CN114231256B - Magnetic high graphitization carbon-based photo-thermal composite phase change material and application thereof - Google Patents
Magnetic high graphitization carbon-based photo-thermal composite phase change material and application thereof Download PDFInfo
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- 239000012782 phase change material Substances 0.000 title claims abstract description 107
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000005087 graphitization Methods 0.000 title abstract description 14
- 239000006249 magnetic particle Substances 0.000 claims abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 27
- 239000010941 cobalt Substances 0.000 claims abstract description 27
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 238000010000 carbonizing Methods 0.000 claims abstract description 3
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 36
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 238000003763 carbonization Methods 0.000 claims description 17
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 16
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000013110 organic ligand Substances 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- ZYURHZPYMFLWSH-UHFFFAOYSA-N octacosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC ZYURHZPYMFLWSH-UHFFFAOYSA-N 0.000 claims description 4
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 claims description 4
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 3
- 238000005338 heat storage Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- 229940038384 octadecane Drugs 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims 1
- 229920005862 polyol Polymers 0.000 claims 1
- 150000003077 polyols Chemical class 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 30
- 238000002360 preparation method Methods 0.000 description 19
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 5
- 239000003599 detergent Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000031700 light absorption Effects 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000003446 ligand Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000002135 phase contrast microscopy Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 208000032825 Ring chromosome 2 syndrome Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- GDUDPOLSCZNKMK-UHFFFAOYSA-L cobalt(2+);diacetate;hydrate Chemical compound O.[Co+2].CC([O-])=O.CC([O-])=O GDUDPOLSCZNKMK-UHFFFAOYSA-L 0.000 description 1
- XZXAIFLKPKVPLO-UHFFFAOYSA-N cobalt(2+);dinitrate;hydrate Chemical compound O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XZXAIFLKPKVPLO-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 239000002803 fossil fuel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000002149 hierarchical pore Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The embodiment of the invention relates to the field of phase change materials, in particular to a magnetic high graphitization carbon-based photo-thermal composite phase change material and application thereof. The magnetic high graphitized porous carbon is a carbon material which is obtained by carbonizing a metal organic framework at high temperature and is highly uniformly dispersed with magnetic particles, the magnetic particles are one or more of iron, nickel and cobalt magnetic particles, and the magnetic particles account for 20% -50% of the total weight of the magnetic high graphitized porous carbon. According to the invention, the phase change material is packaged by taking the magnetic graphitized carbon as a base material, the graphitization degree of the magnetic graphitized carbon is high, the ultra-high dispersion magnetic particles can further improve the photo-thermal conversion capability of the composite phase change material through the Surface Plasmon Resonance (SPR) effect, and can also serve as a heat conduction node and a heterogeneous nucleation site, so that the heat conduction of the material is improved, and the crystallization capability of the phase change material in a three-dimensional carbon carrier structure is regulated.
Description
Technical Field
The invention relates to the field of phase change materials, in particular to a magnetic high graphitization carbon-based photo-thermal composite phase change material and application thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
With the development of low-carbon industry and the reduction of fossil fuel resources, solar energy is receiving increasing attention as an environment-friendly energy source. Latent heat storage systems (TES) based on organic phase change materials have large energy storage capacities, near constant phase change temperatures and reversible charge and discharge processes, exhibiting great potential in solar thermal storage. However, the organic phase-change material has the disadvantages of poor light absorption, low heat conductivity, easy leakage and the like, which limits the wide application.
Porous carbon materials are receiving much attention as carriers for phase change materials. For example, patent CN104710965A discloses a method for preparing a hierarchical pore carbon-based composite phase change material. Patent CN112391149a discloses a preparation method of carbonized wood-based composite phase change energy storage material. Although the preparation methods can adjust the porous material structure to a certain extent and solve the leakage problem of the phase change material, the functions of the metal material and the adjusting and reinforcing functions of the metal material on the carbon structure are ignored, the used carbon material has single function, and the preparation method is complex and limits the application of the carbon material.
