CN113372883A - High-thermal-conductivity composite phase change material based on solvent replacement method and preparation method thereof - Google Patents
High-thermal-conductivity composite phase change material based on solvent replacement method and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-thermal-conductivity composite phase change material based on a solvent replacement method. The composite phase-change material is prepared by carrying out reduction gelation, water washing and freezing on graphene oxide/heat-conducting filler dispersion liquid and then carrying out solvent replacement on water, an organic solvent and the phase-change material for two times. Compared with the existing high-thermal-conductivity composite phase change material, the high-thermal-conductivity composite phase change material has the advantages of high efficiency and environmental protection in a processing mode, and the thermal conductivity of the phase change material can be remarkably improved on the premise of ensuring the enthalpy value of the phase change material. The appearance of the composite phase-change material can greatly reduce the threshold of the industrial production of the high-heat-conductivity composite phase-change material, and promote the application of the high-heat-conductivity phase-change material in the fields of temperature management, energy scheduling and the like.
Description
Technical Field
The invention belongs to the field of energy storage composite materials, and particularly relates to a high-thermal-conductivity composite phase change material based on a solvent replacement method and a preparation method thereof.
Background
Energy storage technologies and temperature management technologies based on phase change materials are gaining more and more attention and application. The phase change material can realize large-capacity latent heat storage and release in the phase change process, namely, a large amount of heat energy is stored or released, and the temperature is basically kept unchanged. At present, organic phase change materials which are used and researched more have the advantages of strong heat storage capacity, good circulation stability and the like, but the inherent low thermal conductivity (generally lower than 1W/m.K) greatly limits the heat exchange rate between the phase change materials and the environment, so that the working efficiency of the organic phase change materials as energy storage materials and temperature management materials is influenced.
In order to solve the problem of low thermal conductivity of the organic phase change material and improve the thermal response performance of the organic phase change material, heat conduction materials such as graphene, expanded graphite, boron nitride and the like can be blended into the organic phase change material to construct a composite phase change material. However, in the composite phase change material, the heat conduction materials have high dispersity and are mutually isolated, which is not beneficial to phonon transmission, so that the improvement of the heat conductivity is limited. The heat conduction materials are constructed into a three-dimensional heat conduction network structure and then introduced into the phase change material, and the effect of improving the thermal conductivity is more prominent than that of directly blending under the condition of the addition amount of the heat conduction materials with the same mass fraction. The composite phase-change material based on the three-dimensional heat conduction structure reported at present is generally prepared by constructing a three-dimensional heat conduction network in advance and then impregnating the phase-change material. In the mode of preparing the three-dimensional heat conduction structure, the modes of chemical vapor deposition, freeze drying and the like consume energy and time, large-scale preparation cost is difficult to control, and how to economically and environmentally prepare the high-heat-conduction composite phase change material is still a big problem to be overcome.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-thermal-conductivity composite phase-change material based on a solvent replacement method so as to solve the problem that the preparation of the high-thermal-conductivity composite phase-change material in the prior art is time-consuming and energy-consuming.
The invention provides a high-thermal-conductivity composite phase-change material based on a solvent replacement method, which is obtained by omitting a drying process in the process of processing a three-dimensional porous heat-conducting network by using heat-conducting filler slurry, replacing water in the three-dimensional porous heat-conducting network by using an organic solvent, then immersing the three-dimensional porous heat-conducting network into a melted phase-change material, and volatilizing the organic solvent.
The heat conducting filler comprises one or more of single-layer graphene, multi-layer graphene, graphene nanosheets, graphene oxide, expanded graphite, flake graphite, carbon nanotubes, boron nitride and aluminum oxide.
The organic solvent comprises one or more of acetone, ethanol and methanol.
The phase-change material comprises one or more of paraffin, polyethylene glycol, phase-change polyalcohol and phase-change polybasic acid.
The invention also provides a preparation method of the high-thermal-conductivity composite phase-change material based on the solvent replacement method, which comprises the following steps:
(1) adding a heat-conducting filler and a reducing agent sodium ascorbate into the graphene oxide dispersion liquid, mixing and stirring for 1h, and preparing a stably-dispersed heat-conducting filler slurry, wherein the mass ratio of the heat-conducting filler to the graphene oxide is 1: 0.1-1: 5, and the mass ratio of the reducing agent sodium ascorbate to the graphene oxide is 1: 0.2-1: 3. And pouring the prepared heat-conducting filler slurry into a mold, and putting the mold into an oven to preserve heat for a period of time for reduction gelation.
