CN117821024A - Preparation method of MXene/sorghum straw biomass aerogel-based composite phase-change material - Google Patents
Preparation method of MXene/sorghum straw biomass aerogel-based composite phase-change material Download PDFInfo
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- 240000006394 Sorghum bicolor Species 0.000 title claims abstract description 134
- 235000011684 Sorghum saccharatum Nutrition 0.000 title claims abstract description 134
- 239000010902 straw Substances 0.000 title claims abstract description 131
- 239000012782 phase change material Substances 0.000 title claims abstract description 83
- 239000002028 Biomass Substances 0.000 title claims abstract description 72
- 239000002131 composite material Substances 0.000 title claims abstract description 72
- 239000004964 aerogel Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000004108 freeze drying Methods 0.000 claims abstract description 19
- 239000000017 hydrogel Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 150000001412 amines Chemical class 0.000 claims abstract description 7
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- 238000005470 impregnation Methods 0.000 claims description 9
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 8
- RVRHBLSINNOLPI-UHFFFAOYSA-N Lythridin Natural products COc1ccc(cc1OC)C2CC(CC3CCCCN23)OC(=O)CC(O)c4ccc(O)cc4 RVRHBLSINNOLPI-UHFFFAOYSA-N 0.000 claims description 5
- LTNZEXKYNRNOGT-UHFFFAOYSA-N dequalinium chloride Chemical group [Cl-].[Cl-].C1=CC=C2[N+](CCCCCCCCCC[N+]3=C4C=CC=CC4=C(N)C=C3C)=C(C)C=C(N)C2=C1 LTNZEXKYNRNOGT-UHFFFAOYSA-N 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 10
- 238000004146 energy storage Methods 0.000 abstract description 6
- 238000005338 heat storage Methods 0.000 abstract description 6
- 239000011232 storage material Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 17
- 239000011148 porous material Substances 0.000 description 10
- 238000007711 solidification Methods 0.000 description 10
- 230000008023 solidification Effects 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
- 238000001931 thermography Methods 0.000 description 2
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- 239000004966 Carbon aerogel Substances 0.000 description 1
- 244000157072 Hylocereus undatus Species 0.000 description 1
- 235000018481 Hylocereus undatus Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
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- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
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- 238000011049 filling Methods 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
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- 238000009413 insulation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
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- 239000003208 petroleum Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of phase change energy storage materials, in particular to a preparation method of an MXene/sorghum straw biomass aerogel-based composite phase change material. The method comprises the following steps: soaking sorghum straw in alkali solution, washing to neutrality, and sequentially freeze-drying and carbonizing to obtain porous carbonized sorghum straw; adding porous carbonized sorghum straw and MXene into water, and stirring to obtain a mixture; adding a cross-linking agent into the mixture, stirring to obtain MXene/sorghum straw hydrogel, then freeze-drying, immersing the obtained MXene/sorghum straw biomass aerogel carrier in melted fatty amine, and heating to obtain the MXene/sorghum straw biomass aerogel-based composite phase change material. The MXene/sorghum straw biomass aerogel-based composite phase-change material has the advantages of high heat storage performance, good leakage resistance, environmental protection and low cost, and can be applied to solar heat conversion.
Description
Technical Field
The invention relates to the technical field of phase change energy storage materials, in particular to a preparation method of an MXene/sorghum straw biomass aerogel-based composite phase change material.
Background
With the development of technology, the demand of people for energy is increasing, and the non-renewable resources such as coal, petroleum, natural gas and the like are increasingly exhausted. In the face of energy crisis and ecological deterioration, energy transformation, i.e. development of renewable energy and development and utilization of new energy are urgent. However, new energy sources such as solar energy, wind energy and the like are influenced by factors such as environment, time and the like, and uncertainty exists, so that energy storage is a key technology for solving energy crisis. The phase change material is used as an energy storage medium, and energy is stored and released through a thermal effect in a reversible phase change process, so that the energy utilization rate can be improved, and the energy is effectively utilized. Among them, a biomass material having high porosity, low density, and heat insulation is a typical representative of a wide variety of porous materials, and can be applied to the field of photo-thermal conversion. The pure biomass material has poor light absorption capacity, and can not meet the requirements of the light-heat conversion material on the light-heat conversion efficiency. Leakage, low thermal conductivity remain major problems limiting the application of phase change materials.
