CN110655910A - Preparation method of graphene aerogel phase-change energy storage material - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 238000004146 energy storage Methods 0.000 title claims abstract description 34
- 239000004964 aerogel Substances 0.000 title claims abstract description 33
- 239000011232 storage material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000012782 phase change material Substances 0.000 claims abstract description 23
- 230000008859 change Effects 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000011240 wet gel Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000012188 paraffin wax Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000000352 supercritical drying Methods 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 229920000098 polyolefin Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000007783 nanoporous material Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 16
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 8
- 235000021314 Palmitic acid Nutrition 0.000 description 4
- 230000004927 fusion Effects 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004134 energy conservation Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002149 hierarchical pore Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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Abstract
The invention belongs to the field of nano porous materials, and relates to a preparation method of a graphene aerogel phase change energy storage material. The method comprises the steps of mixing graphene oxide powder with a solvent, adding a phase-change material, obtaining wet gel by a hydrothermal reduction method, and finally washing, drying and the like to finally prepare the phase-change energy storage material which takes the graphene aerogel as a structural framework and is uniformly distributed with the phase-change material. The invention has the advantages of simple preparation process, better leakage resistance, high latent heat and high heat conductivity, and the like, and is easy to realize mass production.
Description
Technical Field
The invention relates to a preparation method of a novel graphene aerogel phase-change energy storage material, in particular to a preparation method of a graphene aerogel phase-change energy storage material, and belongs to the technical field of nano porous materials and phase-change energy storage.
Background
With the rapid development of society and economy, people have more and more demands on heat energy in the fields of heating and heat preservation, food drying, domestic hot water and the like, but redundant heat in the processes of life and production is often regarded as waste heat to be discharged to the external environment. Energy conservation and environmental protection are one of the basic national policies of China, have important effects on social development and progress, and are particularly important for improving the utilization rate of heat energy.
Phase change energy storage is the most popular energy storage mode at present, namely, the phase change material still has extremely high phase change latent heat and a wider phase change temperature selection range under the condition of small temperature change. When the temperature rises to be close to the melting point temperature of the phase-change material, the phase-change material can absorb heat to perform solid-liquid phase transformation to achieve the effect of energy storage, and the ambient temperature is reduced. The phase change energy storage material can be used in the fields of spaceflight, buildings, clothes, refrigeration equipment, military, communication, electric power and the like, and can realize energy storage, building energy conservation and temperature regulation. However, the phase change material has three main problems in the using process: the degradation problem of thermophysical properties in the circulation process, the problem of easy leakage of the phase-change material from the matrix and the problem of the effect of the phase-change material on the matrix material. Therefore, it is necessary to find a porous matrix which does not react with the phase change material, can well encapsulate the phase change material and has stable enthalpy of phase change.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a graphene aerogel phase-change energy storage material so as to improve the current situation of low heat energy utilization rate and overcome some technical problems.
The technical scheme adopted by the invention is as follows: a preparation method of a graphene aerogel phase change energy storage material comprises the following specific steps:
(1) mixing graphene oxide powder and a solvent, and stirring to form a uniform graphene oxide solution;
(2) adding a phase change material into the graphene oxide solution formed in the step (1), and stirring for 1-10 min;
(3) pouring the mixed system formed in the step (2) into a polytetrafluoroethylene hydrothermal reaction kettle, and reacting at the temperature of 90-240 ℃ for 5-20 hours to obtain graphene phase change energy storage wet gel;
(4) replacing the wet gel obtained in the step (3) with a solvent;
(5) and (5) drying the wet gel obtained in the step (4) to finally obtain the graphene aerogel phase change energy storage material.
Wherein the mass ratio of the graphene oxide to the solvent in the step (1) is (1-20): 1000, and the mass ratio of the phase-change material to the graphene oxide added in the step (2) is (10-100): 1.
preferably, the solvent in step (1) and step (4) is one or a mixture of deionized water, ethanol, acetone, isopropanol or sec-butanol.
Preferably, the phase change material in step (2) is any one or a combination of two or more of paraffin, polyethylene glycol, fatty acid, aromatic hydrocarbon, polyolefin, polyamide or polymeric polyol.
Preferably, the replacing times in the step (4) are 3-9 times, and the standing time is 8-24 hours each time.
Preferably, the drying treatment in the step (5) is carbon dioxide supercritical drying and freeze drying; carbon dioxide is used as a drying medium for supercritical drying of carbon dioxide, the reaction temperature is 50-70 ℃, the pressure in a high-pressure reaction kettle is 8-12 MPa, the air release rate is 5-20L/min, and the drying time is 8-20 h; freeze drying at-20 to-80 deg.c for 5-48 hr, and vacuum drying for 12-36 hr.
The prepared graphene aerogel phase change energy storage material comprises graphene aerogel and a phase change material, wherein the graphene aerogel is formed by carrying out hydrothermal reduction on a Graphene Oxide (GO) sheet layer to form an rGO sheet layer, then a three-dimensional space network structure is assembled by two-dimensional rGO, and the phase change material is uniformly distributed in the three-dimensional space network structure.