(2) And (2) fully washing the gel sample obtained in the step (1) with deionized water to remove residual sodium ascorbate, and then freezing. And then placing the frozen sample into a container containing the organic solvent, wherein the organic solvent is replaced for several times, so that the moisture in the sample is fully replaced.
(3) And (3) completely immersing the sample obtained in the step (2) into the melted phase-change material, heating to a temperature above the boiling point of the organic solvent, taking out the three-dimensional porous heat-conducting structure impregnated with the phase-change material after the organic solvent is completely volatilized, and cooling to room temperature to obtain the high-heat-conductivity composite phase-change material.
The heat conducting filler in the step (1) comprises one or more of graphene, graphene oxide, expanded graphite, flake graphite, carbon nano tubes, boron nitride and aluminum oxide.
The concentration of the graphene oxide dispersion liquid in the step (1) is 0.5-5 wt%.
In the step (1), the reduction gelation temperature is 50-150 ℃, and the reduction gelation time is 0.5-24 h.
The freezing temperature in the step (2) is-190 to-10 ℃, and the freezing time is 0.5 to 24 hours.
The organic solvent in the step (2) comprises one or more of acetone, ethanol and methanol.
The phase-change material in the step (3) comprises one or more of paraffin, polyethylene glycol, phase-change polyalcohol and phase-change polybasic acid.
Advantageous effects
According to the invention, a high-efficiency three-dimensional heat conduction network structure is constructed in the phase-change material in a mode of water-organic solvent-phase-change material stepwise solvent replacement, so that the heat conductivity of the phase-change material is greatly improved. Meanwhile, the method utilizes the temperature condition when the phase-change material is immersed to remove the solvent, and compared with the traditional freeze drying, the method saves the freeze drying process which consumes time and energy, and the evaporated organic solvent can be reused. The preparation method has the advantages of energy conservation, environmental protection and is expected to solve the problem that the high-thermal-conductivity composite phase change material is difficult to prepare on a large scale.
Drawings
Fig. 1 is an optical photograph of the high thermal conductive composite phase change material prepared in example 1 after being placed on a heating stage at 90 ℃ for 10 min.
The specific implementation mode is as follows:
the invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Taking 50.0g of graphene oxide dispersion liquid with the concentration of 0.5 wt%, adding 500mg of heat-conducting filler graphene nanosheet and 0.25g of sodium ascorbate, and stirring at the room temperature and the rotating speed of 1000rpm for 1h to obtain a uniformly mixed suspension. The obtained suspension is poured into a mould and is reduced for 12 hours in an environment with the temperature of 60 ℃ for gelation.
(2) And (2) fully washing the gelled sample obtained in the step (1) with deionized water, and then freezing in a liquid nitrogen (-196 ℃) environment for 15 min. The frozen samples were then immersed in 100ml of acetone and the acetone was changed every 6h, three times.
(3) And (3) completely immersing the sample obtained in the step (2) into the melted paraffin, heating to 90 ℃, taking out the three-dimensional porous heat conduction structure impregnated with the phase change material after no bubbles are generated after the organic solvent is completely volatilized, and cooling to room temperature to obtain the high-heat-conductivity composite phase change material. Wherein the loading amount of the paraffin is 94.5 wt%, the thermal conductivity is 2.3W/m.K, the phase change enthalpy is 205J/g, and the phase change temperature is 42 ℃.
Fig. 1 is an optical photo of the high thermal conductivity composite phase change material prepared based on the solvent replacement method above the melting point, and it can be seen that the composite phase change material prepared by the method has good shape stability and no obvious leakage above the melting point.
Example 2
According to the embodiment 1, the heat-conducting filler graphene nanosheet in the step (1) in the embodiment 1 is changed into the boron nitride nanosheet, the adding amount is changed to 1000mg, and the rest is the same as that in the embodiment 1, so that the high-heat-conducting composite phase-change material is obtained. Wherein the loading amount of the paraffin is 91.2 wt%, the thermal conductivity is 3.6W/m.K, the phase change enthalpy is 200J/g, and the phase change temperature is 41 ℃.
