CN112588214A - Phase-change material microcapsule with photo-thermal conversion and energy storage properties and preparation method thereof - Google Patents
Phase-change material microcapsule with photo-thermal conversion and energy storage properties and preparation method thereof Download PDFInfo
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- 239000012782 phase change material Substances 0.000 title claims abstract description 66
- 239000003094 microcapsule Substances 0.000 title claims abstract description 65
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 48
- 238000004146 energy storage Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 239000002775 capsule Substances 0.000 claims abstract description 11
- 229920002454 poly(glycidyl methacrylate) polymer Polymers 0.000 claims abstract description 9
- 229920000779 poly(divinylbenzene) Polymers 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 19
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 229920002189 poly(glycerol 1-O-monomethacrylate) polymer Polymers 0.000 claims description 15
- ZYURHZPYMFLWSH-UHFFFAOYSA-N octacosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC ZYURHZPYMFLWSH-UHFFFAOYSA-N 0.000 claims description 12
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 claims description 12
- HMSWAIKSFDFLKN-UHFFFAOYSA-N hexacosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC HMSWAIKSFDFLKN-UHFFFAOYSA-N 0.000 claims description 8
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 claims description 8
- 229940038384 octadecane Drugs 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- ZMYIIHDQURVDRB-UHFFFAOYSA-N 1-phenylethenylbenzene Chemical group C=1C=CC=CC=1C(=C)C1=CC=CC=C1 ZMYIIHDQURVDRB-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 238000005338 heat storage Methods 0.000 abstract description 7
- 229920002521 macromolecule Polymers 0.000 abstract description 4
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000011162 core material Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000012071 phase Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 5
- 230000031700 light absorption Effects 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention relates to a phase-change material microcapsule with photothermal conversion and energy storage properties and a preparation method thereof, wherein a microcapsule capsule core is a phase-change material with heat storage capacity; the wall material is of a multi-wall structure, and a polydivinylbenzene high polymer shell layer is arranged inside the wall material and is mainly used for packaging the phase change material; the exterior is an MXene shell layer which can be used for improving the encapsulation rate and the heat storage capacity of the microcapsule and endowing the microcapsule with a photo-thermal conversion effect. The preparation method adopts a one-pot method to prepare the novel phase change material microcapsule in a system in which the amphiphilic macromolecule 1, 1-stilbene terminated polyglycidyl methacrylate and MXene coexist synergistically and stably. The multi-wall structure microcapsule has the advantages of stable shape, high encapsulation efficiency, higher latent heat storage density and excellent photo-thermal conversion performance, and greatly enriches the application of phase change material microcapsules in the fields of solar energy utilization and the like.
Description
Technical Field
The invention belongs to a preparation method of a phase-change material microcapsule, and relates to a phase-change material microcapsule with photothermal conversion and energy storage properties and a preparation method thereof. The microcapsule has a phase-change material as its core, an inner layer of high polymer layer of polydivinylbenzene as its wall and an outer layer of MXene as its wall. The multi-wall microcapsule has high encapsulation efficiency and higher heat energy storage density and photothermal conversion efficiency.
Background
With the increasing world population and the continuous consumption of energy, the problem of energy shortage is more and more obvious, and solar energy is one of the most promising renewable energy sources, and the development trend of improving the storage technology and the utilization efficiency is inevitable. The solar energy conversion by using the novel phase-change composite material is an effective method for solving discontinuity of time and space, and the phase-change material microcapsule is prepared by using a phase-change material as a core material and using materials such as high polymer and the like as wall materials. The core material phase change material is a substance which can absorb or release a large amount of latent heat in the process of phase state transition at a specific temperature so as to realize temperature regulation and control; the wall material can effectively solve the problem of leakage of the phase-change material and prevent the phase-change material from reacting with the surrounding environment. The phase-change material microcapsule has the advantages of high energy storage density, adjustable phase-change temperature, stable performance and the like, and is widely applied to the fields of electronic appliances, energy-saving buildings, aerospace, aviation and the like.
