CN111732778A - Preparation method of high-thermal-conductivity composite material - Google Patents
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Abstract
The invention discloses a preparation method of a high-thermal-conductivity composite material, which comprises the following steps: adding a heat conduction material, a dispersing agent, a natural organic high molecular material and polymer powder into an aqueous solution according to the weight part ratio for pre-dispersion treatment, transferring the mixture into an autoclave for heat treatment after the pre-dispersion treatment, drying the mixture after the heat treatment, adding the dried mixture into an organic solvent, grinding the mixture, obtaining micron-sized mixed heat conduction polymer fiber yarns by an electrostatic spinning technology, and then carrying out melt extrusion and granulation on the heat conduction polymer fiber yarns by a double-screw extruder to obtain the high heat conduction polymer master batch. The invention has the advantages of low addition amount of the heat-conducting filler, excellent heat-conducting property, good dispersibility and the like, has good mechanical property, obtains high heat conductivity and simultaneously has good mechanical property, and solves the problems of poor affinity and uneven dispersion of the heat-conducting filler and a polymer matrix, improved heat conductivity, reduced mechanical property and the like.
Description
Technical Field
The invention relates to the technical field of high-thermal-conductivity composite materials, in particular to a preparation method of a high-thermal-conductivity composite material.
Background
The plastic has the advantages of light weight, stable chemical property, corrosion resistance, easy processing and the like, and has wide application in the fields of electronic and electric products, packaging industry, automobile industry, mechanical manufacturing, aerospace and the like. However, the low thermal conductivity of plastics limits their applications.
In order to obtain a highly heat conductive plastic, a common approach is to add a heat conductive filler, such as: wanwen et al used graphene as a thermal conductive filler, added to polypropylene materials, when the graphene content was 60%, the thermal conductivity increased to 1.32W/(m.K), which was 14 times higher than that of pure polypropylene, but the thermal stability decreased accordingly.
Patent ZL200510101700.0 discloses an injection-molded insulating heat-conducting plastic, which takes metal oxide and silicon carbide as heat-conducting fillers, when the ratio of alumina, magnesia fillers and polyphenylene sulfide matrix is 7:1, the heat conductivity coefficient is 1.967W/(m.K), the tensile strength is 41.4MPa, and the heat conductivity is reduced by 34% compared with pure polyphenylene sulfide (63 MPa). The addition amount of the filler becomes a determining factor of heat conduction, and a large amount of the filler inevitably causes the reduction of the mechanical property and the processability of the polymer, thereby limiting the application of the polymer.
Patent CN108017820A discloses a fiber-reinforced high-density polyethylene/graphene composite material and a preparation method thereof, in which plant fibers and graphene are used as additives to be mixed and filled, and this way can improve the mechanical properties of the composite material to a certain extent, but has a limited influence on the thermal conductivity.
In the current research, the filler has poor affinity and uneven dispersion with the polymer matrix, and the mechanical properties are reduced while the thermal conductivity is improved, which limits the application of the heat-conducting composite material.
Disclosure of Invention
In view of the above technical deficiencies, the present invention provides a method for preparing a high thermal conductive composite material, so as to solve the problems in the background art.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a preparation method of a high-thermal-conductivity composite material, which comprises the following steps:
1) the formula comprises the following components in parts by weight: 0.1-10 parts of heat conduction material, 0.5-2 parts of dispersing agent, 1-5 parts of natural organic high molecular material and 100 parts of polymer powder;
2) adding a heat conduction material, a dispersing agent, a natural organic high polymer material and polymer powder into an aqueous solution according to the proportion in the step 1) for pre-dispersion treatment, and transferring the mixture into an autoclave for heat treatment after the pre-dispersion treatment;
3) drying the solution obtained in the step 2), adding the dried solution into an organic solvent, grinding, and obtaining micron-grade mixed heat-conducting polymer fiber yarns by an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
Preferably, the heat conducting material is one or more of a novel carbon material, a high heat conducting inorganic non-metallic material, a metal or a metal oxide material; the natural organic high molecular material is one or more of starch, chitosan, cellulose or cyclodextrin; the polymer powder is one or more of polyethylene and polypropylene; the dispersant is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent.
Preferably, the organic solvent in step 3) is N, N dimethylformamide.
Preferably, the grinding fineness of the step 3) is less than or equal to 1 μm, and the diameter of the heat-conducting polymer fiber yarn is 5-10 μm.
Preferably, the conditions of the heat treatment of the autoclave in the step 2) are that the temperature in the autoclave is more than 140 ℃, the pressure is more than 0.2MPa, and the reaction process is continuously stirred.