Disclosure of Invention
Object of the Invention
In order to solve the technical problems, the invention aims to provide the magnetic high graphitization carbon-based photo-thermal composite phase change material and the application thereof, the composite phase change material of the invention takes magnetic graphitization carbon as a substrate to encapsulate the phase change material, the graphitization degree of the magnetic graphitization carbon is high, the ultra-high dispersion magnetic particles can further improve the photo-thermal conversion capability of the composite phase change material through the Surface Plasmon Resonance (SPR) effect, and the composite phase change material can also be used as a heat conduction node and a heterogeneous nucleation site, so that the heat conduction of the material and the crystallization capability of the phase change material in a 3D carrier structure are improved, and the road is widened for the multi-dimensional application of the composite phase change material.
Solution scheme
In order to achieve the purpose of the invention, the embodiment of the invention provides a magnetic highly graphitized carbon-based photo-thermal composite phase change material, which comprises magnetic highly graphitized porous carbon and phase change materials adsorbed on the surface and/or in pore channels of the magnetic highly graphitized porous carbon, wherein the magnetic highly graphitized porous carbon is a carbon material which is obtained by carbonizing a metal organic framework at a high temperature and is highly uniformly dispersed with magnetic particles, the magnetic particles are one or more of iron, nickel and cobalt magnetic particles, and the magnetic particles account for 20% -50% of the total weight of the magnetic highly graphitized porous carbon.
Further, in the photo-thermal composite phase-change material, the mass ratio of the magnetic highly graphitized porous carbon to the phase-change material is 3:7-5:5, optionally 3:7-4:6, and preferably 4:6.
Further, the magnetic particles account for 24% -50% of the total weight of the magnetic highly graphitized porous carbon, alternatively 30% -46% of the total weight of the magnetic highly graphitized porous carbon, alternatively 34% -46%; optionally 40% -46%.
Further, I D/IG.ltoreq.1, optionally I D/IG.ltoreq.0.95, optionally I D/IG.ltoreq.0.9, preferably I D/IG.ltoreq.0.85 in the magnetic highly graphitized porous carbon.
Further, the magnetic particles are selected from one or more of elementary iron, elementary nickel and elementary cobalt magnetic particles.
Further, the magnetic particles are highly homogeneously distributed in the carbon material.
Further, the phase change material is a solid-liquid phase change material, and is optionally selected from one or more of a polyalcohol phase change material, an alkane phase change material, a fatty alcohol phase change material and a fatty acid phase change material;
optionally, the polyalcohol phase-change material is selected from one or more of polyethylene glycol and pentaerythritol;
Optionally, the fatty alcohol phase-change material is one or more selected from dodecanol, tetradecanol, hexadecanol and octadecanol;
optionally, the alkane phase change material is selected from one or more of tetradecane, hexadecane, octadecane, eicosane and octacosane;
optionally, the fatty acid phase change material is one or more of dodecanoic acid, tetradecanoic acid, hexadecanoic acid and octadecanoic acid.
Further, the metal organic framework is obtained by reacting metal acetate with an organic ligand; optionally, the metal acetate is selected from one or more of ferric acetate and its hydrated salt, nickel acetate and its hydrated salt, cobalt acetate and its hydrated salt.
Further, the molar ratio of the organic ligand to the metal acetate is 3:1-3, alternatively 3:2-5, alternatively 3:2-4, alternatively 3:3-4, preferably 3:3.
Further, the preparation method of the metal organic framework comprises the following steps: dissolving hydrated metal acetate and an organic ligand in a solvent, stirring, collecting precipitate, washing and drying to obtain a metal organic framework; optionally, the stirring time is 6-12 hours.
Further, the solvent is N, N-dimethylformamide or dimethyl sulfoxide.
Further, the organic ligand is terephthalic acid.
Further, the compounding process of the photo-thermal composite phase change material comprises the following steps: adding the magnetic highly graphitized porous carbon and the phase change material into a solvent, performing ultrasonic treatment, and drying to obtain the composite phase change material.
Further, the ultrasonic time is 10-30 min.
Further, the drying temperature is 60-80 ℃, the drying time is 2-24h, and optionally, the drying time is 6-24 h.
Further, the high temperature carbonization conditions are as follows: raising the temperature to carbonization temperature at a heating rate of 2-8 ℃/min under the inert gas atmosphere; and maintaining the carbonization temperature for 1-6 h, and cooling to obtain the carbon material.