At present, phase change material microcapsules still face many challenges in practical application, and the capsule wall of the existing microcapsules is mostly made of high polymer materials such as melamine resin, urea resin and the like, and is difficult to degrade and easy to corrode from the outside. The low thermal conductivity and lack of energy conversion capability have become critical issues that limit their applications. Researchers usually improve the problem by adopting an improved encapsulation technology or doping a high thermal conductive filler in a phase change material system, and carbon materials such as carbon nanotubes, graphite, graphene, porous carbon and the like are widely used for surface modification of phase change material microcapsules to improve heat transfer efficiency and endow the phase change material microcapsules with a photothermal conversion effect due to excellent light absorption, thermal conductivity and decorative performance. Compared with the carbon material, MXene is a two-dimensional transition metal carbide/nitride with a general formula of Mn+1Xn TxWherein M is a transition metal element, X is carbon, nitrogen, a carbon-nitrogen mixture, TxIs a surface functional group (-OH, -F, etc.), and n is 1, 2 or 3. MXene has high specific surface area, good metal conductivity, hydrophilicity and the like, and has the greatest advantages of self-perfect energy conversion capability and capability of maintaining high absorbanceThe solar energy storage material has near 100% of photothermal conversion efficiency under the condition, can expand the solar spectral response to a near infrared region, and is one of the most potential materials in the field of photothermal conversion energy storage research at present.
Chinese patent publication No. CN107384327A discloses an organic phase change material microcapsule coated with graphene oxide doped silica inorganic wall material and a preparation method thereof. The phase-change material microcapsule prepared by the method has a core-shell structure, the core material is an organic phase-change material, and the wall material is silicon dioxide doped with graphene oxide. Firstly, preparing microcapsules of silicon dioxide coated organic materials through an emulsification reaction, and then adding a graphene oxide solution into a prepared microcapsule dispersion system to dope graphene oxide, wherein the mass percentage of the doping is 0.2% -10%. The phase change material microcapsule prepared by the method has improved heat conductivity coefficient and photo-thermal conversion effect, the phase change heat fluid has light absorption capacity in a visible light range, but the research on the light absorption performance in a near infrared light range is lacked, and the step of doping high heat conduction filler in a two-step method is complicated.
The light absorption capability of the pure phase-change material microcapsule is weak, so that the application of the microcapsule in direct energy conversion is limited. At present, the approaches for realizing the phase-change material microcapsule with photothermal conversion and energy storage properties mainly include doping high thermal conductive filler in a microcapsule system or improving the packaging technology by adopting a material with photothermal conversion effect. However, the existing phase change material microcapsules mainly focus on improving the heat conductivity of the material, neglect the research on the photo-thermal property of the material, and are particularly applied to less technical means for improving the light absorption property of the phase change material microcapsules in the full spectrum range. The contradiction between higher encapsulation rate and excellent photo-thermal conversion performance of the phase-change material microcapsule is difficult to solve, and the work of adopting MXene to encapsulate the phase-change microcapsule is rarely reported.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a phase-change material microcapsule with photothermal conversion and energy storage properties and a preparation method thereof, and solves the problem that the conventional phase-change material microcapsule with photothermal conversion and energy storage properties is difficult to achieve higher encapsulation efficiency and excellent photothermal conversion performance at the same time.
Technical scheme
A phase-change material microcapsule with photo-thermal conversion and energy storage properties is characterized in that: the capsule core is made of phase-change material, and the wall material of the capsule wall is of a multi-wall structure; the multi-wall structure is characterized in that a polydivinylbenzene high polymer shell layer is arranged inside the multi-wall structure, and an MXene shell layer is arranged outside the multi-wall structure.
The phase change material is a waxy material with the phase transition temperature of 0-80 ℃ and capable of being encapsulated by microcapsules.
