CN112679841A - Anisotropic heat-conducting polypropylene/graphene composite film and preparation method thereof - Google Patents
Anisotropic heat-conducting polypropylene/graphene composite film and preparation method thereof Download PDFInfo
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Abstract
The invention provides an anisotropic heat-conducting polypropylene/graphene composite film and a preparation method thereof. The method comprises the following steps: respectively dissolving graphene and 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol by using a xylene solution, and mixing to obtain a mixed solution A; dissolving polypropylene particles in the mixed solution A, and heating to obtain a mixed solution B; evaporating the mixed solution B to dryness, and then adding the dried mixed solution B into an internal mixer for internal mixing to obtain an internal mixing product; and preparing the banburying product into the anisotropic heat-conducting polypropylene/graphene composite film in a hot pressing mode. The invention also provides the anisotropic heat-conducting polypropylene/graphene composite film prepared by the method. The polypropylene/graphene composite film prepared by the preparation method has anisotropic thermal conductivity and high transverse thermal conductivity, and can dissipate heat in a plane direction in time; meanwhile, the longitudinal thermal conductivity is low, so that the heat source can be protected from being influenced by an adjacent heat source.
Description
Technical Field
The invention relates to a polypropylene/graphene composite film, in particular to an anisotropic heat-conducting polypropylene/graphene composite film.
Background
With increasingly high-density integrated packaging of electronic equipment, effective heat dissipation becomes a key to whether electronic components can normally operate. At present, the materials for packaging in electronic components are mainly plastics, and the thermal conductivity of the plastics is low, so that the heat dissipation requirement of the electronic components cannot be met. The graphene has extremely high thermal conductivity which can be 10 times that of metal copper, and has good compatibility with plastics. The polypropylene has regular structure, corrosion resistance and small density, is the lightest general plastic, has the advantages of low cost, easy processing and the like, and can be used as a matrix of the heat-conducting composite film. Graphene is compounded with polypropylene as a filler, so that the heat conductivity of the compound can be greatly improved, and the compound is further applied to the field of heat conduction and heat dissipation.
The thermal management of modern electronic devices increasingly requires flexible films with anisotropic thermal conductivity that dissipate heat from heat sources in a planar direction while insulating heat from adjacent heat sources in the longitudinal direction and protecting the heat from other adjacent heat sources.
In recent years, in heat conduction research for polypropylene composite materials at home and abroad, for example, in the technical scheme disclosed in CN106928545A, a mixture of polypropylene and graphene is obtained by means of extrusion granulation, the heat conductivity of the mixture can reach 8.6W/Mk, and the heat conduction and heat dissipation performance of the polymer are improved well, but the heat conduction of the composite has no anisotropy, and cannot be applied to electronic packaging materials requiring anisotropic heat dissipation; similarly, in the technical scheme disclosed in CN104629187A, a compound with a thermal conductivity exceeding 5W/Mk is obtained by melt-kneading and granulating polypropylene, inorganic particle heat-conducting filler and other processing aids, and can be applied in the field of heat dissipation of various precision instruments, but the heat dissipation of the compound has no anisotropy, and electronic components cannot be protected from other adjacent heat sources.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide an anisotropic heat-conducting polypropylene/graphene composite film and a preparation method thereof.
In order to achieve the above purpose, the present invention provides a preparation method of an anisotropic heat conduction polypropylene/graphene composite film, which comprises the following steps:
respectively dissolving graphene and 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol by using a xylene solution, and mixing to obtain a mixed solution A;
dissolving polypropylene particles in the mixed solution A, and heating to obtain a mixed solution B;
evaporating the mixed solution B to dryness, and then adding the dried mixed solution B into an internal mixer for internal mixing to obtain an internal mixing product;
and preparing the banburying product into the anisotropic heat-conducting polypropylene/graphene composite film in a hot pressing mode.
In the above preparation method, preferably, the density of the anisotropic heat-conducting polypropylene/graphene composite film prepared by hot-pressing is 0.9-1.0g/cm3。
In the above preparation method, preferably, in the anisotropic thermal conductive polypropylene/graphene composite film, the content of graphene is 10 to 30 wt%.