Disclosure of Invention
Based on the above, the invention provides a preparation method of the MXene/sorghum straw biomass aerogel-based composite phase-change material. The invention uses the MXene/sorghum straw biomass aerogel as the carrier to load the phase change material, and can effectively improve the heat conductivity of the composite phase change material on the basis of ensuring the stability and heat storage capacity of the composite phase change material.
In order to achieve the above object, the present invention provides the following solutions:
according to one of the technical schemes, the preparation method of the MXene/sorghum straw biomass aerogel-based composite phase-change material comprises the following steps:
soaking sorghum straw in alkali solution, washing to neutrality, and sequentially freeze-drying and carbonizing to obtain porous carbonized sorghum straw;
adding the porous carbonized sorghum straw and MXene into water and stirring to obtain a mixture;
adding a cross-linking agent into the mixture, and stirring to obtain MXene/sorghum straw hydrogel;
freeze-drying the MXene/sorghum straw hydrogel to obtain an MXene/sorghum straw biomass aerogel carrier;
and immersing the MXene/sorghum straw biomass aerogel carrier in melted fatty amine, and then performing heating treatment to obtain the MXene/sorghum straw biomass aerogel-based composite phase-change material.
According to the second technical scheme, the MXene/sorghum straw biomass aerogel-based composite phase-change material is prepared by the preparation method.
In the third technical scheme of the invention, the application of the MXene/sorghum straw biomass aerogel-based composite phase-change material in solar heat conversion is provided.
According to the invention, by combining the three-dimensional framework material with the organic phase change material, not only can the leakage problem of the phase change material be solved, but also the heat conductivity of the phase change material can be improved, and the porous material has an excellent structure, has higher pore volume, specific surface area and storage capacity, and also has excellent adsorption performance, so that the phase change material can be easily combined into the pores. The phase change material is fixed in the supporting matrix due to various forces such as van der Waals force, hydrogen bond, surface tension and the like, so that the phase change material is prevented from leaking from the pores, and the porous material is responsible for maintaining the overall morphology of all structures in the phase change process. Thus, the phase change material is combined with the supporting matrix, and the heat conduction performance and chemical stability of the phase change material are possibly improved, and the packaging performance and the heat conduction performance of the phase change energy storage material are improved.
The invention discloses the following technical effects:
according to the invention, the MXene and the carbonized sorghum straw are mixed to form the three-dimensional framework structure, so that the interface thermal resistance is effectively reduced, and a rapid heat transfer channel is opened up for loading the phase change material, thereby effectively improving the heat conductivity of the composite material, and effectively improving the filling rate, the photo-thermal conversion efficiency and the leakage performance of the composite phase change material.
The invention firstly adopts directional freeze drying to obtain the MXene/sorghum straw biomass aerogel carrier, and then prepares the saturated-load composite phase-change material by using a vacuum impregnation method, and the preparation method is simple, low in cost and environment-friendly.
The MXene/sorghum straw biomass aerogel-based composite phase-change material prepared by the method has the advantages of good heat storage performance, good leakage resistance, environmental protection and low cost, and can be applied to the aspect of solar heat conversion.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a Scanning Electron Microscope (SEM) image of a cross section of sorghum stalks used in example 1; wherein, the left image is a low-magnification SEM image, and the right image is a high-magnification SEM image.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the porous carbonized sorghum stalks obtained in step 3 of example 1.
Fig. 3 is a Scanning Electron Microscope (SEM) image of the MXene/sorghum straw biomass aerogel carrier obtained in step 6 of example 1.