Further preferably, the rate of temperature increase is 5 ℃/min.
Further, the carbonization temperature is 800-1000 ℃; preferably the carbonization temperature is 1000 ℃.
Further, the carbonization temperature is maintained for 2 to 4 hours, preferably 3 hours.
Further, the inert gas is nitrogen or argon, preferably nitrogen.
On the other hand, the application of the magnetic highly graphitized carbon-based photo-thermal composite phase change material is provided, and the magnetic highly graphitized carbon-based photo-thermal composite phase change material is used as a photo-thermal conversion material, and is optionally used in the field of solar heat storage.
Advantageous effects
(1) The composite phase change material provided by the invention has the advantages that the phase change material is packaged by taking the magnetic graphitized carbon as a base material, the graphitization degree of the magnetic graphitized carbon is high, the superhigh dispersion magnetic particles can further improve the photo-thermal conversion capability of the composite phase change material through the Surface Plasmon Resonance (SPR) effect, the composite phase change material can also be used as a heat conduction node and a heterogeneous nucleation site, the heat conduction of the material and the crystallization capability of the phase change material in a 3D carrier structure are improved, and the road is widened for multi-dimensional application of the composite phase change material.
(2) The magnetic graphitized carbon of the present invention is obtained by directly calcining a magnetic metal organic framework to derive a highly graphitized 3D carbon structure with highly dispersed magnetic particles in situ. The high graphitized carbon with excellent light absorption capacity is used as a photon capturing agent, and the high graphitized carbon and uniformly dispersed magnetic metal ions are used as a nano heater to cooperatively enhance the stability and the light-heat conversion capacity of the composite phase change material, so that the prepared composite phase change material has high latent heat, strong stability and excellent light-heat conversion capacity, can meet the requirements of different scenes, and provides a new thought for the design and construction of the composite phase change material.
(3) In the calcining process of the metal organic framework, magnetic metal particles (iron/cobalt/nickel) can be reduced into a simple substance form in situ in the metal organic framework lattice, and further catalyze graphitization of carbon, and uniformly distributed magnetic graphitized carbon powder is obtained; the octadecanol with higher melting enthalpy value is used as a phase change material, the magnetic graphitized carbon powder is used as a carrier, and the phase change material is loaded in the 3D graphitized carbon for compounding by capillary action of holes to obtain the magnetic graphitized carbon-based composite phase change material, so that the prepared composite phase change material has high latent heat, strong stability and excellent photothermal conversion capability.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings. The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
FIG. 1 is a drawing of a magnetic graphitized carbon Scanning Electron Microscope (SEM) used in examples 1-3 of the present invention;
FIG. 2 is an X-ray diffraction (XRD) pattern and a Raman spectrum pattern of the magnetic graphitized carbon used in examples 1 to 3 of the present invention; where a is the X-ray diffraction (XRD) pattern and b is the raman spectrum.
FIG. 3 is an X-ray diffraction (XRD) and thermogravimetric analysis (TGA) pattern of the magnetic graphitized carbon and corresponding composite phase change materials used in example 1 of the present invention; where a is the X-ray diffraction (XRD) pattern and b is the thermogravimetric analysis (TGA) pattern.
FIG. 4 is a graph of photo-thermal conversion temperature versus time and a graph of photo-thermal conversion efficiency for three composite phase change materials according to embodiments 1-3 of the present invention; wherein a is a photo-thermal conversion temperature-time graph, and b is a photo-thermal conversion temperature-time graph.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
In addition, numerous specific details are set forth in the following description in order to provide a better illustration of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, elements, methods, means, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.
In the examples described below, the starting materials used were all commercially available materials.
In the following examples, the photo-thermal conversion efficiency of the composite phase change material is calculated by the following formula (I):
Wherein m is the mass of the sample, delta H is the enthalpy value of the sample, P is the intensity of sunlight simulated by the experiment, and T s and T f are the phase change starting time and the phase change-ending time when the illumination is heated.
In the following examples, the calculation formula of the load amount of the Phase Change Material (PCMs) is as follows: the loading of pcms= [ mass of PCMs/(mass of pcms+mass of magnetic graphitized carbon support material) ]x100%.
