CN113880997A - Thermoplastic polyethylene glycol-based phase-change energy storage material and preparation method and application thereof - Google Patents
Thermoplastic polyethylene glycol-based phase-change energy storage material and preparation method and application thereof Download PDFInfo
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- CN113880997A CN113880997A CN202110965038.2A CN202110965038A CN113880997A CN 113880997 A CN113880997 A CN 113880997A CN 202110965038 A CN202110965038 A CN 202110965038A CN 113880997 A CN113880997 A CN 113880997A
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- polyethylene glycol
- energy storage
- storage material
- change energy
- monoacrylated
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- 239000002202 Polyethylene glycol Substances 0.000 title claims abstract description 158
- 229920001223 polyethylene glycol Polymers 0.000 title claims abstract description 158
- 238000004146 energy storage Methods 0.000 title claims abstract description 72
- 239000011232 storage material Substances 0.000 title claims abstract description 67
- 229920001169 thermoplastic Polymers 0.000 title claims abstract description 31
- 239000004416 thermosoftening plastic Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 65
- 230000008859 change Effects 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000001723 curing Methods 0.000 claims description 30
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 17
- 238000000016 photochemical curing Methods 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910021389 graphene Inorganic materials 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 11
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 10
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 8
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- 229920001187 thermosetting polymer Polymers 0.000 claims description 6
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 5
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002612 dispersion medium Substances 0.000 claims description 5
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 5
- 238000001029 thermal curing Methods 0.000 claims description 5
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 3
- 238000004134 energy conservation Methods 0.000 claims description 3
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 claims description 3
- 125000002816 methylsulfanyl group Chemical group [H]C([H])([H])S[*] 0.000 claims description 3
- 125000004573 morpholin-4-yl group Chemical group N1(CCOCC1)* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 3
- 239000004753 textile Substances 0.000 claims description 3
- 239000002918 waste heat Substances 0.000 claims description 3
- HGXJDMCMYLEZMJ-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOOC(=O)C(C)(C)C HGXJDMCMYLEZMJ-UHFFFAOYSA-N 0.000 claims description 2
- JJRDRFZYKKFYMO-UHFFFAOYSA-N 2-methyl-2-(2-methylbutan-2-ylperoxy)butane Chemical compound CCC(C)(C)OOC(C)(C)CC JJRDRFZYKKFYMO-UHFFFAOYSA-N 0.000 claims description 2
- BLCKNMAZFRMCJJ-UHFFFAOYSA-N cyclohexyl cyclohexyloxycarbonyloxy carbonate Chemical compound C1CCCCC1OC(=O)OOC(=O)OC1CCCCC1 BLCKNMAZFRMCJJ-UHFFFAOYSA-N 0.000 claims description 2
- -1 ethyl 2,4, 6-trimethylbenzoyl phenyl Chemical group 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000007711 solidification Methods 0.000 abstract description 3
- 230000008023 solidification Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 50
- 239000000463 material Substances 0.000 description 29
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- 239000007791 liquid phase Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 4
- 238000010382 chemical cross-linking Methods 0.000 description 4
- 125000004386 diacrylate group Chemical group 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
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- 230000007547 defect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
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- 238000003860 storage Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical group CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- 108010053481 Antifreeze Proteins Proteins 0.000 description 1
- 241000408529 Libra Species 0.000 description 1
- 206010057040 Temperature intolerance Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- YMCOIFVFCYKISC-UHFFFAOYSA-N ethoxy-[2-(2,4,6-trimethylbenzoyl)phenyl]phosphinic acid Chemical compound CCOP(O)(=O)c1ccccc1C(=O)c1c(C)cc(C)cc1C YMCOIFVFCYKISC-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
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- 230000037048 polymerization activity Effects 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E70/00—Other energy conversion or management systems reducing GHG emissions
- Y02E70/30—Systems combining energy storage with energy generation of non-fossil origin
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention belongs to the technical field of phase change energy storage materials, and particularly relates to a thermoplastic polyethylene glycol-based phase change energy storage material, and a preparation method and application thereof. The method comprises the following steps: dissolving high-molecular-weight solid monoacrylated polyethylene glycol, an initiator and a nano heat-conducting filler dispersion liquid into low-molecular-weight liquid monoacrylated polyethylene glycol according to the mass ratio, and uniformly stirring to obtain a phase-change energy-storage material precursor; and curing and molding the precursor to obtain the thermoplastic polyethylene glycol-based phase change energy storage material. The raw material selected for preparing the thermoplastic polyethylene glycol-based phase-change energy storage material is monoacrylated polyethylene glycol with different molecular weights, and the molecular structure is that an acrylic acid molecule is connected with one end of a polyethylene glycol molecular chain, so that after solidification and forming, the content of other substances except the polyethylene glycol in the phase-change energy storage material is extremely low, the phase-change enthalpy of the polyethylene glycol is reduced to the minimum extent, and the phase-change energy storage material can be widely applied to the field of heat energy storage.