FIG. 4 is a Differential Scanning Calorimeter (DSC) diagram of a composite phase change material based on the biomass aerogel of the MXene/sorghum straw obtained in example 1 and the product of the composite phase change material (corresponding to the product of the process of producing the biomass aerogel of the MXene/sorghum straw) from the sample; the left graph is the tetramine, and the right graph is the MXene/sorghum straw biomass aerogel-based composite phase-change material.
FIG. 5 is an infrared thermal imaging of the MXene/sorghum straw biomass aerogel-based composite phase change material obtained in example 1.
Fig. 6 is a photo-thermal conversion image of the composite phase change material (corresponding to the decamine/MXene/sorghum straw in the figure) based on biomass aerogel of the decamine and MXene/sorghum straw obtained in example 1.
FIG. 7 is a graph showing the thermal conductivity of the composite phase change material based on biomass aerogel of MXene/sorghum straw obtained in example 1 and of the material (corresponding to the material of the graph).
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
In the present invention, "%" indicates mass percent unless otherwise specified.
The term "normal temperature" as used herein refers to 15-30deg.C unless otherwise specified.
The invention provides a preparation method of an MXene/sorghum straw biomass aerogel-based composite phase-change material, which comprises the following steps:
soaking sorghum straw in alkali solution, washing to neutrality, and sequentially freeze-drying and carbonizing to obtain porous carbonized sorghum straw;
adding the porous carbonized sorghum straw and MXene into water and stirring to obtain a mixture;
adding a cross-linking agent into the mixture, and stirring to obtain MXene/sorghum straw hydrogel;
freeze-drying the MXene/sorghum straw hydrogel to obtain an MXene/sorghum straw biomass aerogel carrier;
and immersing the MXene/sorghum straw biomass aerogel carrier in melted fatty amine, and then performing heating treatment to obtain the MXene/sorghum straw biomass aerogel-based composite phase-change material.
The introduction of carbonized sorghum straw can not only increase the porosity and specific surface area of the carrier, but also improve the photo-thermal conversion efficiency of the phase-change material by doping MXene filler, and the synergistic effect of the two aspects can stably load more phase-change materials, thereby improving the stability and heat storage capacity of the formed composite material. On the basis, a directional freeze drying technology is adopted to prepare the MXene/sorghum straw biomass aerogel. The large-size carbon micrometer sheet layer can effectively reduce interface thermal resistance, and meanwhile, the anisotropic structure is beneficial to heat conduction along an ordered channel, so that heat transfer efficiency is improved. Therefore, the thermal conductivity of the composite phase change material can be effectively improved on the basis of ensuring the stability and the heat storage capacity of the composite phase change material by constructing the MXene/sorghum straw biomass aerogel-based carrier.
In a preferred embodiment of the invention, the alkaline solution is 8mol/L sodium hydroxide alkaline solution, and the soaking time is 24 hours; the washing to neutrality is concretely to adopt hydrochloric acid and deionized water to wash until the solution is neutral.
The purpose of the alkaline solution soaking is to activate the sorghum straw to form holes, thereby increasing the porosity of the sorghum straw. Too high a concentration of alkali solution will affect the reduction of the average pore size, too low a concentration will reduce the specific surface area of sorghum straw, and 8mol/L sodium hydroxide alkali solution is selected as the optimal concentration. Too long or too short soaking time can also affect the specific surface area and pore size of sorghum straw.
And after the sorghum straw is soaked in the alkali solution, washing to be neutral, and then sequentially performing freeze-drying and carbonization treatment, wherein the time of freeze-drying is 2 days in the step of obtaining the porous carbonized sorghum straw.
In a preferred embodiment of the invention, the fatty amine is decamine.
In a preferred embodiment of the invention, the carbonization treatment is in particular a heat preservation for 2-4 hours at 800-1000 ℃ under an inert atmosphere.
The carbonization treatment can successfully increase the porosity and specific surface area of the subsequent carbon aerogel, and meanwhile, the doping of MXene is beneficial to improving the photo-thermal conversion efficiency of the composite material.