In the following examples, the method for calculating the cobalt content in the magnetic graphitized carbon is ω=k 1 × (relative atomic mass of cobalt)/k 1 (relative atomic mass of cobalt) +k 2 × (relative molecular mass of benzene ring-2), where k 1 is the mole number of cobalt, and the mole number of k 2 terephthalic acid is obtained according to the coordination principle and the reaction characteristic of the organic molecule at high temperature, although the theoretical calculation value deviates from the actual detection value to some extent, the deviation is not large, because cobalt belongs to a high boiling point simple substance, is not easily evaporated at carbonization temperature, and it is known that cobalt in the magnetic graphitized carbon is a simple substance and remains stable in thermal weight (almost no material loss at 900-1000 ℃ and indicates that cobalt exists stably in a simple substance form) by combining the X-ray diffraction (XRD) patterns, raman spectrograms and thermograms of fig. 2 and 3, so that the theoretical calculation value can be used as a reference value of the actual content of cobalt in a reasonable range, and the cobalt content in a product can be approximately characterized.
Example 1
(1) Preparation of cobalt MOF
3Mmol of terephthalic acid and 3mmol of cobalt acetate tetrahydrate are dissolved in 25ml of dimethyl sulfoxide, stirred at room temperature for 12h, washed three times with N, N-dimethylformamide and ethanol respectively as detergents and dried in a vacuum oven at 60℃for 24h.
(2) Preparation of magnetic graphitized carbon
And (3) heating the MOF powder obtained in the step (1) to 1000 ℃ at a heating rate of 5 ℃/min in a tube furnace under a nitrogen atmosphere, and preserving the temperature for 3 hours at 1000 ℃, so that the finally obtained product is the magnetic graphitized carbon 1.
(3) Preparation of magnetic graphitized carbon-based composite phase change material
Dissolving 0.6g of stearyl alcohol and 0.4g of magnetic graphitized carbon in the step (2) in 15ml of ethanol, carrying out ultrasonic treatment for 20min to dissolve the stearyl alcohol, uniformly mixing, putting the uniform mixed solution into an oven at 80 ℃, preserving heat for 6h to completely volatilize the ethanol, and obtaining a solid, namely the composite phase-change material 1.
Example 2
(1) Preparation of cobalt MOF
3Mmol of terephthalic acid and 2mmol of cobalt acetate tetrahydrate are dissolved in 25ml of dimethyl sulfoxide, stirred at room temperature for 12h, washed three times with N, N-dimethylformamide and ethanol respectively as detergents and dried in a vacuum oven at 60℃for 24h.
(2) Preparation of magnetic graphitized carbon
And (3) heating the MOF powder obtained in the step (1) to 1000 ℃ at a heating rate of 5 ℃/min in a tube furnace under a nitrogen atmosphere, and preserving the temperature for 3 hours at 1000 ℃, so that the finally obtained product is the magnetic graphitized carbon 2.
(3) Preparation of magnetic graphitized carbon-based composite phase change material
Dissolving 0.6g of stearyl alcohol and 0.4g of the magnetic graphitized carbon in the step (2) in 15ml of ethanol, carrying out ultrasonic treatment for 20min to dissolve the stearyl alcohol, uniformly mixing, putting the uniform mixed solution into an oven at 80 ℃, preserving heat for 6h to completely volatilize the ethanol, and obtaining a solid, namely the composite phase-change material 2.
The load capacity of the phase change material in the composite phase change material of the embodiment is 60% and the photo-thermal conversion capacity is 83.4%.
Example 3
(1) Preparation of cobalt MOF
3Mmol of terephthalic acid and 1mmol of cobalt acetate tetrahydrate are dissolved in 25ml of dimethyl sulfoxide, stirred at room temperature for 12h, washed three times with N, N-dimethylformamide and ethanol respectively as detergents and dried in a vacuum oven at 60℃for 24h.
(2) Preparation of magnetic graphitized carbon
And (3) heating the MOF powder obtained in the step (1) to 1000 ℃ at a heating rate of 5 ℃/min in a tube furnace under a nitrogen atmosphere, and preserving the temperature for 3 hours at 1000 ℃, so that the finally obtained product is the magnetic graphitized carbon 3.