The graphene aerogel phase-change energy storage material can be used in the fields of aerospace, buildings, clothes, refrigeration equipment, military, communication, electric power and the like, and can realize energy storage, building energy conservation and temperature regulation.
Has the advantages that:
the method and the graphene aerogel phase change energy storage material prepared by the method have the following characteristics:
(1) high latent heat and high thermal conductivity. Graphene is used as a stable carbon material, no chemical action exists between the graphene and a phase-change material, and phase-change coating is carried out only by means of capillary force of graphene aerogel, so that the phase-change material can keep the characteristic of high enthalpy change, and meanwhile, the high heat conduction of the graphene well improves the phase-change response rate.
(2) Better leakage-proof performance. The pore diameter of the graphene aerogel in the graphene aerogel phase-change energy storage material is formed by microporous-mesoporous-macroporous hierarchical pores, so that the graphene aerogel phase-change energy storage material has excellent adsorption performance and can effectively prevent the phase-change material from melting and leaking.
Drawings
Fig. 1 is a photograph of a graphene aerogel polyethylene glycol phase change energy storage material prepared in example 1;
fig. 2 is SEM images of graphene aerogel paraffin phase-change energy storage material prepared in example 3 at different times;
fig. 3 is a DSC curve before and after cycling of the graphene aerogel palmitic acid phase change energy storage material prepared in example 4.
Detailed Description
Example 1
Uniformly mixing and stirring graphene oxide and deionized water according to the mass ratio of 1:1000, then adding polyethylene glycol with the mass ratio of 10:1 to the graphene oxide, stirring for 1min, pouring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat at 90 ℃ for 20 hours, taking out a sample, replacing the sample with the deionized water for 3 times, standing for 24 hours each time, then freezing for 5 hours at-20 ℃, vacuumizing and drying for 12 hours to obtain the final graphene aerogel polyethylene glycol phase change energy storage material. The sample diagram is shown in fig. 1, it can be seen from the diagram that the surface of the sample is relatively smooth, the overall color is shown as black of the graphene aerogel, and the white polyethylene glycol phase-change material is well filled in the porous skeleton of the graphene aerogel; the density of the sample was 0.16g/cm3The enthalpy of fusion was 127.6J/g.
Example 2
Uniformly mixing and stirring graphene oxide and ethanol according to the mass ratio of 20:1000, then adding stearic acid with the mass ratio of 100:1 to the graphene oxide, stirring for 10min, pouring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat for 5 hours at 240 ℃, taking out a sample, and performing deionized water treatment on the sampleAnd (3) replacing for 9 times, standing for 8h each time, freezing for 48h in an environment of-80 ℃, vacuumizing, and drying for 36h to obtain the final graphene aerogel stearic acid phase change energy storage material. The density of the sample was 0.36g/cm3The enthalpy of fusion is 346.7J/g.
Example 3
Uniformly mixing and stirring graphene oxide and acetone according to the mass ratio of 16:1000, then adding paraffin wax with the mass ratio of 50:1 to the graphene oxide, stirring for 10min, pouring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat for 9 hours at 240 ℃, taking out a sample, replacing the sample with ethanol for 9 times, and standing for 8 hours each time. And then placing the graphene aerogel paraffin phase-change energy storage material in a CO2 supercritical reaction kettle, and drying for 8 hours in a high-pressure reaction kettle with the reaction temperature of 70 ℃, the pressure of 8MPa and the air release rate of 5L/min, thereby obtaining the final graphene aerogel paraffin phase-change energy storage material. The density of the sample was 0.26g/cm3The SEM picture is as shown in fig. 2, the left image shows the lamellar network structure of the graphene aerogel, and the right image shows that the paraffin phase change material is better filled into the skeleton of the graphene aerogel; the enthalpy of fusion was 236.7J/g.
Example 4
Uniformly mixing and stirring graphene oxide and isopropanol according to the mass ratio of 7:1000, then adding palmitic acid with the mass ratio of 40:1 to the graphene oxide, stirring for 10min, pouring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat for 13 hours at 90 ℃, taking out a sample, replacing the sample with ethanol for 3 times, and standing for 12 hours each time. Then it is placed in CO2And (3) drying the graphene aerogel palmitic acid phase change energy storage material in a supercritical reaction kettle for 20 hours in a high-pressure reaction kettle with the reaction temperature of 50 ℃, the pressure of 12MPa and the air release rate of 20L/min, thereby obtaining the final graphene aerogel palmitic acid phase change energy storage material. The density of the sample was 0.21g/cm3The cycle DSC curve of the melting and solidification process is shown in FIG. 3, from which it can be seen that the melting enthalpy before the cycle test is 139.4J/g, and the solidification enthalpy is 175.7J/g; the enthalpy of fusion remained unchanged after the cycling test, and was still 139.4J/g, while the enthalpy of solidification decreased to 149.0J/g.