Description
Technical Field
The invention belongs to the technical field of phase change energy storage materials, and particularly relates to a thermoplastic polyethylene glycol-based phase change energy storage material, and a preparation method and application thereof.
Background
Phase change energy storage materials (PCM) refer to materials that absorb or release phase change heat during a phase transformation process, thereby storing energy and regulating the temperature of the environment. The material can solve the contradiction that the energy supply and demand are not matched in time and space, and is a hot spot for the research on energy utilization and material science at home and abroad. The phase change energy storage material has wide application prospect in the fields of aerospace, building energy conservation, solar energy utilization, electric power peak regulation, waste heat utilization, cold chain transportation, coating industry, textile industry, agricultural engineering and the like. Commonly used organic phase changes include mainly paraffin, acetic acid, fatty acids, polyethylene glycol and other organic substances. The phase change enthalpy of polyethylene glycol (PEG) is high, the phase change enthalpy is 140-175J/g, and the thermal hysteresis effect is low; the molecular weight is adjustable, and after PEG with different molecular weights is mixed according to a certain proportion, thermal performance parameters can be adjusted, so that the melting temperature and the crystallization temperature of a crystal region move to be within a required phase transition temperature range. Therefore, PEG with different polymerization degrees can be selected as the energy storage material under different application conditions. The phase-change temperature of PEG with different molecular weights is 45-70 ℃, so that the PEG is a solid-liquid phase-change energy storage material, and the phase-change energy storage material generates a liquid phase in the phase-change process and must be packaged by a special container, so that the thermal resistance between a heat transfer medium and the phase-change material is increased, the heat transfer efficiency is reduced, and the production cost is greatly improved. In order to overcome the defects of the solid-liquid phase change energy storage material, a certain technical means is required to be adopted to convert the solid-liquid phase change material into the solid-solid phase change material, and the commonly used technical means mainly comprise a microcapsule technology, a chemical crosslinking technology, a physical adsorption technology and the like. However, the above technical means has the disadvantages that the preparation method is complicated in the process of preparing the solid-solid phase change material, the phase change latent heat of the composite phase change material is easily reduced, the phase change enthalpy is reduced, or the composite phase change material is easily denatured in the long-term phase change process. In addition, polyethylene glycol is used as an organic phase-change heat storage material, has low heat conductivity coefficient and is not beneficial to heat transfer.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a preparation method of a thermoplastic polyethylene glycol-based phase change energy storage material.
The invention also aims to provide the thermoplastic polyethylene glycol-based phase change energy storage material prepared by the method.
The invention further aims to provide application of the thermoplastic polyethylene glycol-based phase change energy storage material in the fields of heat energy storage such as aerospace, building energy conservation, solar energy utilization, electric power peak regulation, waste heat utilization, cold chain transportation, coating industry, textile industry, agricultural engineering and the like.
A preparation method of a thermoplastic polyethylene glycol-based phase change energy storage material comprises the following steps:
dissolving high molecular weight monoacrylated polyethylene glycol, an initiator and a nano heat-conducting filler dispersion liquid in low molecular weight monoacrylated polyethylene glycol according to a mass ratio, and uniformly stirring to obtain a precursor; and curing and molding the precursor to obtain the thermoplastic polyethylene glycol-based phase change energy storage material.