Preferably, the pre-dispersion treatment in the step 2) adopts ultrasonic dispersion or sand mill dispersion.
Preferably, the drying in step 3) is freeze-drying or spray-drying, and the freeze-drying conditions are as follows: the freeze-drying temperature is maintained at-50-30 ℃, the freeze-drying time is 10-40 h, and the vacuum degree is 1-300 Pa; the spray drying conditions were: the inlet temperature is 100-350 ℃, the outlet temperature is 40-150 ℃, and the drying medium is hot air.
The invention has the beneficial effects that:
1. the invention adopts a molding process of steam pressure-spinning-melt blending, wherein the steam pressure is to compound the heat conduction material and the polymer powder by using a natural organic macromolecular compound auxiliary agent, the spinning is to uniformly mix the composite material in a micron order, the melt blending is to further uniformly mix the composite material to uniformly mix the composite material, and the high heat conduction composite material prepared by the process has higher heat conductivity than the existing product and excellent heat conduction performance.
2. The invention adopts the molding process of steam pressure-spinning-melting blending to realize micron-grade mixing of the composite material, improve the dispersibility of the heat-conducting filler in the polymer and solve the problem of poor compatibility of the heat-conducting filler and the polymer matrix.
3. The addition amount of the heat conduction material is not more than 10 percent, the problem of mechanical property reduction caused by overlarge addition amount of the heat conduction filler is avoided, and simultaneously, the autoclaved-spun-melted molding process is utilized to play a role in strengthening and toughening.
4. The high-thermal-conductivity composite material prepared by the invention has the advantages of low addition amount of the thermal-conductivity filler, excellent thermal conductivity, good dispersibility and the like, has good mechanical properties, obtains high thermal conductivity and simultaneously has good mechanical properties, and solves the problems of poor affinity and uneven dispersion of the thermal-conductivity filler and a polymer matrix, improved thermal conductivity, reduced mechanical properties and the like.
Drawings
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a photomicrograph of a thermally conductive polymer filament prepared in step 3) of example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
as shown in fig. 1, the present invention provides a method for preparing a high thermal conductive composite material, comprising the following steps:
1) the formula comprises the following components in parts by weight:
the heat conduction material is a mixture of graphene and copper powder, wherein 0.4 part of graphene and 0.1 part of copper powder are used as the heat conduction material;
0.8 part of silane coupling agent serving as a dispersing agent;
2 parts of natural organic high polymer material, namely starch;
the polymer powder is polyethylene, 100 parts;
2) adding graphene, copper powder, a silane coupling agent, starch and polyethylene into an aqueous solution according to the proportion in the step 1), performing pre-dispersion treatment by adopting ultrasonic dispersion, transferring the pre-dispersed material into an autoclave for heat treatment, wherein the treatment temperature is 150 ℃, the pressure is 0.25MPa, and the reaction process is continuously stirred;
3) carrying out freeze drying treatment on the solution obtained in the step 2), wherein the treatment conditions are as follows: maintaining the freeze-drying temperature at-30 ℃, the freeze-drying time at 25h and the vacuum degree at 100Pa, drying, adding the dried mixture into N, N dimethylformamide solvent, grinding the mixture to the fineness of less than or equal to 1 mu m, and obtaining the heat-conducting polymer fiber yarns with the diameter of 5-10 mu m by using an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
Example 2:
the invention provides a preparation method of a high-thermal-conductivity composite material, which comprises the following steps:
1) the formula comprises the following components in parts by weight:
the heat conduction material is a mixture of graphene and aluminum oxide, wherein 0.4 part of graphene and 0.1 part of aluminum oxide are used as the heat conduction material;
0.7 part of titanate coupling agent serving as a dispersing agent;
1.5 parts of cyclodextrin serving as a natural organic high polymer material;
the polymer powder is polyethylene, 100 parts;
2) adding graphene, aluminum oxide, titanate coupling agent, chitosan and polyethylene into an aqueous solution according to the proportion in the step 1), performing pre-dispersion treatment by adopting ultrasonic dispersion, transferring the pre-dispersed material into an autoclave for heat treatment, wherein the treatment temperature is 150 ℃, the pressure is 0.25MPa, and the reaction process is continuously stirred;