In the above preparation method, preferably, in the anisotropic thermal conductive polypropylene/graphene composite film, the mass content of 2- (2H-benzothiazol-2-yl) -4, 6-diamyl phenol is 10-20%.
In the above preparation method, preferably, the thickness of the anisotropic thermal conductive polypropylene/graphene composite film is 50 μm to 80 μm.
According to a particular embodiment of the present invention, preferably, the preparation method comprises the following particular steps:
1) dissolving graphene in a proper amount of xylene solution, stirring and ultrasonically dispersing until the graphene is completely dissolved to obtain a graphene solution;
2) dissolving 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol in a proper amount of xylene solution, stirring and ultrasonically dispersing until the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is completely dissolved to obtain a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution; mixing the graphene solution with a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution to obtain a mixed solution A;
3) dissolving polypropylene particles in the mixed solution A, stirring and ultrasonically dispersing until the polypropylene particles are completely dissolved, and then heating to obtain a mixed solution B;
4) after the mixed solution B is evaporated to dryness, adding the obtained solid into an internal mixer for internal mixing to obtain an internal mixing product;
5) and preparing the banburying product into the anisotropic heat-conducting polypropylene/graphene composite film in a hot pressing mode.
In the above preparation method, preferably, the ultrasonic power of the ultrasonic dispersion in step 1) is 80W, and the time is 30-50 min.
In the above preparation method, preferably, the ultrasonic power of the ultrasonic dispersion in step 2) is 80W, and the time is 30-50 min.
In the above preparation method, preferably, the ultrasonic power of the ultrasonic dispersion in step 3) is 80W, and the time is 30min-2 h.
In the above preparation method, preferably, the heating temperature is 125 ℃ and the time is 1-3 h; stirring is preferably carried out during heating. In one embodiment, the heating is carried out at 125 ℃, and after the rod climbing effect appears, the heating is continued for 1 hour.
In the above production method, the temperature at which the mixed solution is evaporated to dryness is preferably 70 ℃, and it is preferably performed using a rotary evaporator.
In the preparation method, the temperature of the internal mixer is preferably 190-220 ℃, and the rotating speed is preferably 40-80 r/min.
In the above preparation method, preferably, the temperature of the hot pressing is 190 ℃ to 220 ℃, and the pressure is 5MPa to 10 MPa; preferably, it is carried out using a press vulcanizer.
In the above production method, xylene does not participate in the reaction, and the concentration of the xylene solution may be selected according to the actual circumstances, for example, from 5mg/mL to 10 mg/mL.
In the preparation method, in the hot pressing process of the polypropylene/graphene composite, the heat-conducting filler graphene is oriented in the composite along the plane direction, and the obtained composite film has high heat conductivity in the transverse direction and low heat conductivity in the longitudinal direction, so that the composite film with the anisotropic heat-conducting function is formed.
According to a specific embodiment of the present invention, the above preparation method may comprise the following specific steps:
1) dissolving 5-20g of graphene in 500mL of dimethylbenzene solution with the concentration of 1mg/mL, stirring and performing ultrasonic treatment until the graphene is completely dissolved to obtain a graphene solution; the ultrasonic power is 80W, and the time is 30-50 min;
2) dissolving 5-20g of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol in 500mL of xylene solution, stirring and carrying out ultrasonic treatment until the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is completely dissolved to obtain a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution; the ultrasonic power is 80W, and the time is 30-50 min; mixing the graphene solution with a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution to obtain a mixed solution A;
3) dissolving 30-50g of polypropylene particles in the mixed solution A, stirring and ultrasonically dispersing until the polypropylene particles are completely dissolved, and then heating at 125 ℃ until a rod climbing effect appears, and continuing heating for 1h to obtain a mixed solution B; the ultrasonic power is 80W, and the time is 30min-2 h; continuously stirring in the heating process;
4) evaporating the mixed solution B to dryness by using a rotary evaporator (the temperature is 70 ℃), adding the obtained solid into an internal mixer (the temperature is 190-220 ℃, and the rotating speed is 40-80r/min), and carrying out internal mixing to obtain an internal mixing product;
5) and (3) placing the banburying product under a steel plate in a flat vulcanizing machine for compression (the temperature is 190-220 ℃, and the pressure is 5-10 MPa), so as to obtain the polypropylene/graphene composite film with anisotropic heat conduction.