The average molecular weight of the high molecular weight monoacrylated polyethylene glycol is 1000-20000, the high molecular weight monoacrylated polyethylene glycol is in a solid state, and the high molecular weight monoacrylated polyethylene glycol is used as a prepolymer in the preparation process of the thermoplastic phase-change energy storage material.
The average molecular weight of the monoacrylated polyethylene glycol is 200-1000, the monoacrylated polyethylene glycol is in a liquid state, and the monoacrylated polyethylene glycol is used as an active diluent in the preparation process of the thermoplastic phase-change energy storage material.
The monoacrylated polyethylene glycol is at least one of polyethylene glycol monoacrylate, polyethylene glycol monomethacrylate, methoxy polyethylene glycol monoacrylate, methoxy polyethylene glycol monomethacrylate, ethoxy polyethylene glycol monoacrylate and ethoxy polyethylene glycol monomethacrylate.
The curing method is one of photo-curing or thermal curing.
The initiator is one of a photo-initiator or a thermal initiator.
The photoinitiator is at least one of 1-hydroxycyclohexyl phenyl ketone (Irgacure-184), 2-hydroxy-2-methyl-1-phenyl acetone (Irgacure-1173), 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone (Irgacure-907), 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide (TPO) and 2,4, 6-trimethylbenzoyl phenyl ethyl phosphonate (TPO-L).
The thermal initiator is at least one of azobisisobutyronitrile, dimethyl azobisisobutyrate, benzoyl peroxide, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, tert-butyl peroxybenzoate, tert-butyl peroxypivalate, di-tert-butyl peroxide and di-tert-amyl peroxide.
The mass ratio of the high molecular weight monoacrylated polyethylene glycol to the low molecular weight monoacrylated polyethylene glycol is (10-30): (70-90).
The amount of the initiator is 1-5% of the total mass of the high molecular weight monoacrylated polyethylene glycol and the low molecular weight monoacrylated polyethylene glycol.
The nano heat-conducting filler dispersion liquid mainly comprises a dispersion phase, a dispersion medium and a conventional wetting agent, wherein the dispersion phase is one of nano boron nitride, nano aluminum nitride and nano graphene oxide, the particle size of the dispersion phase is 20-200 nm, the dispersion medium is liquid polyethylene glycol, the average molecular weight of the dispersion medium is 200-800, and the mass concentration of the dispersion liquid is 5-30%.
The dosage of the nano heat-conducting filler dispersion liquid is 0-10% of the total mass of the high-molecular-weight monoacrylated polyethylene glycol and the low-molecular-weight monoacrylated polyethylene glycol. The thermal conductivity of the material can be improved to a greater extent by adding the nano heat-conducting filler dispersion liquid. But when the requirement of partial materials on the thermal conductivity is not high, the addition amount of the nano heat-conducting filler dispersion liquid can also be 0.
The photocuring is performed by ultraviolet light or LED lamp light irradiation; the ultraviolet light wavelength is 245-365 nm, the power is 1-5 kW, the LED light wavelength is 320-420 nm, and the power is 10-100W.
The heating curing temperature is 80-160 ℃.
The photocuring time is 1-5 min, and the thermocuring time is 10-60 min.
The solid-solid phase change energy storage material is prepared by adopting the monoacrylated polyethylene glycol through a photocuring or thermocuring method, so that the application range of the phase change energy storage material can be further expanded. The phase change energy storage material is prepared by adopting a photocuring method, so that the phase change energy storage material can be applied to the field of heat sensitivity, and the damage of heating and curing to the application environment is overcome. The thermosetting method can effectively overcome the limitations of the photocuring method in the aspects of light penetration force, curing depth and the like, and can prepare phase change energy storage materials with various shapes and thicknesses.