(3) Preparation of magnetic graphitized carbon-based composite phase change material
Dissolving 0.6g of stearyl alcohol and 0.4g of the magnetic graphitized carbon in the step (2) in 15ml of ethanol, carrying out ultrasonic treatment for 20min to dissolve the stearyl alcohol, uniformly mixing, putting the uniform mixed solution into an oven at 80 ℃, preserving heat for 6h to completely volatilize the ethanol, and obtaining a solid, namely the composite phase-change material 3.
The load capacity of the phase change material in the composite phase change material of the embodiment is 60% and the photo-thermal conversion capacity is 81.3%.
The magnetic graphitized carbon and the composite phase change material obtained in examples 1,2 and 3 were subjected to the following characterization, and the results are shown in fig. 1 to 4.
As can be seen from fig. 1, the reduced magnetic particles are uniformly distributed on graphitized carbon, and the ultra-high dispersion of the magnetic particles can make the sample generate heat more uniformly.
As can be seen from fig. 2 (a), the XRD diffraction peak positions of the magnetic graphitized carbon 1, 2, 3 are consistent with the standard diffraction pattern of the cobalt simple substance, which indicates that the metal ions are reduced to the metal simple substance by high temperature calcination, and the intensity of the XRD peak positions is gradually increased, which indicates the increase of the cobalt content; as can be seen from the raman analysis result of fig. 2 (b), as the cobalt content increases, the I D/IG value gradually decreases, indicating that the graphitization degree increases, and the high graphitization degree contributes to the improvement of the photo-thermal conversion efficiency. The theoretical calculated values of the cobalt content in the magnetic graphitized carbon 1, 2 and 3 are about 44%, 34% and 21%, respectively.
As can be seen from fig. 3 (a), the diffraction pattern of the composite phase change material 1 is a simple superposition of the magnetic graphitized carbon and the stearyl alcohol diffraction pattern, no new phase is generated, which indicates that the combination between the carrier and the phase change material is a physical effect, and the combination can effectively avoid the leakage of the phase change material. The thermogravimetric curve in fig. 3 (b) shows that the decomposition of stearyl alcohol starts from about 200 ℃ and ends at 400 ℃, while the decomposition interval of the composite phase change material 1 is 220 ℃ to 410 ℃ and the initial decomposition temperature is higher than that of stearyl alcohol, which proves that the magnetic graphitized carbon carrier improves the thermal stability of stearyl alcohol and the specific gravity of stearyl alcohol in the composite phase change material 1 is about 60% (which is the maximum load of the magnetic graphitized carbon 1). Wherein, the magnetic graphitized carbon has excellent thermal stability below 900 ℃, and can be used as an excellent thermal stability phase change carrier material to improve the leakage problem.
Fig. 4 shows temperature-time curves and efficiency histograms of three composite phase change materials under simulated sunlight, the efficiency of the composite phase change materials is improved with the increase of cobalt content, and the photo-thermal conversion efficiencies of the composite phase change materials 1,2 and 3 obtained in examples 1,2 and 3 are 87.7%,83.4% and 81.3%, respectively, which illustrates that the increase of cobalt content is advantageous to improve the photo-thermal conversion capability to some extent.
Example 4
(1) Preparation of cobalt MOF
3Mmol of terephthalic acid and 3mmol of cobalt acetate tetrahydrate are dissolved in 25ml of dimethyl sulfoxide, stirred at room temperature for 8h, washed three times with N, N-dimethylformamide and ethanol respectively as detergents and dried in a vacuum oven at 60℃for 24h.
(2) Preparation of magnetic graphitized carbon
And (3) heating the MOF powder obtained in the step (1) to 900 ℃ at a heating rate of 5 ℃/min in a tubular furnace under argon atmosphere, and preserving the temperature for 3 hours at 900 ℃, so that the finally obtained product is the magnetic graphitized carbon 4.