The invention also provides an anisotropic heat-conducting polypropylene/graphene composite film which is prepared by the preparation method. Preferably, the transverse thermal conductivity of the anisotropic heat-conducting polypropylene/graphene composite film is 4.00-11.00W/Mk, the longitudinal thermal conductivity is 0.1-1.0W/Mk, and the transverse thermal conductivity is far higher than the longitudinal thermal conductivity.
The anisotropic heat-conducting polypropylene/graphene composite film provided by the invention is a mixed film of polypropylene, graphene and 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol, and is prepared by means of solution blending, banburying and hot pressing. In the process of solution blending and banburying, a small amount of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is used as a conjugated crosslinking agent to modify graphene, the graphene and the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol are firstly connected through pi-pi conjugation, and then are uniformly mixed with polypropylene to form a stable and uniform blending system; in the hot pressing process, the graphene serving as the heat-conducting filler is oriented in the compound along the plane direction to form the composite film with the anisotropic heat-conducting function. The composite film has higher thermal conductivity in the plane direction and lower thermal conductivity in the longitudinal direction, can solve the heat dissipation problem of modern electronic devices, and is applied to electronic components with higher requirements on anisotropic heat dissipation.
Compared with the prior art, the invention has the following outstanding advantages:
(1) the matrix polypropylene adopted by the preparation method has the advantages of small density, good mechanical property, corrosion resistance, easy processing, low cost and the like;
(2) the preparation method is simple to operate, has high efficiency and can realize large-scale production;
(3) the polypropylene/graphene composite film prepared by the preparation method has anisotropic thermal conductivity and high transverse thermal conductivity, and can dissipate heat in a plane direction in time; meanwhile, the longitudinal thermal conductivity is low, so that the heat source can be protected from being influenced by an adjacent heat source.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides a preparation method of an anisotropic heat-conducting polypropylene/graphene composite film, which comprises the following steps:
1) dissolving 5g of graphene in 500mL of xylene solution, stirring and carrying out ultrasonic treatment (with the power of 80W) for 30min until the graphene is completely dissolved to obtain graphene solution;
2) dissolving 5g of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol in 500mL of xylene solution, stirring and carrying out ultrasonic treatment (the power is 80W) for 30min until the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is completely dissolved to obtain a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution; mixing the graphene solution with a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution to obtain a mixed solution A;
3) dissolving 30g of polypropylene particles in the mixed solution A, stirring and carrying out ultrasonic treatment (with the power of 80W) for 30min until the polypropylene particles are completely dissolved, then heating at 125 ℃ for 1h to generate a climbing effect, and then continuing heating for 1h to obtain a mixed solution B; continuously stirring in the heating process;
4) evaporating the mixed solution B to dryness by using a rotary evaporator (the temperature is 70 ℃), and then adding the obtained solid into an internal mixer (the temperature is 190 ℃ and the rotating speed is 40r/min) for internal mixing to obtain an internal mixing product;
5) and (3) placing the banburying product under a steel plate in a flat vulcanizing machine for compression (the temperature is 190 ℃ and the pressure is 5MPa), so as to obtain the anisotropic heat-conducting polypropylene/graphene composite film with the mass fraction of 12.5 wt%, namely the polypropylene/graphene composite film containing 12.5 wt% of graphene. In the polypropylene/graphene composite film, the mass content of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is 12.5%.
The transverse thermal conductivity of the anisotropic thermal conductive polypropylene/graphene composite film is 4.98W/Mk, the longitudinal thermal conductivity of the anisotropic thermal conductive polypropylene/graphene composite film is 0.17W/Mk, and the anisotropic thermal conductive polypropylene/graphene composite film has obvious thermal conductive anisotropy.