The graft copolymerization is that the chain end of the long chain of the crystalline phase-change material polyethylene glycol is grafted on another skeleton polymer with higher melting point, high strength and stable structure through chemical reaction. In the heating process, the PEG macromolecular branched chain is subjected to solid-liquid phase transition from a crystalline state to an amorphous state, and a macromolecular main chain with a high melting point is not melted, so that the macroscopic flow of PEG is limited, the material is kept in a solid state on the whole, and the aim of realizing solid phase transition energy storage by using the solid-liquid phase transition material can be fulfilled. The solid-solid phase change energy storage material is prepared by adopting monoacrylated polyethylene glycol through a photocuring or thermocuring method, and the prepared polymer is in a linear structure and is thermoplastic resin. The raw material of the monoacrylated polyethylene glycol contains an acrylic double bond at one end and a group without polymerization activity at the other end, so that the formed polymer is linear and the main chain has a branch chain with a molecular brush structure during polymerization and solidification. In the polymer, the main chain is polyacrylate, and the branched chain is a polyethylene glycol chain segment. The polyethylene glycol molecular chains are connected in series through the polyacrylate main chain, so that when the polymer absorbs heat, the polyethylene glycol molecular chains can move flexibly to form regular crystals, and the change of phase change enthalpy relative to pure polyethylene glycol is not large. Due to the fixing effect of the polyacrylate main chain, the polyethylene glycol cannot be melted and leaked when being heated. The phase-change energy storage material prepared by polymerization reaction of diacrylated polyethylene glycol has a network structure of the polymer due to double bonds at both ends of the polyethylene glycol in the raw material, is thermosetting resin, and is not easy to be heated to generate phase-change energy storage. In addition, because the two ends of the polyethylene glycol are polymerized and fixed, when the polyethylene glycol is heated, the movement of the polyethylene glycol molecular chain is greatly limited, and the polyethylene glycol molecular chain is prevented from forming regular crystals, so that the phase change enthalpy of the polyethylene glycol is reduced by a larger extent than that of pure polyethylene glycol.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the ultraviolet curing technology is a rapid curing molding technology, and the essence of the technology is that polymerization reaction occurs to form polymers with high molecular weight. The invention uses the light curing technology to prepare the phase change energy storage material, the preparation method is very simple, only needs one step to complete, and the curing and forming speed is extremely high, and only needs a few seconds to a few minutes to complete the curing and forming. The polyethylene glycol in the invention belongs to chemical crosslinking and curing, and forms a high molecular weight polymer after curing, so that the leakage problem can not exist.
(2) The raw material selected for preparing the polyethylene glycol-based phase-change energy storage material is polyethylene glycol diacrylate with different molecular weights, and the molecular structure is that two ends of a polyethylene glycol molecular chain are respectively connected with an acrylic acid molecule, so that after the polyethylene glycol-based phase-change energy storage material is solidified and formed, the content of other substances except the polyethylene glycol in the phase-change energy storage material is extremely low, and the phase-change enthalpy of the polyethylene glycol is reduced to the minimum extent.
(3) The polyethylene glycol-based phase change energy storage material prepared by the invention is thermoplastic resin, and can be processed into various shapes by heating, melting and extrusion molding after polymerization and solidification, so that the application requirements of various fields can be met. The thermoplastic resin has good toughness, large damage tolerance, good dielectric constant, unlimited storage period, no need of low-temperature storage, no need of large-scale special equipment such as autoclave for molding, and especially has the characteristics of good recyclability, recoverability, reusability and no environmental pollution, thus being suitable for the development direction of current material environmental protection.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The materials referred to in the following examples are commercially available. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
70g of polyethylene glycol monoacrylate with the average molecular weight of 10000, 3g of photoinitiator 1-hydroxycyclohexyl phenyl ketone (Irgacure-184) and 0g or 1g of nano boron nitride dispersion are added into 30g of methoxy polyethylene glycol monomethacrylate with the average molecular weight of 200, the mixture is uniformly stirred, then the precursor is poured into a mold, and the mixture is cured for 2min under the ultraviolet light with the wavelength of 365nm and the power of 1kW, so that the photo-curing polyethylene glycol based phase-change energy storage material is obtained. The particle size of boron nitride in the nano boron nitride dispersion liquid is 200nm, the dispersed phase is polyethylene glycol with the molecular weight of 200, and the mass concentration of the dispersion liquid is 5%. The thermal conductivity of the sample prepared in this example is tested, and it is found that, compared with a product without the nano thermal conductive filler dispersion (with an addition amount of 0g), after the nano thermal conductive filler dispersion is added, the thermal conductivity of the prepared thermoplastic polyethylene glycol-based phase change energy storage material is improved by 14.2 times.