(3) Preparation of magnetic graphitized carbon-based composite phase change material
Dissolving 0.6g of stearyl alcohol and 0.4g of the magnetic graphitized carbon in the step (2) in 15ml of ethanol, carrying out ultrasonic treatment for 40min to dissolve the stearyl alcohol, uniformly mixing, putting the uniform mixed solution into a 60 ℃ oven, and carrying out heat preservation for 8h to completely volatilize the ethanol, thus obtaining a solid, namely the composite phase-change material 4.
The loading amount of the phase change material in the composite phase change material of the embodiment is 60%, and the photo-thermal conversion efficiency is 82.6%.
Example 5
(1) Preparation of cobalt MOF
3Mmol of terephthalic acid and 3mmol of cobalt acetate tetrahydrate are dissolved in 25ml of dimethyl sulfoxide, stirred at room temperature for 6h, washed three times with N, N-dimethylformamide and ethanol respectively as detergents and dried in a vacuum oven at 60℃for 12h.
(2) Preparation of magnetic graphitized carbon
And (3) heating the MOF powder obtained in the step (1) to 1000 ℃ at a heating rate of 5 ℃/min in a tube furnace under a nitrogen atmosphere, and preserving heat at 1000 ℃ for 2 hours, wherein the finally obtained product is the magnetic graphitized carbon 5.
(3) Preparation of magnetic graphitized carbon-based composite phase change material
Dissolving 0.6g of stearyl alcohol and 0.4g of the magnetic graphitized carbon in the step (2) in 15ml of ethanol, carrying out ultrasonic treatment for 60min to dissolve the stearyl alcohol, uniformly mixing, putting the uniform mixed solution into a 60 ℃ oven, and carrying out heat preservation for 8h to completely volatilize the ethanol, thus obtaining a solid, namely the composite phase-change material 5.
The loading amount of the phase change material in the composite phase change material of the embodiment is 60%, and the photo-thermal conversion capability is 85.3%.
The inventors of the present invention found that MOFs of large-sized crystals were more easily obtained with cobalt acetate hydrate than cobalt nitrate hydrate.
The inventor of the present invention found in the research and development process that the molar ratio of the metal ligand to the organic ligand in the metal-organic framework has a larger influence on the photothermal conversion capability, and increasing the content of the metal ligand within a certain range can increase the graphitization degree of the porous carbon and also increase the photothermal conversion capability, probably because the appropriate content of the metal ligand can increase the light absorption capability, and the synergistic effect with the phase change material is more remarkable, thereby increasing the photothermal conversion capability. The inventor also finds that proper carbonization temperature and carbonization time have great influence on the photo-thermal conversion capability of the obtained composite phase change material, and excessive carbonization time can influence the dispersion distribution of the cobalt simple substance and the pore diameter of porous carbon, thereby influencing the light absorption capability.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (34)
1. The application of the magnetic highly graphitized carbon-based photo-thermal composite phase change material in preparing the photo-thermal conversion material is characterized in that the photo-thermal composite phase change material comprises magnetic highly graphitized porous carbon and phase change materials adsorbed on the surface and/or in pore channels of the magnetic highly graphitized porous carbon, wherein the magnetic highly graphitized porous carbon is a carbon material which is obtained by carbonizing a metal organic frame at a high temperature and is highly uniformly dispersed with magnetic particles, the magnetic particles are one or more of iron, nickel and cobalt magnetic particles, and the magnetic particles account for 20% -50% of the total weight of the magnetic highly graphitized porous carbon;
In the photo-thermal composite phase-change material, the mass ratio of the magnetic high graphitized porous carbon to the phase-change material is 3:7-5:5;
i D/IG in the magnetic high graphitized porous carbon is less than or equal to 1;
The phase change material is solid-liquid phase change material, and is selected from one or more of polyalcohol phase change material, alkane phase change material, fatty alcohol phase change material and fatty acid phase change material.
2. The use according to claim 1, wherein in the photo-thermal composite phase change material, the mass ratio of the magnetic highly graphitized porous carbon to the phase change material is 3:7 to 5:5.
3. The use according to claim 1, wherein in the photo-thermal composite phase change material, the mass ratio of the magnetic highly graphitized porous carbon to the phase change material is 4:6.
4. The use according to claim 1, characterized in that the magnetic particles account for 24% -50% of the total weight of the magnetic highly graphitized porous carbon.