In a preferred embodiment of the invention, the concentration of porous carbonized sorghum stalks in the mixture is 50-100mg/mL; the concentration of MXene in the mixture is 2-6mg/mL.
The concentration of porous carbonized sorghum stalks and the concentration of MXene in the mixture are defined as the reasons for the above parameter ranges: while the latent heat of the composite material is not reduced, the heat conductivity of the composite material is ensured, the porous carbonized sorghum straw is used as a supporting material, the concentration of the porous carbonized sorghum straw is optimally selected to be 50-100mg/mL, the heat conductivity of the porous carbonized sorghum straw can be influenced by the too high concentration of the porous carbonized sorghum straw, and the latent heat of the porous carbonized sorghum straw can be influenced by the too low concentration of the porous carbonized sorghum straw; as the heat conduction agent, the MXene can enhance the heat conduction coefficient, the increase of the heat conduction coefficient of the composite phase change material is not obvious due to the too low concentration of the MXene, and the latent heat of the composite phase change material can be influenced due to the too high concentration, so that the concentration of the MXene is determined to be 2-6mg/mL according to the comprehensive heat conductivity and the latent heat effect.
In a preferred embodiment of the invention, the cross-linking agent is a mixture of citric acid and disodium hydrogen phosphate in a mass ratio of 1:1; the mass ratio of the cross-linking agent to the porous carbonized sorghum straw is 1:2.
Carboxyl in citric acid in the cross-linking agent can be esterified with hydroxyl on the surface of MXene, and disodium hydrogen phosphate can be cross-linked with carbonized straws to form a network structure. The two are compounded to be used as the cross-linking agent, and compared with the single citric acid or disodium hydrogen phosphate which is used as the cross-linking agent, the cross-linking effect is better.
The ratio of citric acid to disodium hydrogen phosphate in the cross-linking agent and the ratio of the cross-linking agent to the porous carbonized sorghum straw are limited to the above parameters, so that the cross-linking effect is optimal, and the higher or lower numerical value of the ratio can lead to looser structure and lower strength of the prepared MXene/sorghum straw biomass aerogel.
The invention uses citric acid and sodium dihydrogen phosphate to induce MXene and carbonized sorghum straw to crosslink to prepare hydrogel, and on the basis, the MXene/sorghum straw biomass aerogel is prepared by adopting a directional freeze drying method; finally, vacuum impregnation is adopted to load the tetramine as a phase change material, and aliphatic amine series with large latent heat and a series of melting points is selected as a loaded phase change material, so that the application range of the composite material can be widened.
In a preferred embodiment of the present invention, the method further comprises the step of standing the MXene/sorghum straw hydrogel for 4 hours before freeze-drying the MXene/sorghum straw hydrogel; the MXene/sorghum straw hydrogels were freeze-dried for 2 days.
The purpose of standing at room temperature is to form a gel.
In a preferred embodiment of the invention, the impregnation is specifically: immersing in vacuum at 60-70deg.C for 12-24 hr.
The impregnation temperature needs to be higher than the phase change temperature of the phase change material, the impregnation time is selected to be 12-24 hours for the phase change material to be impregnated sufficiently, and the short impregnation time can lead to insufficient impregnation of the phase change material, so that the latent heat of the composite material is affected.
In a preferred embodiment of the present invention, the temperature of the heating treatment is 60℃and the time is 1 hour.
The purpose of the heat treatment is to remove tetradecylamine that is not stably adsorbed.
The second aspect of the invention provides an MXene/sorghum straw biomass aerogel-based composite phase-change material prepared by the preparation method.
The third aspect of the invention provides an application of the MXene/sorghum straw biomass aerogel-based composite phase change material in solar heat conversion.
The raw materials used in the examples of the present invention, unless otherwise specified, were all available commercially.
The MXene used in the embodiments of the present invention is specifically Ti 3 C 2 -MXene powder prepared by the steps of: will be 1g Ti 3 AlC 2 Adding 10mL of 40% HF, stirring at normal temperature for 24h, centrifuging at 3500r/min for 5min, collecting precipitate, repeatedly washing and centrifuging until pH is greater than 6, and collecting precipitate; finally, freeze-drying to obtain black Ti 3 C 2 -MXene powder.
