CN115433389A - Dual-heat-conduction-network polyurethane heat-conduction composite material constructed by two-step method and preparation method thereof - Google Patents
Dual-heat-conduction-network polyurethane heat-conduction composite material constructed by two-step method and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a dual heat-conducting network polyurethane heat-conducting composite material constructed by a two-step method and a preparation method thereof, wherein a thermoplastic polyurethane material is used as a matrix of the composite material, a heat-conducting network 1 is constructed in a porous polymer framework by a heat-conducting filler A based on an in-situ foaming polymerization process, and a heat-conducting filler B is adsorbed on the three-dimensional porous framework of a polymer to form a heat-conducting network 2. The method utilizes a two-step preparation process to regulate and control two different heat-conducting fillers to successfully construct an even and ordered dual heat-conducting path in a polymer matrix, and compared with the traditional method of directly and simply mixing and filling two fillers to prepare the heat-conducting composite material, the method can more finely regulate and control the even distribution of the heat-conducting fillers, construct an efficient heat-conducting passage and obviously improve the heat-conducting property of the polymer material. The preparation method of the polymer composite material with the three-dimensional double heat-conducting network, provided by the invention, is simple in process, is easy to realize large-scale production, and has important industrial potential.
Description
Technical Field
The invention belongs to the field of polymer-based heat-conducting composite materials and preparation thereof, and particularly relates to a dual heat-conducting network polyurethane heat-conducting composite material constructed by a two-step method and a preparation method thereof.
Background
In recent years, with the rapid development of microelectronic technology, the demand for high performance heat dissipation technology and high thermal conductivity material has increased to an unprecedented level. The traditional heat conduction materials such as metal and inorganic heat conduction materials have the defects of large mass, poor flexibility and the like, and the polymer has the characteristics of high insulativity, easy processability, flexibility and the like, and the compounding of the polymer and the high heat conduction filler is a simple and efficient strategy for preparing the heat conduction polymer composite material.
For the polymer heat-conducting composite material, the key to obtain excellent heat-conducting performance is whether the heat-conducting fillers can be connected with each other to form an effective heat-conducting path. When most of single heat conduction filler fills preparation heat conduction polymer composite, often the heat conductivility is relatively poor when lower filler content, can not satisfy the in-service use requirement, and when higher heat conduction filler content, though the heat conductivility is good, but mechanical properties is showing to descend and processing difficulty.
The prior literature reports that two or more heat-conducting fillers with different sizes and appearances are used together, and the heat-conducting property of the polymer composite material filled with the single filler can be obviously better than that of the polymer composite material filled with the single filler under the same filling amount. In addition, the heat conduction efficiency can be effectively improved by connecting the heat conduction fillers with each other by virtue of the template to form a highly-interconnected three-dimensional heat conduction network. Therefore, the polymer is used as a matrix to construct an efficient heat conduction network template through structure/function integrated design, and the ordered heat conduction network construction between the fillers is regulated and controlled based on a specific preparation process on the basis of the synergistic effect generated by different sizes and different forms of two or more heat conduction fillers, so that the heat conduction effect can be further remarkably improved, and the low-filling-amount polymer heat conduction composite material with both mechanical and heat conduction properties is obtained.
Disclosure of Invention
Aiming at the technical problems, the invention provides a dual heat-conducting network polyurethane heat-conducting composite material constructed by a two-step method and a preparation method thereof. The preparation method of the polyurethane composite material with the three-dimensional double heat-conducting network provided by the invention is simple in process, easy to realize large-scale production and has important industrial potential.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention relates to a polyurethane heat-conducting composite material with double heat-conducting networks, which takes a thermoplastic polyurethane material as a matrix of the composite material, constructs a heat-conducting network 1 in a porous polymer framework by using a heat-conducting filler A based on an in-situ foaming polymerization process, and adsorbs a heat-conducting filler B on the three-dimensional porous framework of a polymer to form a heat-conducting network 2.
The heat conducting filler A is one or more of flaky heat conducting fillers or whisker-shaped heat conducting fillers.