Example 2
The embodiment provides a preparation method of an anisotropic heat-conducting polypropylene/graphene composite film, which comprises the following steps:
1) dissolving 10g of graphene in 500mL of xylene solution, stirring and performing ultrasonic treatment (with the power of 80W) for 40min until the graphene is completely dissolved to obtain graphene solution;
2) dissolving 5g of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol in 500mL of xylene solution, stirring and performing ultrasonic treatment (the power is 80W) for 40min until the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is completely dissolved to obtain a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution; mixing the graphene solution with a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution to obtain a mixed solution A;
3) dissolving 35g of polypropylene particles in the mixed solution A, stirring and carrying out ultrasonic treatment (with the power of 80W) for 1h until the polypropylene particles are completely dissolved, then heating at 125 ℃ for 1.5h for generating a rod climbing effect, and then continuing heating for 1h to obtain a mixed solution B; continuously stirring in the heating process;
4) evaporating the mixed solution B to dryness by using a rotary evaporator (the temperature is 70 ℃), adding the obtained solid into an internal mixer (the temperature is 200 ℃, and the rotating speed is 60r/min), and carrying out internal mixing to obtain an internal mixing product;
5) and (3) placing the banburying product under a steel plate in a flat vulcanizing machine for compression (the temperature is 200 ℃, and the pressure is 7MPa), so as to obtain the anisotropic heat-conducting polypropylene/graphene composite film with the mass fraction of 20 wt%, namely the polypropylene/graphene composite film containing 20 wt% of graphene. In the polypropylene/graphene composite film, the mass content of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is 10%.
The transverse thermal conductivity of the anisotropic thermal conductive polypropylene/graphene composite film is 6.32W/Mk, the longitudinal thermal conductivity of the anisotropic thermal conductive polypropylene/graphene composite film is 0.37W/Mk, and the anisotropic thermal conductive polypropylene/graphene composite film has obvious thermal conductive anisotropy.
Example 3
The embodiment provides a preparation method of an anisotropic heat-conducting polypropylene/graphene composite film, which comprises the following steps:
1) dissolving 20g of graphene in 500mL of xylene solution, stirring and carrying out ultrasonic treatment (with the power of 80W) for 50min until the graphene is completely dissolved to obtain graphene solution;
2) dissolving 10g of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol in 500mL of xylene solution, stirring and carrying out ultrasonic treatment (the power is 80W) for 50min until the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is completely dissolved to obtain a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution; mixing the graphene solution with a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution to obtain a mixed solution A;
3) dissolving 50g of polypropylene particles in the mixed solution A, stirring and carrying out ultrasonic treatment (with the power of 80W) for 1.5h until the polypropylene particles are completely dissolved, then heating at 125 ℃ for 2h to generate a rod climbing effect, and then continuing heating for 1h to obtain a mixed solution B; continuously stirring in the heating process;
4) evaporating the mixed solution B to dryness by using a rotary evaporator (the temperature is 70 ℃), adding the obtained solid into an internal mixer (the temperature is 220 ℃, and the rotating speed is 80r/min), and carrying out internal mixing to obtain an internal mixing product;
5) and (3) placing the banburying product under a steel plate in a flat vulcanizing machine for compression (the temperature is 220 ℃ and the pressure is 10MPa), and obtaining the anisotropic heat-conducting polypropylene/graphene composite film with the mass fraction of 25 wt%, namely the polypropylene/graphene composite film containing 25 wt% of graphene. In the polypropylene/graphene composite film, the mass content of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is 12.5%.
The transverse thermal conductivity of the polypropylene/graphene composite film with anisotropic thermal conductivity is 10.02W/Mk, the longitudinal thermal conductivity of the polypropylene/graphene composite film is 0.71W/Mk, and the polypropylene/graphene composite film has obvious thermal conductivity anisotropy.
Claims (11)
1. A preparation method of an anisotropic heat-conducting polypropylene/graphene composite film comprises the following steps:
respectively dissolving graphene and 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol by using a xylene solution, and mixing to obtain a mixed solution A;
dissolving polypropylene particles in the mixed solution A, and heating to obtain a mixed solution B;
evaporating the mixed solution B to dryness, and then adding the dried mixed solution B into an internal mixer for internal mixing to obtain an internal mixing product;
and preparing the banburying product into the anisotropic heat-conducting polypropylene/graphene composite film in a hot pressing mode.