Example 2
Adding 90g of polyethylene glycol monomethacrylate with the average molecular weight of 2000, 0g or 1g of photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone (Irgacure-1173) and 5g of nano aluminum nitride dispersion into 10g of polyethylene glycol monoacrylate with the average molecular weight of 1000, uniformly stirring, pouring the precursor into a mold, and curing for 5min under the LED light with the wavelength of 320nm and the power of 10W to obtain the photocuring polyethylene glycol-based phase-change energy storage material. The particle size of the aluminum nitride in the nano aluminum nitride dispersion liquid is 100nm, the dispersed phase is polyethylene glycol with the molecular weight of 600, and the mass concentration of the dispersion liquid is 20%. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was increased by 12.4 times after the addition of the nano thermal conductive filler dispersion.
Example 3
Adding 80g of polyethylene glycol monoacrylate with the average molecular weight of 3000, 2g of photoinitiator 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone (Irgacure-907) and 0g or 1g of nano graphene oxide dispersion into 20g of methoxy polyethylene glycol monoacrylate with the average molecular weight of 600, uniformly stirring, pouring the precursor into a mold, and curing for 2min under the ultraviolet light with the wavelength of 305nm and the power of 5kW to obtain the photocuring polyethylene glycol-based phase change energy storage material. The particle size of graphene oxide in the nano graphene oxide dispersion liquid is 20nm, the dispersed phase is polyethylene glycol with the molecular weight of 800, and the mass concentration of the dispersion liquid is 30%. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 13.8 times after the addition of the nano thermal conductive filler dispersion.
Example 4
Adding 75g of ethoxy polyethylene glycol monomethacrylate with the average molecular weight of 8000, 5g of photoinitiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide (TPO) and 0g or 5g of nano aluminum nitride dispersion liquid into 25g of polyethylene glycol monomethacrylate with the average molecular weight of 400, uniformly stirring, pouring the precursor into a mold, and curing for 5min under the ultraviolet light with the wavelength of 245nm and the power of 2.5kW to obtain the photocuring polyethylene glycol-based phase-change energy storage material. The particle size of aluminum nitride in the nano aluminum nitride dispersion liquid is 150nm, the dispersed phase is polyethylene glycol with the molecular weight of 500, and the mass concentration of the dispersion liquid is 25%. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 14.5 times after the addition of the nano thermal conductive filler dispersion.
Example 5
Adding 80g of polyethylene glycol monoacrylate with the average molecular mass of 20000, 4g of photoinitiator ethyl 2,4, 6-trimethylbenzoylphenylphosphonate (TPO-L) and 0g or 8g of nano graphene oxide dispersion liquid into 20g of polyethylene glycol monoacrylate with the average molecular weight of 400, uniformly stirring, pouring the precursor into a mold, and curing for 1min under the LED light with the wavelength of 420nm and the power of 50W to obtain the photocuring polyethylene glycol-based phase-change energy storage material. The particle size of graphene oxide in the nano graphene oxide dispersion liquid is 120nm, the dispersion phase is polyethylene glycol with the molecular weight of 400, and the mass concentration of the dispersion liquid is 15%. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was increased by 12.8 times after the addition of the nano thermal conductive filler dispersion.
Example 6
70g of methoxy polyethylene glycol monoacrylate with the average molecular weight of 3400, 3g of photoinitiator 1-hydroxycyclohexyl phenyl ketone (Irgacure-184) and 0g or 6g of nano boron nitride dispersion are added into 30g of polyethylene glycol monoacrylate with the average molecular weight of 1000, the mixture is uniformly stirred, then the precursor is poured into a mold, and the mixture is cured for 2min under the ultraviolet light with the wavelength of 370nm and the power of 100W, so that the photo-curing polyethylene glycol based phase change energy storage material is obtained. The particle size of boron nitride in the nano boron nitride dispersion liquid is 140nm, the dispersed phase is polyethylene glycol with the molecular weight of 300, and the mass concentration of the dispersion liquid is 10%. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 13.9 times after the addition of the nano thermal conductive filler dispersion.