The invention is further illustrated by the following examples.
Example 1
Step 1, weighing a certain amount of sorghum straw (SEM image is shown in figure 1), and soaking in 200mL of 8mol/L sodium hydroxide solution for one day;
step 2, washing the soaked sorghum straw with hydrochloric acid and deionized water until the solution is neutral, and then freeze-drying for 2 days;
step 3, carrying out high-temperature treatment on the product obtained after freeze drying in the step 2 for 2 hours at 800 ℃ in an argon atmosphere to obtain porous carbonized sorghum stalks (SEM images are shown as figure 2);
step 4, weighing 0.5g of the porous carbonized sorghum straw and MXene prepared in the step 3, adding the porous carbonized sorghum straw and the MXene into 10mL of water (the concentration of the MXene in the water is 2 mg/mL), and then vigorously stirring to obtain a clear solution;
step 5, weighing 0.25g of a mixture of citric acid and disodium hydrogen phosphate in a mass ratio of 1:1, adding the mixture into the solution in the step 4, and vigorously stirring the mixture for 2 hours to obtain MXene/sorghum straw hydrogel;
step 6, placing the hydrogel in the step 5 in a polytetrafluoroethylene mould, standing for 4 hours, and then freeze-drying for 2 days to obtain the MXene/sorghum straw biomass aerogel carrier (SEM image is shown in figure 3);
step 7, weighing a certain amount of tetradecylamine and melting to obtain liquid;
step 8, soaking the MXene/sorghum straw biomass aerogel carrier prepared in the step 6 in the liquid in the step 7, and placing the carrier in a vacuum drying oven for vacuum impregnation: maintaining at 60 ℃ for 12 hours in a vacuum environment;
and 9, taking out the material immersed in the step 8, and continuously heating at 60 ℃ for 1 hour to remove the tetradecylamine which is not stably adsorbed, thus obtaining the MXene/sorghum straw biomass aerogel-based composite phase-change material with the saturated load of the tetracmine.
The enthalpy and thermal conductivity of composite phase change material thermal management applications are important, and considering that varying the MXene content of the carrier can vary the force between the carrier and tetradecylamine, the carrier is specifically varied by adjusting the ratio of MXene in example 1, and a Differential Scanning Calorimeter (DSC) is used to measure the enthalpy. On the other hand, the thermal conductivity of the composite phase-change material depends on the structure of the carrier, so that MXene/sorghum straw biomass aerogel carriers with different proportions are prepared and carried with tetramine as a comparative example, an infrared thermal imager is adopted to directly observe the temperature change of the composite phase-change material, and a xenon lamp is used for simulating a sunlight system to test and calculate the photo-thermal conversion efficiency of the composite phase-change material.
FIG. 4 is a DSC melting, solidification curve and enthalpy value of the composite material of the biomass aerogel based on the MXene/sorghum straw obtained in example 1 (corresponding to the melting, solidification curve and enthalpy value of the composite material of the biomass aerogel based on the sorghum straw of the MXene/sorghum straw in the figure), wherein the construction of the composite material can reduce the enthalpy value, the solidification temperature of the composite material of the biomass aerogel based on the MXene/sorghum straw is 29.03 ℃, the solidification latent heat is 180.1J/g, and the solidification latent heat of the pure tetradecylamine phase change material is 207.9J/g.
FIG. 5 is an infrared thermal imaging of the MXene/sorghum straw biomass aerogel-based composite phase change material obtained in example 1. Compared with pure tetramine, the MXene/sorghum straw biomass aerogel-based composite phase-change material prepared by the method disclosed by the invention is more sensitive to temperature reaction under the same condition. The phase-change composite material obtained by the invention has higher heat conductivity, and the anisotropic carrier is beneficial to heat rapid conduction.