Example 3
According to example 1, the reductive gelation conditions in step (1) of example 1 were changed to 80 ℃ for 8 hours. The rest is the same as the embodiment 1, and the high-thermal-conductivity composite phase-change material is obtained. Wherein the loading amount of the paraffin is 92.8 wt%, the thermal conductivity is 4.6W/m.K, the phase change enthalpy is 201J/g, and the phase change temperature is 41 ℃.
Example 4
The freezing conditions in step (2) of example 1 were changed to-30 ℃ for 2h according to example 1. The rest is the same as the embodiment 1, and the high-thermal-conductivity composite phase-change material is obtained. Wherein the loading amount of the paraffin is 94.8 wt%, the thermal conductivity is 2.7W/m.K, the phase change enthalpy is 205J/g, and the phase change temperature is 41 ℃.
Example 5
The organic solvent of step (2) of example 1 was changed to ethanol according to example 1. The heating temperature in the step (3) is changed to 100 ℃. The rest is the same as the embodiment 1, and the high-thermal-conductivity composite phase-change material is obtained. Wherein the loading amount of the paraffin is 93.5 wt%, the thermal conductivity is 2.5W/m.K, the phase change enthalpy is 201J/g, and the phase change temperature is 41 ℃.
Claims (9)
1. A high-thermal-conductivity composite phase-change material based on a solvent replacement method is characterized in that graphene oxide/thermal-conductivity filler dispersion liquid is subjected to reduction gelation, water washing and freezing and then subjected to solvent replacement twice through a water-organic solvent-phase-change material.
2. The phase-change material as claimed in claim 1, wherein the thermally conductive filler comprises one or more of graphene, graphene oxide, expanded graphite, flake graphite, carbon nanotubes, boron nitride, and aluminum oxide.
3. The phase-change material as claimed in claim 1, wherein the phase-change material comprises one or more of paraffin, polyethylene glycol, phase-change polyol, and phase-change polyacid.
4. A preparation method of a high-thermal-conductivity composite phase change material based on a solvent replacement method comprises the following steps:
(1) adding a heat-conducting filler and a reducing agent sodium ascorbate into the graphene oxide dispersion liquid, mixing and stirring for 1h, and preparing a stably-dispersed heat-conducting filler slurry, wherein the mass ratio of the heat-conducting filler to the graphene oxide is 1: 0.1-1: 5, and the mass ratio of the reducing agent sodium ascorbate to the graphene oxide is 1: 0.2-1: 3. And pouring the prepared heat-conducting filler slurry into a mold, and putting the mold into an oven to preserve heat for a period of time for reduction gelation.
(2) And (2) fully washing the gel sample obtained in the step (1) with deionized water to remove residual sodium ascorbate, and then freezing. And then placing the frozen sample into a container containing the organic solvent, wherein the organic solvent is replaced for several times, so that the moisture in the sample is fully replaced.
(3) And (3) completely immersing the sample obtained in the step (2) into the melted phase-change material, heating to a temperature above the boiling point of the organic solvent, taking out the three-dimensional porous heat-conducting structure impregnated with the phase-change material after the organic solvent is completely volatilized, and cooling to room temperature to obtain the high-heat-conductivity composite phase-change material.
5. The method according to claim 4, wherein the heat conductive filler in step (1) comprises one or more of graphene, graphene oxide, expanded graphite, flake graphite, carbon nanotubes, boron nitride and aluminum oxide.
6. The method according to claim 4, wherein the temperature of the reductive gelation in the step (1) is 50 to 150 ℃ and the reductive gelation time is 0.5 to 24 hours.
7. The method as claimed in claim 4, wherein the freezing temperature in the step (2) is-190 to-10 ℃, and the freezing time is 0.5 to 24 hours.
8. The method according to claim 4, wherein the organic solvent in step (2) comprises one or more of acetone, ethanol and methanol.
9. The method as claimed in claim 4, wherein the phase-change material in step (3) comprises one or more of paraffin, polyethylene glycol, a phase-change polyol, and a phase-change polyacid.
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| CN114316908A (en) * | 2022-01-14 | 2022-04-12 | 青岛理工大学 | Phase-change cooling composite material, preparation method and application thereof |
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