CN114196381A - High-energy-storage-density phase-change material and preparation method thereof - Google Patents
High-energy-storage-density phase-change material and preparation method thereof Download PDFInfo
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- CN114196381A CN114196381A CN202111673293.6A CN202111673293A CN114196381A CN 114196381 A CN114196381 A CN 114196381A CN 202111673293 A CN202111673293 A CN 202111673293A CN 114196381 A CN114196381 A CN 114196381A
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- 239000012782 phase change material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000004146 energy storage Methods 0.000 title claims abstract description 12
- 240000007182 Ochroma pyramidale Species 0.000 claims abstract description 41
- 239000004964 aerogel Substances 0.000 claims abstract description 36
- 229920002678 cellulose Polymers 0.000 claims abstract description 25
- 239000001913 cellulose Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000011069 regeneration method Methods 0.000 claims abstract description 12
- 230000008929 regeneration Effects 0.000 claims abstract description 9
- 238000003763 carbonization Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 claims description 20
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 claims description 20
- 235000021360 Myristic acid Nutrition 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002023 wood Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229920005610 lignin Polymers 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000011162 core material Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 239000000835 fiber Substances 0.000 abstract description 7
- 239000002121 nanofiber Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000004627 regenerated cellulose Substances 0.000 abstract description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 210000002421 cell wall Anatomy 0.000 description 5
- 238000002135 phase contrast microscopy Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- MTJGVAJYTOXFJH-UHFFFAOYSA-N 3-aminonaphthalene-1,5-disulfonic acid Chemical compound C1=CC=C(S(O)(=O)=O)C2=CC(N)=CC(S(O)(=O)=O)=C21 MTJGVAJYTOXFJH-UHFFFAOYSA-N 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 229920001046 Nanocellulose Polymers 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005338 heat storage Methods 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
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000002025 wood fiber Substances 0.000 description 1
Images
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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
Abstract
The invention relates to the technical field of materials, in particular to a high-energy-storage-density phase-change material and a preparation method thereof. The invention adopts a cellulose reinforced regeneration method to prepare the regenerated cellulose network balsa wood aerogel, and the balsa wood block is soaked in a simple ethanol regeneration bath to have a regenerated nano fiber network structure with high specific surface area and high porosity. And finally, further modifying the regenerated fiber network by high-temperature carbonization, and optimizing the internal structure, the surface porosity and the heat conductivity coefficient of the regenerated fiber network again. The reinforced regenerated fiber skeleton is used as a support material, so that the shape-stabilized phase change material has better mechanical support performance, high enthalpy value, high heat conduction and high photothermal conversion performance. The whole preparation process of the invention has the advantages of economy, high efficiency, environmental protection.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a high-energy-storage-density phase-change material and a preparation method thereof.
Background
A phase change material is a substance that is capable of undergoing a phase change behavior in a specific narrow temperature range, which is a phase change phenomenon from one state to another, and stores and releases latent heat during the phase change. The organic phase-change material has the advantages of good thermal reliability, chemical stability, corrosion resistance, high energy storage density, low supercooling and the like, but the heat conductivity coefficient is low, so that the practical application of the organic phase-change material is hindered, and the energy charge and discharge rate of the phase-change material is easily reduced. One solution is to combine a porous scaffold with a phase change material to produce a shaped phase change material. Various porous carriers for supporting organic phase change materials, such as foamed metal, graphite porous material, carbon aerogel, graphene, porous carbon, etc., have been developed. However, the current preparation process of the porous carrier still has the defects of high process cost, large environmental pollution caused by the preparation process and the like.
Disclosure of Invention
The invention adopts a cellulose reinforced regeneration method to prepare the regenerated cellulose network balsa wood aerogel, and the balsa wood block is soaked in a simple ethanol regeneration bath to have a regenerated nano fiber network structure with high specific surface area and high porosity. And finally, further modifying the regenerated fiber network by high-temperature carbonization, and optimizing the internal structure, the surface porosity and the heat conductivity coefficient of the regenerated fiber network again. The reinforced regenerated fiber skeleton is used as a support material, so that the shape-stabilized phase change material has better mechanical support performance, high enthalpy value, high heat conduction and high photothermal conversion performance. The whole preparation process of the invention has the advantages of economy, high efficiency, environmental protection.