The phase change material includes, but is not limited to: tridecane, octadecane, eicosane, hexacosane, octacosane, paraffin sections for organisms, or a combination of several of them.
A method for preparing the phase-change material microcapsule with photothermal conversion and energy storage properties is characterized by comprising the following steps:
step 1: introducing nitrogen into 42.0g of glycidyl methacrylate, 0.54g of 1, 1-diphenylethylene and 480mL of deionized water, and reacting for 10 minutes at 200rpm in a water bath at the temperature of 80 ℃;
dissolving 0.09g of potassium persulfate in 120mL of deionized water, adding the solution into the reaction system, and continuing to polymerize for 18 hours in a nitrogen atmosphere;
distilling and dialyzing the obtained transparent product for one week to obtain a concentrated 1, 1-stilbene end-capped hydrolyzed polyglycidyl methacrylate D-PGMA solution;
step 2: 1.0g of the D-PGMA solution obtained in the step 1, 1.5g of divinylbenzene purified and deblocked by an alkaline alumina column, 1.0g of phase change material, 20-50mg of MXene and 15g of deionized water are subjected to high-speed shearing emulsification for 1 hour at 4000rpm in a water bath at the temperature of 50-70 ℃;
then introducing nitrogen, and reacting for 10-14 hours at the temperature of 80 ℃ in a water bath at 200 rpm;
and centrifuging, washing and freeze-drying the product to obtain the double-wall microcapsule.
The phase change material is a waxy material with the phase transition temperature of 0-80 ℃ and capable of being encapsulated by microcapsules.
The phase change material includes, but is not limited to: tridecane, octadecane, eicosane, hexacosane, octacosane, paraffin sections for organisms, or a combination of several of them.
Advantageous effects
The invention provides a phase-change material microcapsule with photothermal conversion and energy storage properties and a preparation method thereof, wherein a microcapsule capsule core is a phase-change material with heat storage capacity; the wall material is of a multi-wall structure, and a polydivinylbenzene high polymer shell layer is arranged inside the wall material and is mainly used for packaging the phase change material; the exterior is an MXene shell layer which can be used for improving the encapsulation rate and the heat storage capacity of the microcapsule and endowing the microcapsule with a photo-thermal conversion effect. The preparation method adopts a one-pot method to prepare the novel phase change material microcapsule in a system in which the amphiphilic macromolecule 1, 1-stilbene terminated polyglycidyl methacrylate and MXene coexist synergistically and stably. The multi-wall structure microcapsule has the advantages of stable shape, high encapsulation efficiency, higher latent heat storage density and excellent photo-thermal conversion performance, and greatly enriches the application of phase change material microcapsules in the fields of solar energy utilization and the like.
The invention has the beneficial effects that: the invention provides a preparation method of a phase change material microcapsule with photothermal conversion and energy storage properties. The prepared D-PGMA macromolecule has hydrophilic hydroxyl side chain and hydrophobic main chain, can be used as an emulsifier to stabilize the whole emulsion system, can generate free radicals at a high temperature to be used as an initiator to prepare polymer particles in an oil/water system, and is an ideal choice for constructing a long-term synergistic stable emulsion system together with MXene. In the whole oil/water system, D-PGMA macromolecules preferentially migrate to an oil-water interface, and a monomer divinyl benzene is initiated at the interface to form a high polymer shell layer serving as a phase change core material encapsulated by the inner wall of the microcapsule, so that the leakage of the phase change material can be effectively prevented. Then the MXene sheets in the water phase diffuse to the interface, effectively interact with D-PGMA through hydrogen bonds and are fixed on the interface, and finally the whole polymer shell layer is paved to form the MXene shell. The MXene shell can absorb part of light sources in a visible light region and a near infrared light region and efficiently convert the light sources into heat energy, the heat energy can be rapidly transferred into the phase change material microcapsules due to the high heat conduction performance of the MXene shell, and the core material phase change material can store the part of heat energy in the phase change process, so that the effects of photo-thermal conversion and energy storage are achieved. Therefore, the phase change material microcapsule prepared by the method has the advantages of stable shape, high encapsulation efficiency, higher latent heat storage density and excellent photo-thermal conversion performance.