Example 7
The conditions in this example are the same as in example 1, except that: the photoinitiator was replaced with the thermal initiator azobisisobutyronitrile, the curing temperature was 80 ℃ and the curing time was 60 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 14.0 times after the addition of the nano thermal conductive filler dispersion.
Example 8
The conditions in this example are the same as in example 2, except that: the photoinitiator was replaced with thermal initiator dimethyl azodiisobutyrate at a cure temperature of 80 ℃ for a cure time of 60 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was increased by 12.6 times after the addition of the nano thermal conductive filler dispersion.
Example 9
The conditions in this example are the same as in example 3, except that: the photoinitiator was replaced with thermal initiator benzoyl peroxide, curing temperature was 120 ℃ and curing time was 30 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 14.1 times after the addition of the nano thermal conductive filler dispersion.
Example 10
The conditions in this example are the same as in example 4, except that: the photoinitiator was replaced with the thermal initiator diisopropyl peroxydicarbonate, the curing temperature was 120 ℃ and the curing time was 30 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 14.2 times after the addition of the nano thermal conductive filler dispersion.
Example 11
The conditions in this example were the same as in example 5, except that: the photoinitiator was replaced with t-butyl peroxybenzoate as a thermal initiator at 160 ℃ for 10 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 13.1 times after the addition of the nano thermal conductive filler dispersion.
Example 12
The conditions in this example are the same as in example 6, except that: replacing the photoinitiator with a thermal initiator of di-tert-butyl peroxide, wherein the curing temperature is 160 ℃, and the curing time is 10 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 13.6 times after the addition of the nano thermal conductive filler dispersion.
Example 13
The conditions in this example are the same as in example 1, except that: the illumination time is 5 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 14.1 times after the addition of the nano thermal conductive filler dispersion.
Example 14
The conditions in this example are the same as in example 2, except that: the wavelength of the light is 405 nm. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was increased by 12.6 times after the addition of the nano thermal conductive filler dispersion.
Example 15
The conditions in this example are the same as in example 3, except that: the photoinitiator is 2-hydroxy-2-methyl-1-phenyl acetone (Irgacure-1173). The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 13.2 times after the addition of the nano thermal conductive filler dispersion.
Example 16
The conditions in this example were the same as in example 7, except that: the curing temperature was 160 ℃. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was increased by 12.3 times after the addition of the nano thermal conductive filler dispersion.
Example 17
The conditions in this example are the same as those in example 8, except that: the curing time was 60 min. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was increased by 12.5 times after the addition of the nano thermal conductive filler dispersion.
Example 18
The conditions in this example were the same as in example 9, except that: the thermal initiator is diisopropyl peroxydicarbonate. The thermal conductivity of the sample prepared in this example was tested, and it was found that the thermal conductivity of the prepared material was improved by 14.5 times after the addition of the nano thermal conductive filler dispersion.
Comparative example 1
Heating and melting 70g of polyethylene glycol with the average molecular weight of 3400, adding 1g of nano graphene oxide dispersion liquid, stirring uniformly, pouring the mixed liquid into a mold, heating to the temperature of 140 ℃, and curing for 20min to obtain the thermosetting polyethylene glycol-based phase change energy storage material. The particle size of graphene oxide in the nano graphene oxide dispersion liquid is 20nm, the dispersed phase is polyethylene glycol with the molecular weight of 800, and the mass concentration of the dispersion liquid is 10%.
Comparative example 2
Heating and melting 70g of polyethylene glycol with the average molecular weight of 3400, adding 1g of nano boron nitride dispersion liquid, stirring uniformly, pouring the precursor into a mold, heating to the temperature of 140 ℃ and curing for 20min to obtain the thermosetting polyethylene glycol-based phase change energy storage material. The particle size of boron nitride in the nano boron nitride dispersion liquid is 20nm, the dispersed phase is polyethylene glycol with the molecular weight of 800, and the mass concentration of the dispersion liquid is 10%.