5. The use according to claim 1, wherein the magnetic particles account for 30% -46% of the total weight of the magnetic highly graphitized porous carbon.
6. The use according to claim 1, wherein the magnetic particles account for 34% -46% of the total weight of the magnetic highly graphitized porous carbon.
7. The use according to claim 1, wherein the magnetic particles account for 40% -46% of the total weight of the magnetic highly graphitized porous carbon.
8. Use according to claim 1, characterized in that the magnetic particles are highly homogeneously distributed in the carbon material.
9. The use according to claim 1, wherein I D/IG ∈0.95 in the magnetic highly graphitized porous carbon;
the magnetic particles are selected from one or more of elementary iron, elementary nickel and elementary cobalt magnetic particles.
10. The use according to claim 1, wherein I D/IG in the magnetic highly graphitized porous carbon is equal to or less than 0.9.
11. The use according to claim 1, wherein I D/IG in the magnetic highly graphitized porous carbon is equal to or less than 0.85.
12. The use according to claim 1, wherein the polyol phase change material is selected from one or more of polyethylene glycol, pentaerythritol;
the fatty alcohol phase-change material is one or more of dodecanol, tetradecanol, hexadecanol and octadecanol;
The alkane phase change material is one or more selected from tetradecane, hexadecane, octadecane, eicosane and octacosane;
the fatty acid phase change material is one or more of dodecanoic acid, tetradecanoic acid, hexadecanoic acid and octadecanoic acid.
13. Use according to any one of claims 1 to 12, wherein the metal-organic framework is obtained by reacting a metal acetate with an organic ligand.
14. The use according to claim 13, wherein the metal acetate is selected from one or more of iron acetate and its hydrated salts, nickel acetate and its hydrated salts, cobalt acetate and its hydrated salts;
The molar ratio of the organic ligand to the metal acetate is 3:1-5.
15. The use according to claim 13, wherein the molar ratio of the organic ligand to the metal acetate is 3:2-5.
16. The use according to claim 13, wherein the molar ratio of the organic ligand to the metal acetate is 3:2-4.
17. The use according to claim 13, wherein the molar ratio of the organic ligand to the metal acetate is 3:3-4.
18. The use according to claim 13, wherein the molar ratio of organic ligand to metal acetate is 3:3.
19. The use according to claim 13, wherein the metal-organic framework is prepared by the following method: dissolving hydrated metal acetate and organic ligand in solvent, stirring, collecting precipitate, washing and drying to obtain metal organic frame.
20. The use according to claim 19, wherein the stirring time is 6-12 hours.
21. Use according to claim 19, wherein the solvent is N, N-dimethylformamide or dimethylsulfoxide.
22. Use according to claim 19, wherein the organic ligand is terephthalic acid.
23. The use according to any one of claims 1 to 12, wherein the compounding process of the photothermal composite phase change material comprises the steps of: adding the magnetic highly graphitized porous carbon and the phase change material into a solvent, performing ultrasonic treatment, and drying to obtain the composite phase change material.
24. The use according to claim 23, wherein the ultrasound time is 10-30 min.
25. The use according to claim 23, wherein the drying temperature is 60-80 ℃ and the drying time is 2-24 h.
26. The use of claim 25, wherein the drying time is 6-24 hours.
27. The use according to any one of claims 1 to 12, wherein the high temperature carbonization conditions are: raising the temperature to carbonization temperature at a heating rate of 2-8 ℃/min under the inert gas atmosphere; and maintaining the carbonization temperature for 1-6 h, and cooling to obtain the carbon material.
28. Use according to claim 27, wherein the rate of temperature increase is 5 ℃/min.
29. Use according to claim 27, characterized in that the carbonization temperature is 800-1000 ℃.
30. Use according to claim 27, characterized in that the carbonization temperature is 1000 ℃.
31. The use according to claim 27, wherein the carbonization temperature is maintained for 2-4 hours.
32. Use according to claim 27, wherein the carbonization temperature retention time is 3 h.
33. Use according to claim 27, wherein the inert gas is nitrogen or argon.
34. Use according to any one of claims 1 to 12, in the field of solar heat storage.
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