The heat-conducting filler B is one or more of granular heat-conducting filler, flaky heat-conducting filler and whisker-shaped heat-conducting filler.
The flaky heat conducting filler is one or more of graphene nanosheets, boron nitride nanosheets and flaky aluminum nitride; the granular heat-conducting filler is one or more of aluminum nitride, aluminum oxide, silicon nitride and the like; the whisker-shaped heat-conducting filler is one or more of carbon nano tubes, carbon fibers, fibrous carbon powder and the like.
The preparation method of the polyurethane heat-conducting composite material with the double heat-conducting networks comprises the following steps:
step 1: the preparation method comprises the steps of blending a polyurethane foaming white material raw material and a heat-conducting filler A to uniformly mix the heat-conducting filler, adding a black material (isocyanate) to stir uniformly, and carrying out in-situ polymerization foaming at room temperature to prepare the heat-conducting filler A/polyurethane foaming composite material with a three-dimensional porous framework structure. The thermally conductive filler forms a continuous thermally conductive network 1 within the polymer matrix.
The white material comprises the following raw materials in parts by mass: 60-80 parts of trifunctional polyether polyol, 6-10 parts of cross-linking agent, 0.5-1 part of amine catalyst, 0.5-1 part of water, 5-8 parts of foaming agent and 0.4-0.8 part of foam stabilizer silicone oil.
The black material is 45-55 parts of polymethylene polyisocyanate.
Step 2: dispersing the heat-conducting filler B in an ethanol solution (the dispersion concentration is 0.2-1 mg/mL), soaking the polyurethane foam obtained in the step 1 in the solution, accelerating the uniform passing of the dispersion liquid in a suction filtration mode, and circulating for 5-10 times; and taking out the impregnated foam, drying the solution on the surface of the foam by using a high-temperature air gun, then placing the foam in an air-blowing drying oven for drying treatment for 60-120 minutes, and uniformly adsorbing the heat-conducting filler B in a three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to form a three-dimensional heat-conducting network 2.
The addition amount of the heat-conducting filler A is 5-25% of the total mass of the white material and the black material; the addition amount of the heat-conducting filler B is 5-15% of the total mass of the white material and the black material.
And step 3: and (3) carrying out high-temperature hot-press molding on the polymer foam obtained in the step (2) at 175 ℃ and 10MPa to obtain the compact polyurethane heat-conducting composite material with the double heat-conducting filler network.
Compared with the prior art, the invention has the beneficial effects that:
the invention has the beneficial effects that: the invention designs a brand-new preparation method of a polymer-based multi-filler heat-conducting composite material according to the foaming process and the controllability of a cellular structure of polyurethane, and the heat-conducting filler A is uniformly doped in a foam framework by utilizing the polyurethane in-situ foaming polymerization process, so that a continuous heat-conducting path of the filler A is formed while foam is foamed and molded. And continuously utilizing the three-dimensional network skeleton structure of the foam after the foam is formed, and adsorbing a layer of heat-conducting filler on the cell wall to form a heat-conducting path of the filler B. Compared with the traditional filling type heat conduction material, the two different fillers in the polymer matrix are directly mixed to form more ordered arrangement and connection, so that a more efficient heat conduction path is constructed, and the heat conduction performance of the composite material is obviously improved under the same filling amount.
Drawings
FIG. 1 is a diagram of the preparation process and heat transfer mechanism of the composite material.
FIG. 2 is a scanning electron microscope image of the composite material under different magnifications.
Detailed Description
The technical solution of the present invention is further described in detail by the following specific examples, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the following examples.
The polyurethane foam matrix formulations used in the examples are shown in the following table:
in the following examples, the mechanical property test method is in accordance with the national standard GB/T6344-2008, and the stretching rate is 200mm/min. The thermal conductivity performance test conforms to the standard GB/T22588-2008, and the experimental condition is 25 ℃ at room temperature. The invention also carries out scanning electron microscope observation on the microscopic surface of the obtained composite material.