Specifically, the preparation method of the high energy storage density phase-change material comprises the following steps:
1) pretreatment of balsa wood
Completely soaking the dried balsa blocks in distilled water for 24 hours, and placing the completely soaked balsa blocks in NaClO2In the solution, the pH of the solution is adjusted to 4.6 by acetic acid; heating in 100 deg.C water bath for 6 hr to remove lignin, washing the wood blocks with deionized water, and boiling until the yellow green color of the wood blocks gradually turns to colorless;
2) preparation of cellulose reinforced regenerated balsawood aerogel
The cleaned delignified pieces were transferred to NaOH (7 wt%)/CH4N2Dissolving cellulose in O (12 wt%) solution, and then soaking part of the dissolved wood blocks into 30ml of absolute ethyl alcohol for cellulose regeneration; washing the regenerated Basha wood blocks with deionized water, and freeze-drying at-60 deg.C for 48h to obtain cellulose regenerated aerogel; finally, the aerogel is placed at a temperature of 450 DEG CCarrying out high-temperature carbonization;
3) preparation of novel composite shape-stabilized phase-change material
The preparation method comprises the following steps of preparing a novel composite shape-stabilized phase change material by using myristic acid as a core material and carbonized cellulose-reinforced regenerated balsawood aerogel as a carrier, and specifically comprising the following steps: putting myristic acid in a water bath kettle at 80 ℃ and heating until the myristic acid is completely melted, then putting the carbonized cellulose reinforced regenerated balsawood aerogel in a melted myristic acid beaker, and carrying out the whole impregnation process in a vacuum oven.
Preferably, the size of the balsa wood in the step 1) is 15mm × 15mm × 10 mm.
Preferably, NaClO is used in the step 1)2The concentration of the solution was 1 wt%.
Preferably, the Basha wood and NaClO in the step 1)2The weight to volume ratio of the solution was 3:250 g/ml.
Preferably, the delignified block in step 2) is mixed with NaOH (7 wt%)/CH4N2The weight to volume ratio g/ml of the O (12 wt%) solution was 1.05: 50.
Preferably, the mass ratio of the myristic acid to the cellulose-reinforced regenerated balsawood aerogel in the step 3) is 9.1: 1.
The method removes part of cellulose and hemicellulose in the balsawood by a cellulose reinforced regeneration method, and regulates the surface performance and the pore structure of the balsawood under proper treatment time and dissolution concentration by an ethanol regeneration technology to enable a nano-fiber network structure to grow in the cell walls of the balsawood blocks. Compared with untreated balsa wood, the cellulose-reinforced regenerated balsa wood aerogel combines undissolved fibers in cell walls, effectively obtaining higher specific surface area, better mechanical stability and higher extrudability. And then carbonizing the balsawood aerogel after the cellulose strengthening regeneration at high temperature to obtain the high-heat-conductivity carbonized balsawood aerogel, wherein the high-heat-conductivity carbonized balsawood aerogel still retains rich internal nanofiber network structures, and the high-heat-conductivity high-load-rate novel shape-stabilized phase change material is prepared by taking the balsawood aerogel as a carrier. The combination of the high-performance carbonized balsa aerogel enables the novel shape-stabilized phase change material to have higher temperature rise rate and higher heat transfer rate under the same illumination condition. And the strong capillary force and van der waals force generated by the regenerated nanofiber network structure make the novel shaped phase change material have excellent latent heat and high encapsulation stability. More importantly, due to the green preparation process and the low-cost synthesis strategy, the energy consumption and the influence of chemicals on water can be effectively reduced.
Drawings
FIG. 1 is an SEM image of untreated balsa wood in the examples.
Fig. 2 is an SEM image of balsa wood after removal of lignin in the examples.
FIG. 3 is an SEM image of cellulose-reinforced regenerated balsa aerogel in the examples.
FIG. 4 shows the results of the thermal difference analysis in examples.
FIG. 5 shows the thermogravimetric analysis results in the examples.