Fig. 6 is a photo-thermal conversion performance graph of the biomass aerogel-based composite phase change material (corresponding to the decamine/MXene/sorghum straw in the graph) of MXene/sorghum straw obtained in example 1. FIG. 6 shows that the photo-thermal conversion efficiency of the MXene/sorghum straw biomass aerogel-based composite phase-change material obtained in example 1 is as high as 91.7%.
FIG. 7 is a graph showing the thermal conductivity of the composite phase change material based on the biomass aerogel of MXene/sorghum straw obtained in example 1 and the thermal conductivity of the composite phase change material based on the biomass aerogel of MXene/sorghum straw obtained in example 1 (corresponding to the graph), wherein the thermal conductivity of the composite phase change material based on the biomass aerogel of MXene/sorghum straw is 0.408W/mK, which is 1.55 times that of the composite phase change material based on the biomass of the MXene/sorghum straw.
Example 2
Step 1, the same as in example 1, step 1;
step 2, the same as step 2 of example 1;
step 3, the same as step 3 of example 1;
step 4, weighing 0.5g of the porous carbonized sorghum straw prepared in the step 3 and 4mg/mL of MXene, adding the porous carbonized sorghum straw and the 4mg/mL of MXene into 10mL of water, and then vigorously stirring to obtain a clear solution;
step 5, same as step 5 of example 1;
step 6, the same as step 6 of example 1;
step 7, same as step 7 of example 1;
step 8, same as step 8 of example 1;
step 9, same as step 9 of example 1.
Example 3
Step 1, the same as in example 1, step 1;
step 2, the same as step 2 of example 1;
step 3, the same as step 3 of example 1;
step 4, weighing 0.5g of the porous carbonized sorghum straw prepared in the step 3 and 6mg/mL of MXene, adding the porous carbonized sorghum straw and 6mg/mL of MXene into 10mL of water, and then vigorously stirring to obtain a clear solution;
step 5, same as step 5 of example 1;
step 6, the same as step 6 of example 1;
step 7, same as step 7 of example 1;
step 8, same as step 8 of example 1;
step 9, same as step 9 of example 1.
Example 4
Step 1, the same as in example 1, step 1;
step 2, the same as step 2 of example 1;
step 3, the same as step 3 of example 1;
step 4, 1.0g of the porous carbonized sorghum straw prepared in the step 3 and 6mg/mL of MXene are weighed and added into 10mL of water, and then the mixture is vigorously stirred to obtain a clear solution;
step 5, weighing 0.5g of a mixture of citric acid and disodium hydrogen phosphate in a mass ratio of 1:1, adding the mixture into the solution in the step 4, and vigorously stirring the mixture for 2 hours to obtain MXene/sorghum straw hydrogel;
step 6, the same as step 6 of example 1;
step 7, same as step 7 of example 1;
step 8, same as step 8 of example 1;
step 9, same as step 9 of example 1.
Comparative example 1
The only difference from example 1 is that in step 5, 0.25g of citric acid was weighed into the solution of step 4 and vigorously stirred for 2 hours to give a MXene/sorghum straw hydrogel. The remaining procedure parameters were the same as in example 1.
The effect verification of the MXene/sorghum straw biomass aerogel-based composite phase-change material prepared in the comparative example is carried out in the same way as in the example 1, and the result shows that the solidification temperature of the MXene/sorghum straw biomass aerogel-based composite phase-change material is 27.52 ℃, the solidification latent heat is 160.9J/g, the photo-thermal conversion efficiency is 89.4%, and the heat conductivity coefficient is 0.328W/mK.
Comparative example 2
The difference from example 1 was only that in step 5, 0.25g of disodium hydrogen phosphate was weighed into the solution of step 4 and vigorously stirred for 2 hours to give an MXene/sorghum straw hydrogel. The remaining procedure parameters were the same as in example 1.
The effect verification of the MXene/sorghum straw biomass aerogel-based composite phase-change material prepared in the comparative example is carried out in the same way as in the example 1, and the result shows that the solidification temperature of the MXene/sorghum straw biomass aerogel-based composite phase-change material is 27.21 ℃, the solidification latent heat is 149.7J/g, the photo-thermal conversion efficiency is 85%, and the heat conductivity coefficient is 0.335W/mK.