3) carrying out freeze drying treatment on the solution obtained in the step 2), wherein the treatment conditions are as follows: maintaining the freeze-drying temperature at-30 ℃, the freeze-drying time at 25h and the vacuum degree at 100Pa, drying, adding the dried mixture into N, N dimethylformamide solvent, grinding the mixture to the fineness of less than or equal to 1 mu m, and obtaining the heat-conducting polymer fiber yarns with the diameter of 5-10 mu m by using an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
Example 3:
the invention provides a preparation method of a high-thermal-conductivity composite material, which comprises the following steps:
1) the formula comprises the following components in parts by weight:
the heat conducting material is a mixture of carbon microspheres and silicon carbide, wherein the carbon microspheres are 0.2 part by weight and the silicon carbide is 0.2 part by weight;
1.5 parts of an aluminate coupling agent as a dispersing agent;
2.5 parts of natural organic high polymer material, namely cellulose;
the polymer powder is polyethylene, 100 parts;
2) adding carbon microspheres, silicon carbide, an aluminate coupling agent, cellulose and polyethylene into an aqueous solution according to the proportion in the step 1), dispersing by adopting a sand mill for pre-dispersion treatment, transferring the pre-dispersed material into an autoclave for heat treatment after the pre-dispersion treatment, wherein the treatment temperature is 160 ℃, the pressure is 0.3MPa, and the reaction process is continuously stirred;
3) carrying out spray drying treatment on the solution obtained in the step 2), wherein the treatment conditions are as follows: the inlet temperature is 150 ℃, the outlet temperature is 60 ℃, the drying medium is hot air, the hot air is added into N, N dimethylformamide solvent after being dried, the mixture is ground until the fineness is less than or equal to 1 mu m, and the heat-conducting polymer fiber yarns with the diameter of 5-10 mu m are obtained through an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
Example 4:
the invention provides a preparation method of a high-thermal-conductivity composite material, which comprises the following steps:
1) the formula comprises the following components in parts by weight:
the heat conducting material is a mixture of carbon microspheres and silicon nitride, wherein the carbon microspheres are 0.2 part and the silicon nitride is 0.2 part;
0.5 part of aluminate coupling agent serving as a dispersing agent;
1 part of natural organic high polymer material is cellulose;
the polymer powder is polyethylene, 100 parts;
2) adding carbon microspheres, silicon nitride, an aluminate coupling agent, cellulose and polyethylene into an aqueous solution according to the proportion in the step 1), dispersing by adopting a sand mill for pre-dispersion treatment, transferring the pre-dispersed mixture into an autoclave for heat treatment after the pre-dispersion treatment, wherein the treatment temperature is 160 ℃, the pressure is 0.3MPa, and the reaction process is continuously stirred;
3) carrying out spray drying treatment on the solution obtained in the step 2), wherein the treatment conditions are as follows: the inlet temperature is 150 ℃, the outlet temperature is 60 ℃, the drying medium is hot air, the hot air is added into N, N dimethylformamide solvent after being dried, the mixture is ground until the fineness is less than or equal to 1 mu m, and the heat-conducting polymer fiber yarns with the diameter of 5-10 mu m are obtained through an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
Example 5:
the invention provides a preparation method of a high-thermal-conductivity composite material, which comprises the following steps:
1) the formula comprises the following components in parts by weight:
the heat conduction material is a mixture of graphene and aluminum oxide, wherein 5 parts of graphene and 1 part of aluminum oxide are used;
the dispersing agent is a mixture of silane coupling agent and aluminate coupling agent, wherein 1 part of silane coupling agent and 0.5 part of aluminate coupling agent;
3 parts of cyclodextrin serving as a natural organic high polymer material;
100 parts of polypropylene as polymer powder;
2) adding graphene, alumina, a silane coupling agent, an aluminate coupling agent, cyclodextrin and polypropylene into an aqueous solution according to the proportion of the step 1), dispersing by adopting a sand mill for pre-dispersion treatment, transferring the pre-dispersed material into an autoclave for heat treatment after the pre-dispersion treatment, wherein the treatment temperature is 200 ℃, the pressure is 0.5MPa, and the reaction process is continuously stirred;