Comparative example 3
70g of polyethylene glycol diacrylate with the average molecular weight of 3400, 3g of photoinitiator 1-hydroxycyclohexyl phenyl ketone (Irgacure-184) and 0g or 1g of nano boron nitride dispersion liquid are added into 30g of polyethylene glycol diacrylate with the average molecular weight of 1000, the mixture is uniformly stirred, then the precursor is poured into a mould, and the mixture is cured for 2min under ultraviolet light with the wavelength of 400nm, so that the photo-curing polyethylene glycol based phase change energy storage material is obtained. The particle size of boron nitride in the nano boron nitride dispersion liquid is 140nm, the dispersed phase is polyethylene glycol with the molecular weight of 300, and the mass concentration of the dispersion liquid is 10%.
Comparative example 4
The comparative example was conducted under the same conditions as in example 11 except that: polyethylene glycol monoacrylate with the average molecular weight of 1000 is adopted, namely 100g of polyethylene glycol monoacrylate with the average molecular weight of 1000, 4g of thermal initiator tert-butyl peroxybenzoate and 7g of nano boron nitride dispersion are mixed and stirred uniformly.
Example for testing the Performance of thermoplastic polyethylene glycol-based phase-change energy storage Material
The thermoplastic polyethylene glycol-based phase change energy storage materials prepared in examples 1 to 18 (data detection results are not shown in the table below when the addition amount of the nano heat conductive filler dispersion is 0g) and comparative examples 1 to 4 were tested for their relevant performance.
The phase transition temperature and enthalpy of transition (melting and condensation process) were tested using a german Netzsch Q8000 DSC analyzer. Rate of temperature rise or decrease: 10 ℃/min; atmosphere: nitrogen gas. Prior to testing, the samples were heated from 0 ℃ to 100 ℃ and held at 100 ℃ for 5min to eliminate thermal history. The procedure was to heat all samples from 0 ℃ to 100 ℃ and hold at 100 ℃ for 5min, then cool to 0 ℃ and hold at 0 ℃ for 5min, and the DSC curves were recorded for all samples.
Thermal stability analysis (heat loss analysis) was carried out using a thermogravimetric analyzer of the Netzsch type 209F1 Libra, Germany. Test temperature range: 30-650 ℃, heating rate: 10 ℃/min; atmosphere: nitrogen gas. The mass loss ratio at different temperatures for each example was recorded.
Table 1 results of thermal performance test of the products of each test example
For the polyethylene glycol-based phase change material, the closer the enthalpy change value of the composite phase change material is to the enthalpy change value of pure PEG, the better the performance is, the enthalpy change values of the composite phase change material are all larger than 140J/g and are very close to the enthalpy change value of PEG of 140-175J/g. The thermal stability is another important index of the composite phase-change material, the thermal weight loss of the composite phase-change material is less than 1% at 200 ℃ which exceeds the melting point of PEG, and the thermal weight loss at 400 ℃ is less than 2%, which shows that the composite phase-change material has excellent thermal stability, and liquid leakage after polyethylene glycol is melted can not occur in the using process. The phase change energy storage material directly prepared by physically blending boron nitride or graphene oxide with polyethylene glycol has poor thermal stability, and particularly, the heat loss is very large at 400 ℃ when the boron nitride is directly blended with the polyethylene glycol. The phase change energy storage material prepared by blending the graphene oxide and the polyethylene glycol has a hydrogen bond effect and a small amount of chemical crosslinking, so that the thermal stability of the phase change energy storage material is improved to a certain extent. In addition, the scheme also researches the reaction product of the polyethylene glycol diacrylate and the nano heat-conducting filler dispersion liquid, and can be obtained from the table above, the phase change break of the product in the melting process and the condensation process is 0, namely the function of phase change energy storage is completely avoided.