The invention also tries to replace the sorghum straw biomass material with other biomass materials, such as dragon fruit peel, rice straw and the like, and the result shows that the solidification latent heat, the photo-thermal conversion efficiency and the heat conductivity coefficient of the composite phase change material prepared by using other biomass materials are not the same as those of the composite phase change material prepared by taking the sorghum straw as the raw material, which is probably caused by the special microscopic morphology of the sorghum straw.
According to the invention, the sorghum straw biomass material with low price is selected to be combined with the organic phase change material, the derivative porous carbon provides a large specific surface area for the adhesion of fatty amine (tetradecylamine), so that the interfacial thermal resistance is effectively reduced, an effective heat transfer path and a continuous channel are provided for phonon propagation, the MXene nano-sheet is introduced to further play a role in enhancing heat transfer, and the carbonized sorghum straw after being treated by an alkali solution has excellent adsorption performance, so that the phase change material can be easily combined into pores, and the phase change material is prevented from leaking from the pores. Therefore, the phase change material is not only jointed with the supporting matrix, but also can improve the heat conduction performance and chemical stability, improve the packaging performance of the phase change energy storage material, and also can retain the heat storage capacity of the phase change material to a great extent.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (10)
1. The preparation method of the MXene/sorghum straw biomass aerogel-based composite phase-change material is characterized by comprising the following steps of:
soaking sorghum straw in alkali solution, washing to neutrality, and sequentially freeze-drying and carbonizing to obtain porous carbonized sorghum straw;
adding the porous carbonized sorghum straw and MXene into water and stirring to obtain a mixture;
adding a cross-linking agent into the mixture, and stirring to obtain MXene/sorghum straw hydrogel;
freeze-drying the MXene/sorghum straw hydrogel to obtain an MXene/sorghum straw biomass aerogel carrier;
and immersing the MXene/sorghum straw biomass aerogel carrier in melted fatty amine, and then performing heating treatment to obtain the MXene/sorghum straw biomass aerogel-based composite phase-change material.
2. The method for preparing the MXene/sorghum straw biomass aerogel-based composite phase change material according to claim 1, wherein the carbonization treatment is specifically carried out in an inert atmosphere at 800-1000 ℃ for 2-4 hours.
3. The method for preparing the MXene/sorghum straw biomass aerogel-based composite phase change material according to claim 1, characterized in that the concentration of porous carbonized sorghum straw in the mixture is 50-100mg/mL; the concentration of MXene in the mixture is 2-6mg/mL.
4. The method for preparing the MXene/sorghum straw biomass aerogel-based composite phase change material according to claim 1, wherein the cross-linking agent is a mixture of citric acid and disodium hydrogen phosphate in a mass ratio of 1:1; the mass ratio of the cross-linking agent to the porous carbonized sorghum straw is 1:2.
5. The method for preparing the MXene/sorghum straw biomass aerogel based composite phase change material according to claim 1, characterized in that the time for freeze drying the MXene/sorghum straw hydrogel is 2 days.
6. The method for preparing the MXene/sorghum straw biomass aerogel-based composite phase-change material according to claim 1, characterized in that the impregnation is specifically: immersing in vacuum at 60-70deg.C for 12-24 hr.
7. The method for preparing the MXene/sorghum straw biomass aerogel-based composite phase-change material according to claim 1, characterized in that the temperature of the heating treatment is 60 ℃ for 1 hour.
8. The method for preparing the MXene/sorghum straw biomass aerogel-based composite phase-change material according to claim 1, characterized in that the fatty amine is decamine.
9. The MXene/sorghum straw biomass aerogel-based composite phase-change material prepared by the preparation method according to any one of claims 1-8.
10. The use of an MXene/sorghum straw biomass aerogel based composite phase change material according to claim 9 for solar thermal conversion.
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