3) carrying out spray drying treatment on the solution obtained in the step 2), wherein the treatment conditions are as follows: the inlet temperature is 200 ℃, the outlet temperature is 80 ℃, the drying medium is hot air, the hot air is added into N, N dimethylformamide solvent after being dried, the mixture is ground until the fineness is less than or equal to 1 mu m, and the heat-conducting polymer fiber yarns with the diameter of 5-10 mu m are obtained through an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
Example 6:
the invention provides a preparation method of a high-thermal-conductivity composite material, which comprises the following steps:
1) the formula comprises the following components in parts by weight:
the heat conduction material is a mixture of graphene, copper powder and aluminum oxide, wherein 6 parts of graphene, 2 parts of copper powder and 2 parts of aluminum oxide are used;
the dispersant is an aluminate coupling agent, 2 parts;
the natural organic high molecular material is a mixture of chitosan and cyclodextrin, wherein the chitosan accounts for 3 parts, and the cyclodextrin accounts for 2 parts;
100 parts of polypropylene as polymer powder;
2) adding graphene, copper powder, alumina, an aluminate coupling agent, chitosan, cyclodextrin and polypropylene into an aqueous solution according to the proportion in the step 1), dispersing by adopting a sand mill for pre-dispersion treatment, transferring the pre-dispersed mixture into an autoclave for heat treatment after the pre-dispersion treatment, wherein the treatment temperature is 200 ℃, the pressure is 0.5MPa, and the reaction process is continuously stirred;
3) carrying out freeze drying treatment on the solution obtained in the step 2), wherein the treatment conditions are as follows: maintaining the freeze-drying temperature at-20 ℃, the freeze-drying time for 30 hours and the vacuum degree of 100Pa, drying, adding the dried mixture into N, N dimethylformamide solvent, grinding the mixture to the fineness of less than or equal to 1 mu m, and obtaining the heat-conducting polymer fiber yarns with the diameter of 5-10 mu m by using an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
FIG. 1 is a photomicrograph of the thermally conductive polymer fiber prepared in step 3) of example 1, wherein the diameter is 5-10 μm.
Experimental example:
sample a is the product prepared in example 1, sample B is the product prepared in example 2, sample C is the product prepared in example 3, sample D is the product prepared in example 4, sample E is the product prepared in example 5, sample F is the product prepared in example 6, the control sample is HDPE powder, manufacturer: model number LG-DOW in Korea; 5019 RQ.
1. Tensile strength test
The test basis is as follows: GB/16491-
The test instrument: universal tensile testing machine
And (3) test results: as can be seen from Table 1, the tensile strength of the sample A, B is more than 35MPa, the tensile strength of the sample C is 34.3MPa, the tensile strength of the sample D, E is more than 33MPa, the tensile strength of the sample F is 32.7MPa, the overall tensile strength is 32.7-35.5MPa, and is obviously improved compared with the tensile strength of the control sample of 28.5MPa, so that the tensile strength of the high-thermal-conductivity composite material prepared by the method is superior to that of the existing product.
TABLE 1 tensile Strength test results
| Sample (I) | Tensile strength (MPa) |
| A | 35.1 |
| B | 35.5 |
| C | 34.3 |
| D | 33.8 |
| E | 33.1 |
| F | 32.7 |
| Control sample | 28.5 |
2. Thermal conductivity test
The test basis is as follows: GB/T3399-1982
The test instrument: heat conductivity coefficient tester
And (3) test results: as can be seen from table 2, the thermal conductivity of sample a is 1.013W/(m · K), the thermal conductivity of sample B is 0.917W/(m · K), the thermal conductivity of sample C is 0.650W/(m · K), the thermal conductivity of sample a is better than that of sample B, the thermal conductivity of sample B is better than that of sample C, the thermal conductivity of sample D is 0.708W/(m · K), the thermal conductivity of sample E is 0.923W/(m · K), the thermal conductivity of sample F is 1.009W/(m · K), and the thermal conductivity of the control sample is only 0.410W/(m · K), which is lower than that of samples a to F.
Table 2 results of thermal conductivity test
3. Dispersion size scale test:
the test basis is as follows: GB/T18251-2019
The test instrument: carbon black dispersity tester
And (3) test results: as can be seen from table 3, the dispersion size grade of the sample a is 5.9, the dispersion size grade of the sample B is 5.7, the dispersion size grade of the sample C is 5.1, the dispersion size grade of the sample D is 5.1, the dispersion size grade of the sample E is 5.0, and the dispersion size grade of the sample F is 4.9, while the dispersion size grade of the comparison sample is only 3.5, which is lower than that of the samples a to F, it can be seen that the dispersion size grade of the high thermal conductive composite material prepared by the present invention is superior to that of the existing product, and the dispersibility of the thermal conductive filler in the polymer is improved.