Detailed Description
The following examples are intended to further illustrate the present invention, but they are not intended to limit or restrict the scope of the invention. NaOH (7 wt%)/CH4N2Preparation of O (12 wt%) solution: 81ml of deionized water, 7g of NaOH, 12gCH4N2O。
Examples
1) Pretreatment of balsa wood
Completely soaking dried Barsha wood blocks 15mm by 10mm about 0.6g in distilled water for 24 hr, and placing the completely soaked Barsha wood blocks in 50ml of NaClO2In the solution, the pH of the solution is adjusted to 4.6 by acetic acid; heating in 100 deg.C water bath for 6 hr to remove lignin, washing the wood blocks with deionized water, and boiling until the yellow green color of the wood blocks gradually turns to colorless; the SEM image is shown in FIG. 2. The lignified cell wall at this time has a hollow structure, and the inside is very clean and tidy without fillers. SEM images of untreated balsa wood are shown in figure 1.
2) Preparation of cellulose reinforced regenerated balsawood aerogel
1.05g of the washed delignified cake were transferred to 50ml NaOH (7 wt%)/CH4N2Dissolving cellulose in O (12 wt%) solution, and then soaking part of the dissolved wood blocks into 30ml of absolute ethyl alcohol for cellulose regeneration; washing the regenerated Basha wood blocks with deionized water, and freeze-drying at-60 deg.C for 48h to obtain cellulose regenerated aerogel; finally, putting the aerogel at the temperature of 450 ℃ for high-temperature carbonization; the SEM image is shown in FIG. 3. The hollow interior of the lignified cell wall is filled with the nanocellulose network, so that the capillary force and the van der Waals force are improved, the organic phase-change material can be better adsorbed, and a better continuous heat conduction channel is provided for the phase-change material.
SEM results show that the balsa wood with lignin removed has cleaner texture and the wood fiber is clearer by comparing the figure 1 and the figure 2. In NaOH/CH4N2Under the action of the O solution, the cellulose in the balsa wood is partially dissolved, and after the treatment with absolute ethanol, the dissolved cell walls are regenerated in the absolute ethanol, resulting in the reformation of intermolecular hydrogen bonds and the coagulation of the dissolved cellulose chains, and the flocculation and highly porous nanofiber network structure is regenerated in situ in the cavity (fig. 3).
3) Preparation of novel composite shape-stabilized phase-change material
The preparation method comprises the following steps of preparing a novel composite shape-stabilized phase change material by taking myristic acid as a core material and taking carbonized cellulose-reinforced regenerated balsawood aerogel as a carrier (the mass ratio of the myristic acid to the cellulose-reinforced regenerated balsawood aerogel is 9.1: 1), and specifically comprises the following steps: 15g of myristic acid is placed in a water bath kettle at 80 ℃ and heated to be completely melted, then the carbonized cellulose reinforced regenerated balsawood aerogel is placed in a beaker of melted myristic acid, and the whole impregnation process is carried out in a vacuum oven.
Thermal difference analysis step: 10mg of pure myristic acid is placed in an aluminum crucible, nitrogen is used as protective gas at the temperature of 0-120 ℃, and the heating and cooling rates are the same and are 10 ℃/min. Similarly, the above process was repeated with 10mg of cellulose reinforced regenerative aerogel shape-stabilized phase change material, and the heat storage performance during heat absorption and heat release was tested.
The results of the thermal difference analysis show that: curve 1 of pure myristic acid shows a melting peak at 54.2 ℃ with a melting enthalpy of 246.9J/g, a crystallization peak at 47.5 ℃ and a solidification enthalpy of 246.8J/g. The cellulose reinforced regeneration aerogel shaping phase-change material shows a melting peak at 52.8 ℃, the melting enthalpy is 190.3J/g, an exothermic crystallization peak at 70.5 ℃, and the solidification enthalpy is 184.7J/g. The cellulose reinforced regeneration aerogel shape-stabilized phase change material is loaded with a large amount of myristic acid molecules, and the enthalpy value reaches to 190J/g (the enthalpy value of myristic acid is 246J/g).