After the temperature is higher than 500 ℃, the thermal weight loss of the phase-change material is very obvious and is higher than 80%, the temperature exceeds the heat-resistant temperature of PEG, and the normal heat loss exists, but the heat loss is still far smaller than that of comparative examples 1 and 2 because the chemical crosslinking is adopted in the invention and the comparative example 3.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (14)
1. The preparation method of the thermoplastic polyethylene glycol-based phase change energy storage material is characterized by comprising the following steps of:
dissolving high-molecular-weight monoacrylated polyethylene glycol, an initiator and a nano heat-conducting filler dispersion liquid into low-molecular-weight monoacrylated polyethylene glycol according to a mass ratio, uniformly stirring to obtain a precursor, and curing and molding the precursor to obtain the thermoplastic polyethylene glycol-based phase-change energy storage material;
the curing method is photocuring or thermocuring;
the average molecular weight of the high molecular weight monoacrylated polyethylene glycol is 1000-20000; the low molecular weight monoacrylated polyethylene glycol has an average molecular weight of 200-1000.
2. The method for preparing the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 1, wherein the high molecular weight monoacrylated polyethylene glycol is in a solid state; the low molecular weight monoacrylated polyethylene glycol is in a liquid state.
3. The method for preparing the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 1, wherein the monoacrylated polyethylene glycol is at least one of polyethylene glycol monoacrylate, polyethylene glycol monomethacrylate, methoxy polyethylene glycol monoacrylate, methoxy polyethylene glycol monomethacrylate, ethoxy polyethylene glycol monoacrylate, and ethoxy polyethylene glycol monomethacrylate.
4. The method for preparing the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 1, wherein the initiator is one of a photoinitiator or a thermal initiator;
the photoinitiator is at least one of 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl acetone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide and ethyl 2,4, 6-trimethylbenzoyl phenyl phosphonate;
the thermal initiator is at least one of azobisisobutyronitrile, dimethyl azobisisobutyrate, benzoyl peroxide, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, tert-butyl peroxybenzoate, tert-butyl peroxypivalate, di-tert-butyl peroxide and di-tert-amyl peroxide.
5. The preparation method of the thermoplastic polyethylene glycol-based phase-change energy storage material according to claim 1, wherein the mass ratio of the high molecular weight monoacrylated polyethylene glycol to the low molecular weight monoacrylated polyethylene glycol is (10-30): (70-90).
6. The preparation method of the thermoplastic polyethylene glycol-based phase-change energy storage material according to claim 1, wherein the amount of the initiator is 1-5% of the total mass of the high molecular weight monoacrylated polyethylene glycol and the low molecular weight monoacrylated polyethylene glycol.
7. The preparation method of the thermoplastic polyethylene glycol-based phase-change energy storage material according to claim 1, wherein the dispersed phase in the nano heat-conducting filler dispersion liquid is one of nano boron nitride, nano aluminum nitride and nano graphene oxide, and the particle size of the dispersed phase is 20-200 nm; the dispersion medium in the nano heat-conducting filler dispersion liquid is liquid polyethylene glycol, and the average molecular weight of the dispersion medium is 200-800; the mass concentration of the nano heat-conducting filler dispersion liquid is 5-30%.
8. The preparation method of the thermoplastic polyethylene glycol-based phase-change energy storage material according to claim 1, wherein the amount of the nano heat-conducting filler dispersion is 0-10% of the total mass of the high-molecular-weight monoacrylated polyethylene glycol and the low-molecular-weight monoacrylated polyethylene glycol.
9. The preparation method of the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 1, wherein the photocuring is performed by ultraviolet light or LED lamp irradiation;
the ultraviolet light wavelength is 245-365 nm, the power is 1-5 kW, the LED light wavelength is 320-420 nm, and the power is 10-100W.
10. The preparation method of the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 1, wherein the photocuring time is 1-5 min.
11. The preparation method of the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 1, wherein the thermosetting temperature is 80-160 ℃ and the thermosetting time is 10-60 min.
12. A thermoplastic polyethylene glycol-based phase change energy storage material prepared by the preparation method according to any one of claims 1 to 11.
13. Use of the thermoplastic polyethylene glycol-based phase change energy storage material according to claim 12 in the field of thermal energy storage.
14. The thermoplastic polyethylene glycol-based phase change energy storage material according to claim 12, which is used in the fields of aerospace, building energy conservation, solar energy utilization, electric power peak regulation, waste heat utilization, cold chain transportation, coating industry, textile industry and agricultural engineering.
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