Comparative example 1:
1) Uniformly mixing polyurethane foaming raw materials, and then carrying out foaming treatment to form a polymer foam body with a three-dimensional continuous cell structure;
2) Carrying out hot pressing on the polyurethane foam obtained in the step 1) at 175 ℃ under the pressure of 10MPa for 10min to obtain a compact polymer material.
Comparative example 2:
1) And (2) blending the polyurethane foaming raw material white material and the heat-conducting filler hexagonal boron nitride to uniformly mix the heat-conducting filler in the polymer raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with the three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polymer matrix;
2) Carrying out hot pressing on the polyurethane foam obtained in the step 1) at 175 ℃ and under the pressure of 10MPa for 10min to obtain the compact polymer-based composite material with the heat conducting network.
Comparative example 3:
1) And (2) blending the polyurethane foaming raw material white material and the heat-conducting filler hexagonal boron nitride to uniformly mix the heat-conducting filler in the polymer raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with the three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polymer matrix;
2) Carrying out hot pressing on the polyurethane foam obtained in the step 1) at 175 ℃ and under the pressure of 10MPa for 10min to obtain the compact polymer-based composite material with the heat conducting network.
Example 1:
1) And mixing the polyurethane foaming raw material A and the heat-conducting filler hexagonal boron nitride to uniformly mix the heat-conducting filler in the polyurethane raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with the three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polyurethane matrix;
2) Dispersing hexagonal boron nitride serving as a heat-conducting filler in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the impregnated foam, drying the solution on the surface of the foam by using a high-temperature air gun, then placing the foam in an air-blast drying oven for drying treatment for 60-120 minutes, and uniformly adsorbing the heat-conducting filler B in a three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain a three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Carrying out hot pressing on the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a double heat-conducting filler network;
example 2:
1) Uniformly mixing polyurethane foaming raw materials, and then carrying out foaming treatment to form a polyurethane foam body with a three-dimensional continuous cell structure;
2) Dispersing hexagonal boron nitride serving as a heat-conducting filler in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the soaked foam, drying the solution on the surface of the foam by using a high-temperature air gun, then placing the foam in a blast drying oven for drying treatment for 60-120 minutes, and uniformly adsorbing the heat-conducting filler in a three-dimensional framework of the polyurethane foam material to obtain the heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Hot-pressing the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a heat-conducting filler network;
example 3:
1) The preparation method comprises the following steps of blending a polyurethane foaming raw material A and hexagonal boron nitride of a heat-conducting filler to uniformly mix the heat-conducting filler in the polyurethane raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with a three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polyurethane matrix;
2) Dispersing hexagonal boron nitride serving as a heat-conducting filler in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the impregnated foam, drying the solution on the surface of the foam by using a high-temperature air gun, then placing the foam in an air-blast drying oven for drying treatment for 60-120 minutes, and uniformly adsorbing the heat-conducting filler B in a three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain a three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Carrying out hot pressing on the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a double heat-conducting filler network;
example 4:
1) Uniformly mixing polyurethane foaming raw materials, and then carrying out foaming treatment to form a polyurethane foam body with a three-dimensional continuous cell structure;
2) Dispersing hexagonal boron nitride serving as a heat-conducting filler in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the impregnated foam, drying the solution on the surface of the foam by using a high-temperature air gun, and then placing the foam in an air-blast drying oven for drying treatment for 60-120 minutes, so that the heat-conducting filler is uniformly adsorbed in a three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain a three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Hot-pressing the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a heat-conducting filler network;
example 5:
1) The preparation method comprises the following steps of blending a polyurethane foaming raw material A and hexagonal boron nitride of a heat-conducting filler to uniformly mix the heat-conducting filler in the polyurethane raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with a three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polyurethane matrix;
2) Dispersing hexagonal boron nitride serving as a heat-conducting filler in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the soaked foam, drying the solution on the surface of the foam by using a high-temperature air gun, and then placing the foam in a blast drying oven for drying treatment for 60-120 minutes, so that the heat-conducting filler B is uniformly adsorbed in the three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain the three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Carrying out hot pressing on the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a double heat-conducting filler network;
example 6:
1) The preparation method comprises the following steps of blending a polyurethane foaming raw material A and hexagonal boron nitride of a heat-conducting filler to uniformly mix the heat-conducting filler in the polyurethane raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with a three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polyurethane matrix;
2) Dispersing the heat-conducting filler carbon nano tubes in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the soaked foam, drying the solution on the surface of the foam by using a high-temperature air gun, and then placing the foam in a blast drying oven for drying treatment for 60-120 minutes, so that the heat-conducting filler B is uniformly adsorbed in the three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain the three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Carrying out hot pressing on the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a double heat-conducting filler network;
example 7:
1) Uniformly mixing polyurethane foaming raw materials, and then carrying out foaming treatment to form a polyurethane foam body with a three-dimensional continuous cell structure;
2) Dispersing hexagonal boron nitride serving as a heat-conducting filler and carbon nano tubes in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the soaked foam, drying the solution on the surface of the foam by using a high-temperature air gun, and then placing the foam in a blast drying oven for drying treatment for 60-120 minutes, so that the heat-conducting filler is uniformly adsorbed in the three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain the three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Hot-pressing the polyurethane foam obtained in the step 2) at 175 ℃ under the pressure of 10MPa for 10min to form a compact polyurethane heat-conducting composite material with a heat-conducting filler network;
example 8:
1) And mixing the polyurethane foaming raw material A and the heat-conducting filler hexagonal boron nitride to uniformly mix the heat-conducting filler in the polyurethane raw material, then carrying out foaming treatment, and carrying out in-situ polymerization foaming to prepare the heat-conducting filler A/polyurethane foaming composite material with the three-dimensional porous skeleton structure. The heat-conducting filler forms a continuous heat-conducting network 1 in the polyurethane matrix;
2) Dispersing the heat-conducting filler aluminum nitride in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the soaked foam, drying the solution on the surface of the foam by using a high-temperature air gun, and then placing the foam in a blast drying oven for drying treatment for 60-120 minutes, so that the heat-conducting filler B is uniformly adsorbed in the three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain the three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Carrying out hot pressing on the polyurethane foam obtained in the step 2) at 175 ℃ under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a double heat-conducting filler network;
example 9:
1) Uniformly mixing polyurethane foaming raw materials, and then carrying out foaming treatment to form polyurethane foam with a three-dimensional continuous cell structure;
2) Dispersing hexagonal boron nitride and aluminum nitride serving as heat-conducting fillers in an ethanol solution, soaking the polyurethane foam obtained in the step 1) in the solution, and circulating the process for 1-5 times. And taking out the soaked foam, drying the solution on the surface of the foam by using a high-temperature air gun, and then placing the foam in a blast drying oven for drying treatment for 60-120 minutes, so that the heat-conducting filler is uniformly adsorbed in the three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to obtain the three-dimensional heat-conducting network 2. Wherein the concentration of the heat-conducting filler solution is 0.2-2 mg/ml;
3) Hot-pressing the polyurethane foam obtained in the step 2) at 175 ℃ and under the pressure of 10MPa for 10min to obtain a compact polyurethane heat-conducting composite material with a heat-conducting filler network;
table 1 shows the raw material ratios of comparative examples and examples 1 to 9
The resulting composite was subjected to physical property tests, and the results are shown in Table 2 below.