Detailed Description
The invention will now be further described with reference to the examples:
the invention provides a preparation method of a multi-wall structure microcapsule with photothermal conversion and energy storage properties. The capsule core of the phase-change material microcapsule related by the method is a phase-change material, the capsule wall is of a multi-wall structure, the inside is a layer of polydivinylbenzene high polymer shell, and the outside is an MXene shell. Firstly, 1-stilbene is used for end capping modified poly glycidyl methacrylate, so that free radicals are generated under a high-temperature state, and the poly glycidyl methacrylate is used as an initiator to initiate the polymerization of monomer divinyl benzene. In a solution system where D-PGMA and MXene coexist synergistically and stably, MXene and D-PGMA are synergistically dispersed in an oil/water interface by high speed shearing action to initiate assembly of monomeric divinylbenzene into a polydivinylbenzene polymer shell at the interface. As the polymerization reaction continues, the MXene nanosheets tightly packed cover the whole surface of the polymer shell to form an outermost capsule wall. Finally, a novel phase change material microcapsule is obtained. The outermost capsule wall MXene of the phase-change material microcapsule prepared by the method is mainly used for absorbing a light source and converting the light source into heat energy, so that the heat energy is transferred to the interior of the phase-change microcapsule, and the core material phase-change material can store the heat energy in the phase-state conversion process, so that the effects of photo-thermal conversion and energy storage are achieved.
Example 1: octacosane as phase change material
Step one, 42.0g of glycidyl methacrylate, 0.54g of 1, 1-diphenylethylene and 480mL of deionized water are weighed. Nitrogen was passed through the reactor and the reaction was carried out at 200rpm in a water bath at 80 ℃ for 10 minutes. Thereafter, 0.09g of potassium persulfate was dissolved in 120mL of deionized water and added to the reaction system to continue the polymerization under a nitrogen atmosphere for 18 hours. The resulting clear product was distilled and dialyzed for one week to give a concentrated 1, 1-stilbene-terminated hydrolyzed polyglycidyl methacrylate (D-PGMA) solution.
Step two, weighing 1.0g of the D-PGMA solution obtained in the step one, 1.5g of divinylbenzene purified and deblocked by an alkaline alumina column, 1.0g of octacosane, 20mg of MXene and 15g of deionized water, and shearing and emulsifying at a high speed of 4000rpm for 1 hour in a water bath at 70 ℃. Then, nitrogen gas was introduced, and the reaction was carried out in a water bath at 80 ℃ and 200rpm for 10 hours. And centrifuging, washing and freeze-drying the product to obtain the double-wall microcapsule.
Example 2: section paraffin as phase-change material
Step one, 42.0g of glycidyl methacrylate, 0.54g of 1, 1-diphenylethylene and 480mL of deionized water are weighed. Nitrogen was passed through the reactor and the reaction was carried out at 200rpm in a water bath at 80 ℃ for 10 minutes. Thereafter, 0.09g of potassium persulfate was dissolved in 120mL of deionized water and added to the reaction system to continue the polymerization under a nitrogen atmosphere for 18 hours. The resulting clear product was distilled and dialyzed for one week to give a concentrated 1, 1-stilbene-terminated hydrolyzed polyglycidyl methacrylate (D-PGMA) solution.
Step two, weighing 1.0g of the D-PGMA solution obtained in the step one, 1.5g of divinylbenzene purified and deblocked by an alkaline alumina column, 1.0g of sliced paraffin, 40mg of MXene and 15g of deionized water, and shearing and emulsifying at a high speed of 4000rpm for 1 hour in a water bath at 60 ℃. Then, nitrogen gas was introduced, and the reaction was carried out in a water bath at 80 ℃ and 200rpm for 12 hours. And centrifuging, washing and freeze-drying the product to obtain the double-wall microcapsule.
