanosheet is prepared by the following steps: and (2) adding metal sodium after h-BN drying treatment, adding nitrogen for protection and sealing, keeping the temperature of 115-125 ℃ for more than 35h under a stirring state in an anhydrous and oxygen-free environment, naturally cooling, then sequentially dropwise adding n-hexane and dimethylformamide, washing with distilled water for multiple times, and carrying out suction filtration and sedimentation to obtain the boron nitride two-dimensional nanosheet.
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