Claims (5)
1. A preparation method of a graphene aerogel phase change energy storage material comprises the following specific steps:
(1) mixing graphene oxide powder and a solvent, and stirring to form a uniform graphene oxide solution;
(2) adding a phase change material into the graphene oxide solution formed in the step (1), and stirring for 1-10 min;
(3) pouring the mixed system formed in the step (2) into a polytetrafluoroethylene hydrothermal reaction kettle, and reacting at the temperature of 90-240 ℃ for 5-20 hours to obtain graphene phase change energy storage wet gel;
(4) replacing the wet gel obtained in the step (3) with a solvent;
(5) and (5) drying the wet gel obtained in the step (4) to finally obtain the graphene aerogel phase change energy storage material.
Wherein the mass ratio of the graphene oxide to the solvent in the step (1) is (1-20): 1000, and the mass ratio of the phase-change material to the graphene oxide added in the step (2) is (10-100): 1.
2. the preparation method according to claim 1, wherein the solvent in step (1) and step (4) is one or a mixture of deionized water, ethanol, acetone, isopropanol or sec-butanol.
3. The method according to claim 1, wherein the phase-change material in step (2) is any one or a combination of two or more of paraffin, polyethylene glycol, fatty acid, aromatic hydrocarbon, polyolefin, polyamide, and polymeric polyol.
4. The preparation method according to claim 1, wherein the number of times of replacement in the step (4) is 3-9, and each standing time is 8-24 hours.
5. The production method according to claim 1, wherein the drying treatment in the step (5) is carbon dioxide supercritical drying and freeze-drying; carbon dioxide is used as a drying medium for supercritical drying of carbon dioxide, the reaction temperature is 50-70 ℃, the pressure in a high-pressure reaction kettle is 8-12 MPa, the air release rate is 5-20L/min, and the drying time is 8-20 h; freeze drying at-20 to-80 deg.c for 5-48 hr, and vacuum drying for 12-36 hr.
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| CN112536004A (en) * | 2020-12-03 | 2021-03-23 | 航天特种材料及工艺技术研究所 | High-temperature-resistant elastic graphene aerogel material and preparation method thereof |
| CN112680195A (en) * | 2020-12-24 | 2021-04-20 | 广东工业大学 | Preparation method and device of graphene-based polyethylene glycol phase-change material |
| CN112724936A (en) * | 2021-01-26 | 2021-04-30 | 山西万家暖节能科技有限公司 | Preparation method of new energy storage material |
| CN113265228A (en) * | 2021-04-26 | 2021-08-17 | 西南交通大学 | Multi-energy-driven shape-stabilized phase change material and preparation method thereof |
| CN113527825A (en) * | 2020-04-13 | 2021-10-22 | 中国科学院大连化学物理研究所 | Graphene-based flexible composite shaped phase-change material film and preparation and application thereof |
| CN113583634A (en) * | 2021-07-22 | 2021-11-02 | 南通强生石墨烯科技有限公司 | Intelligent graphene temperature-sensing phase change fiber |
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| CN114525112A (en) * | 2022-02-28 | 2022-05-24 | 重庆大学 | Improved graphene aerogel and polyethylene glycol composite phase change material and preparation method thereof |
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| CN113527825A (en) * | 2020-04-13 | 2021-10-22 | 中国科学院大连化学物理研究所 | Graphene-based flexible composite shaped phase-change material film and preparation and application thereof |
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| CN113698915A (en) * | 2020-05-22 | 2021-11-26 | 中国科学院大连化学物理研究所 | Graphene-based multi-response shaped composite phase change material and preparation and application thereof |
| CN112536004A (en) * | 2020-12-03 | 2021-03-23 | 航天特种材料及工艺技术研究所 | High-temperature-resistant elastic graphene aerogel material and preparation method thereof |
| CN112680195A (en) * | 2020-12-24 | 2021-04-20 | 广东工业大学 | Preparation method and device of graphene-based polyethylene glycol phase-change material |
| US11339316B1 (en) | 2020-12-24 | 2022-05-24 | Guangdong University Of Technology | Method and device for preparing graphene-based polyethylene glycol phase change material |
| CN112724936A (en) * | 2021-01-26 | 2021-04-30 | 山西万家暖节能科技有限公司 | Preparation method of new energy storage material |
| CN113265228A (en) * | 2021-04-26 | 2021-08-17 | 西南交通大学 | Multi-energy-driven shape-stabilized phase change material and preparation method thereof |
| CN113583634A (en) * | 2021-07-22 | 2021-11-02 | 南通强生石墨烯科技有限公司 | Intelligent graphene temperature-sensing phase change fiber |
| CN114525112A (en) * | 2022-02-28 | 2022-05-24 | 重庆大学 | Improved graphene aerogel and polyethylene glycol composite phase change material and preparation method thereof |
| CN114525112B (en) * | 2022-02-28 | 2024-01-05 | 重庆大学 | Improved graphene aerogel and polyethylene glycol composite phase change material and preparation method thereof |
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