2. The preparation method of claim 1, wherein the density of the anisotropic thermal conductive polypropylene/graphene composite film prepared by the hot pressing method is 0.9-1.0g/cm3。
3. The preparation method according to claim 1, wherein in the anisotropic thermal conductive polypropylene/graphene composite film, the content of graphene is 10-30 wt%;
in the anisotropic heat-conducting polypropylene/graphene composite film, the mass content of 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is 10-20%.
4. The preparation method according to claim 1, wherein the thickness of the anisotropic thermal conductive polypropylene/graphene composite film is 50 μm to 80 μm.
5. The production method according to any one of claims 1 to 4, wherein the production method comprises the steps of:
1) dissolving graphene in a proper amount of xylene solution, stirring and ultrasonically dispersing until the graphene is completely dissolved to obtain a graphene solution;
2) dissolving 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol in a proper amount of xylene solution, stirring and ultrasonically dispersing until the 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol is completely dissolved to obtain a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution; mixing the graphene solution with a 2- (2H-benzothiazole-2-yl) -4, 6-diamyl phenol solution to obtain a mixed solution A;
3) dissolving polypropylene particles in the mixed solution A, stirring and ultrasonically dispersing until the polypropylene particles are completely dissolved, and then heating to obtain a mixed solution B;
4) after the mixed solution B is evaporated to dryness, adding the obtained solid into an internal mixer for internal mixing to obtain an internal mixing product;
5) and preparing the banburying product into the anisotropic heat-conducting polypropylene/graphene composite film in a hot pressing mode.
6. The method of claim 5, wherein,
the ultrasonic power of the ultrasonic dispersion in the step 1) is 80W, and the time is 30-50 min;
the ultrasonic power of the ultrasonic dispersion in the step 2) is 80W, and the time is 30-50 min;
the ultrasonic power of the ultrasonic dispersion in the step 3) is 80W, and the time is 30min-2 h.
7. The method of claim 1 or 5, wherein the heating is at a temperature of 125 ℃ for a time of 1-3 h; stirring is preferably carried out during heating.
8. The process according to claim 1 or 5, wherein the temperature at which the mixed solution B is evaporated to dryness is 70 ℃, preferably by using a rotary evaporator.
9. The process according to claim 1 or 5, wherein the internal mixer has a temperature of 190 ℃ to 220 ℃ and a rotation speed of 40 to 80 r/min.
10. The process according to claim 1 or 5, wherein the hot pressing is at a temperature of 190 ℃ to 220 ℃ and at a pressure of 5MPa to 10 MPa; preferably, it is carried out using a press vulcanizer.
11. An anisotropic heat-conducting polypropylene/graphene composite film prepared by the preparation method of any one of claims 1 to 10;
preferably, the transverse thermal conductivity of the anisotropic heat-conducting polypropylene/graphene composite film is 4.00-11.00W/Mk, the longitudinal thermal conductivity is 0.1-1.0W/Mk, and the transverse thermal conductivity is higher than the longitudinal thermal conductivity.
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Citations (3)
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| CN106893128A (en) * | 2017-02-28 | 2017-06-27 | 上海大学 | Graphene composite heat-conducting film of transparent insulation and preparation method thereof |
| CN107868465A (en) * | 2017-11-30 | 2018-04-03 | 中国科学院合肥物质科学研究院 | A kind of heat conductive insulating composite with anisotropic structure and preparation method thereof |
| US20180105957A1 (en) * | 2012-08-22 | 2018-04-19 | Thuy D. Dang | Process for making composites comprising rigid-rod polymers and graphene nanoparticles |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180105957A1 (en) * | 2012-08-22 | 2018-04-19 | Thuy D. Dang | Process for making composites comprising rigid-rod polymers and graphene nanoparticles |
| CN106893128A (en) * | 2017-02-28 | 2017-06-27 | 上海大学 | Graphene composite heat-conducting film of transparent insulation and preparation method thereof |
| CN107868465A (en) * | 2017-11-30 | 2018-04-03 | 中国科学院合肥物质科学研究院 | A kind of heat conductive insulating composite with anisotropic structure and preparation method thereof |
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