Example 3: octadecane as phase change material
Step one, 42.0g of glycidyl methacrylate, 0.54g of 1, 1-diphenylethylene and 480mL of deionized water are weighed. Nitrogen was passed through the reactor and the reaction was carried out at 200rpm in a water bath at 80 ℃ for 10 minutes. Thereafter, 0.09g of potassium persulfate was dissolved in 120mL of deionized water and added to the reaction system to continue the polymerization under a nitrogen atmosphere for 18 hours. The resulting clear product was distilled and dialyzed for one week to give a concentrated 1, 1-stilbene-terminated hydrolyzed polyglycidyl methacrylate (D-PGMA) solution.
Step two, weighing 1.0g of the D-PGMA solution obtained in the step one, 1.5g of divinylbenzene purified and deblocked by an alkaline alumina column, 1.0g of octadecane, 50mg of MXene and 15g of deionized water, and shearing and emulsifying at a high speed of 4000rpm for 1 hour in a water bath at 50 ℃. Then, nitrogen gas was introduced, and the reaction was carried out for 14 hours at 200rpm in a water bath at 80 ℃. And centrifuging, washing and freeze-drying the product to obtain the double-wall microcapsule.
Claims (6)
1. A phase-change material microcapsule with photo-thermal conversion and energy storage properties is characterized in that: the capsule core is made of phase-change material, and the wall material of the capsule wall is of a multi-wall structure; the multi-wall structure is characterized in that a polydivinylbenzene high polymer shell layer is arranged inside the multi-wall structure, and an MXene shell layer is arranged outside the multi-wall structure.
2. The phase-change material microcapsule having both photothermal conversion and energy storage properties according to claim 1, wherein: the phase change material is a waxy material with the phase transition temperature of 0-80 ℃ and capable of being encapsulated by microcapsules.
3. The phase-change material microcapsule having both photothermal conversion and energy storage properties according to claim 1 or 2, wherein: the phase change material includes, but is not limited to: tridecane, octadecane, eicosane, hexacosane, octacosane, paraffin sections for organisms, or a combination of several of them.
4. A method for preparing the phase-change material microcapsule with photothermal conversion and energy storage properties as described in any one of claims 1 to 3, which is characterized by comprising the following steps:
step 1: introducing nitrogen into 42.0g of glycidyl methacrylate, 0.54g of 1, 1-diphenylethylene and 480mL of deionized water, and reacting for 10 minutes at 200rpm in a water bath at the temperature of 80 ℃;
dissolving 0.09g of potassium persulfate in 120mL of deionized water, adding the solution into the reaction system, and continuing to polymerize for 18 hours in a nitrogen atmosphere;
distilling and dialyzing the obtained transparent product for one week to obtain a concentrated 1, 1-stilbene end-capped hydrolyzed polyglycidyl methacrylate D-PGMA solution;
step 2: 1.0g of the D-PGMA solution obtained in the step 1, 1.5g of divinylbenzene purified and deblocked by an alkaline alumina column, 1.0g of phase change material, 20-50mg of MXene and 15g of deionized water are subjected to high-speed shearing emulsification for 1 hour at 4000rpm in a water bath at the temperature of 50-70 ℃;
then introducing nitrogen, and reacting for 10-14 hours at the temperature of 80 ℃ in a water bath at 200 rpm;
and centrifuging, washing and freeze-drying the product to obtain the double-wall microcapsule.
5. The method of claim 4, wherein: the phase change material is a waxy material with the phase transition temperature of 0-80 ℃ and capable of being encapsulated by microcapsules.
6. The method according to claim 4 or 5, characterized in that: the phase change material includes, but is not limited to: tridecane, octadecane, eicosane, hexacosane, octacosane, paraffin sections for organisms, or a combination of several of them.
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