TABLE 2 physical Properties and thermal conductivities
As can be seen from the test results in Table 2, compared with the method of directly adsorbing the heat-conducting filler on the foam surface, the method of the invention, based on the two-step stepwise filling heat-conducting filler preparation process, can obtain the double-filler network polyurethane heat-conducting composite material with the heat conductivity coefficient obviously higher than that of the composite material obtained by simultaneously adding two heat-conducting fillers into the polyurethane matrix, thereby greatly improving the heat management performance of the polymer material.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (5)
1. A dual heat-conducting network polyurethane heat-conducting composite material constructed by a two-step method is characterized in that:
the double heat-conducting network polyurethane heat-conducting composite material takes a thermoplastic polyurethane material as a matrix of the composite material, a heat-conducting network 1 is constructed in a porous polymer framework by using a heat-conducting filler A based on an in-situ foaming polymerization process, and a heat-conducting filler B is adsorbed on the three-dimensional porous framework of a polymer to form a heat-conducting network 2;
the heat conducting filler A is one or more of flaky heat conducting fillers or whisker-shaped heat conducting fillers;
the heat-conducting filler B is one or more of granular heat-conducting filler, flaky heat-conducting filler and whisker heat-conducting filler.
2. The dual heat-conducting network polyurethane heat-conducting composite material as claimed in claim 1, wherein:
the flaky heat conducting filler is one or more of graphene nanosheets, boron nitride nanosheets and flaky aluminum nitride; the granular heat-conducting filler is one or more of aluminum nitride, aluminum oxide, silicon nitride and the like; the whisker-shaped heat-conducting filler is one or more of carbon nano tubes, carbon fibers, fibrous carbon powder and the like.
3. The preparation method of the polyurethane heat-conducting composite material with the double heat-conducting network as claimed in claim 1 or 2 is characterized by comprising the following steps:
step 1: mixing a polyurethane foaming white material raw material with a heat-conducting filler A to uniformly mix the heat-conducting filler, then adding a black material, uniformly stirring, carrying out in-situ polymerization foaming at room temperature to prepare a heat-conducting filler A/polyurethane foaming composite material with a three-dimensional porous skeleton structure, wherein the heat-conducting filler forms a continuous heat-conducting network 1 in a polymer matrix;
step 2: dispersing the heat-conducting filler B in an ethanol solution, soaking the polyurethane foam obtained in the step 1 in the solution, accelerating the uniform passing of the dispersion liquid in a suction filtration mode, and circulating for 5-10 times; taking out the soaked foam, drying the solution on the surface of the foam, and then placing the foam in a forced air drying oven for drying treatment for 60-120 minutes, wherein the heat-conducting filler B is uniformly adsorbed in a three-dimensional framework of the heat-conducting filler A/polyurethane foaming composite material to form a three-dimensional heat-conducting network 2;
and 3, step 3: and (3) carrying out high-temperature hot-press molding on the polymer foam obtained in the step (2) at 175 ℃ and 10MPa to obtain the compact polyurethane heat-conducting composite material with the double heat-conducting filler network.
4. The production method according to claim 3, characterized in that:
in the step 1, the white material raw material comprises the following components in parts by weight: 60-80 parts of trifunctional polyether polyol, 6-10 parts of cross-linking agent, 0.5-1 part of amine catalyst, 0.5-1 part of water, 5-8 parts of foaming agent and 0.4-0.8 part of foam stabilizer silicone oil; the black material is 45-55 parts of polymethylene polyisocyanate.
5. The production method according to claim 3, characterized in that:
the addition amount of the heat-conducting filler A is 5-25% of the total mass of the white material and the black material; the addition amount of the heat-conducting filler B is 5-15% of the total mass of the white material and the black material.
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| US20130001460A1 (en) * | 2010-03-30 | 2013-01-03 | Tokai Chemical Industries, Ltd. | Urethane foam molded product and method for producing the same |
| CN112574468A (en) * | 2019-09-30 | 2021-03-30 | 天津理工大学 | Heat-conducting polymer composite material with multi-layer continuous network structure and preparation method thereof |
| CN110964305A (en) * | 2019-12-17 | 2020-04-07 | 上海大学 | Polymer-based intelligent heat dissipation material, preparation method and application thereof |
| US20220010187A1 (en) * | 2020-07-13 | 2022-01-13 | L&P Property Management Company | Thermally conductive nanomaterials in flexible foam |
| CN114854087A (en) * | 2022-05-13 | 2022-08-05 | 吉林大学 | Polyimide composite material with double heat-conducting networks and preparation method thereof |
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