TABLE 3 Dispersion Scale test results
| Sample (I) | Grade of dispersed size |
| A | 5.9 |
| B | 5.7 |
| C | 5.1 |
| D | 5.1 |
| E | 5.0 |
| F | 4.9 |
| Control sample | 3.5 |
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (7)
1. The preparation method of the high-thermal-conductivity composite material is characterized by comprising the following steps of:
1) the formula comprises the following components in parts by weight: 0.1-10 parts of heat conduction material, 0.5-2 parts of dispersing agent, 1-5 parts of natural organic high molecular material and 100 parts of polymer powder;
2) adding a heat conduction material, a dispersing agent, a natural organic high polymer material and polymer powder into an aqueous solution according to the proportion in the step 1) for pre-dispersion treatment, and transferring the mixture into an autoclave for heat treatment after the pre-dispersion treatment;
3) drying the solution obtained in the step 2), adding the dried solution into an organic solvent, grinding, and obtaining micron-grade mixed heat-conducting polymer fiber yarns by an electrostatic spinning technology;
4) and 3) carrying out melt extrusion and granulation on the heat-conducting polymer fiber yarns obtained in the step 3) by using a double-screw extruder to obtain the high heat-conducting polymer master batch.
2. The method for preparing a high thermal conductive composite material according to claim 1, wherein the thermal conductive material is one or more of a novel carbon material, a high thermal conductive inorganic non-metallic material, a metal or a metal oxide material; the natural organic high molecular material is one or more of starch, chitosan, cellulose or cyclodextrin; the polymer powder is one or more of polyethylene and polypropylene; the dispersant is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent.
3. The method for preparing a high thermal conductive composite material according to claim 1, wherein the organic solvent in step 3) is N, N dimethylformamide.
4. The preparation method of the high-thermal-conductivity composite material as claimed in claim 1, wherein the grinding fineness of the step 3) is less than or equal to 1 μm, and the diameter of the thermal-conductivity polymer fiber is 5-10 μm.
5. The preparation method of the high thermal conductive composite material as claimed in claim 1, wherein the conditions of the autoclave heat treatment in the step 2) are that the temperature in the autoclave is more than 140 ℃, the pressure is more than 0.2MPa, and the reaction process is continuously stirred.
6. The method for preparing a high thermal conductive composite material according to claim 1, wherein the pre-dispersion treatment in step 2) is ultrasonic dispersion or sand mill dispersion.
7. The method for preparing a high thermal conductive composite material according to claim 1, wherein the drying in step 3) is freeze-drying or spray-drying, and the freeze-drying conditions are as follows: the freeze-drying temperature is maintained at-50-30 ℃, the freeze-drying time is 10-40 h, and the vacuum degree is 1-300 Pa; the spray drying conditions were: the inlet temperature is 100-350 ℃, the outlet temperature is 40-150 ℃, and the drying medium is hot air.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113150400A (en) * | 2021-01-21 | 2021-07-23 | 山东宏建高分子材料科技有限公司 | High-thermal-conductivity rubber material and preparation method thereof |
| CN113149514A (en) * | 2021-04-13 | 2021-07-23 | 南京翌动新材料科技有限公司 | Method for improving mechanical property of ceramic polymer composite material |
| CN114045156A (en) * | 2021-11-29 | 2022-02-15 | 佛山(华南)新材料研究院 | Treatment method of heat-conducting composite material |
| CN114737318A (en) * | 2022-04-18 | 2022-07-12 | 江西昌大高新能源材料技术有限公司 | Preparation method of polyimide-based high-thermal-conductivity graphite nanofiber membrane |
| CN114808183A (en) * | 2022-03-11 | 2022-07-29 | 纳电(深圳)材料科技有限公司 | Electrostatic spinning ink, high-thermal-conductivity fiber membrane and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113150400A (en) * | 2021-01-21 | 2021-07-23 | 山东宏建高分子材料科技有限公司 | High-thermal-conductivity rubber material and preparation method thereof |
| CN113149514A (en) * | 2021-04-13 | 2021-07-23 | 南京翌动新材料科技有限公司 | Method for improving mechanical property of ceramic polymer composite material |
| CN114045156A (en) * | 2021-11-29 | 2022-02-15 | 佛山(华南)新材料研究院 | Treatment method of heat-conducting composite material |
| CN114808183A (en) * | 2022-03-11 | 2022-07-29 | 纳电(深圳)材料科技有限公司 | Electrostatic spinning ink, high-thermal-conductivity fiber membrane and preparation method thereof |
| CN114737318A (en) * | 2022-04-18 | 2022-07-12 | 江西昌大高新能源材料技术有限公司 | Preparation method of polyimide-based high-thermal-conductivity graphite nanofiber membrane |
| CN114737318B (en) * | 2022-04-18 | 2023-11-17 | 江西昌大高新能源材料技术有限公司 | Preparation method of polyimide-based high-heat-conductivity graphite nanofiber membrane |
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