Thermogravimetric analysis step: 20mg of the reinforced regenerated aerogel PCMs are placed in an aluminum crucible, and the thermal stability and the performance of the reinforced regenerated aerogel PCMs are tested by using a thermogravimetric analyzer at the temperature of 5-700 ℃ in a nitrogen atmosphere.
The thermogravimetric analysis results show that: the thermal stability of the enhanced regenerated aerogel PCMs was analyzed by using thermogravimetric analysis, and it can be seen from the thermogravimetric plot that weight loss starts from 113 ℃, myristic acid in the enhanced regenerated aerogel PCMs starts to decompose rapidly after the temperature reaches 164 ℃, and myristic acid is completely decomposed when the temperature rises to 550 ℃, leaving 9.8% of residue. It can be found that the reinforced regenerated aerogel PCMs have excellent thermal stability, start to be rapidly decomposed at 164 ℃, and finally leave only 9.8% of residues, so that about 90% of myristic acid is adsorbed in the porous reinforced regenerated aerogel, and excellent loading rate and high enthalpy value are represented.
Claims (6)
1. A preparation method of a phase-change material with high energy storage density is characterized by comprising the following steps:
1) pretreatment of balsa wood
Completely soaking the dried balsa blocks in distilled water for 24 hours, and placing the completely soaked balsa blocks in NaClO2In the solution, the pH of the solution is adjusted to 4.6 by acetic acid; heating in 100 deg.C water bath for 6 hr to remove lignin, washing the wood blocks with deionized water, and boiling until the yellow green color of the wood blocks gradually turns to colorless;
2) preparation of cellulose reinforced regenerated balsawood aerogel
The cleaned delignified pieces were transferred to NaOH (7 wt%)/CH4N2Dissolving cellulose in O (12 wt%) solution, and then soaking part of the dissolved wood blocks into 30ml of absolute ethyl alcohol for cellulose regeneration; washing the regenerated Basha wood blocks with deionized water, and freeze-drying at-60 deg.C for 48h to obtain cellulose regenerated aerogel; finally, putting the aerogel at the temperature of 450 ℃ for high-temperature carbonization;
3) preparation of novel composite shape-stabilized phase-change material
The preparation method comprises the following steps of preparing a novel composite shape-stabilized phase change material by using myristic acid as a core material and carbonized cellulose-reinforced regenerated balsawood aerogel as a carrier, and specifically comprising the following steps: putting myristic acid in a water bath kettle at 80 ℃ and heating until the myristic acid is completely melted, then putting the carbonized cellulose reinforced regenerated balsawood aerogel in a melted myristic acid beaker, and carrying out the whole impregnation process in a vacuum oven.
2. The method for preparing a phase-change material with high energy storage density as claimed in claim 1, wherein the size of the balsa wood in step 1) is 15mm x 10 mm.
3. The method for preparing the phase-change material with high energy storage density as claimed in claim 1, wherein the NaClO is used in the step 1)2The concentration of the solution was 1 wt%.
4. The method for preparing the phase-change material with high energy storage density as claimed in claim 1, wherein the Basha wood and NaClO in the step 1) are prepared by2The weight to volume ratio of the solution was 3:250 g/ml.
5. The method for preparing the phase-change material with high energy storage density as claimed in claim 1, wherein the delignified block in the step 2) is mixed with NaOH (7 wt%)/CH4N2The weight to volume ratio g/ml of the O (12 wt%) solution was 1.05: 50.
6. The method for preparing the phase-change material with high energy storage density according to claim 1, wherein the mass ratio of the myristic acid to the cellulose-reinforced regenerated balsa wood aerogel in the step 3) is 9.1: 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115498358A (en) * | 2022-08-30 | 2022-12-20 | 苏州大学 | Preparation method of cellulose diaphragm for lithium battery |
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2021
- 2021-12-28 CN CN202111673293.6A patent/CN114196381A/en active Pending
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| CN115498358A (en) * | 2022-08-30 | 2022-12-20 | 苏州大学 | Preparation method of cellulose diaphragm for lithium battery |
| CN115498358B (en) * | 2022-08-30 | 2023-12-12 | 苏州大学 | Preparation method of cellulose diaphragm for lithium battery |
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Application publication date: 20220318 |