CN110527495B - Preparation method of composite phase-change material - Google Patents
Preparation method of composite phase-change material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 239000012782 phase change material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920001690 polydopamine Polymers 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000002105 nanoparticle Substances 0.000 claims abstract description 16
- 239000000969 carrier Substances 0.000 claims abstract description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 44
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 239000007853 buffer solution Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 6
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000011162 core material Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims 2
- 229960003638 dopamine Drugs 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 239000011664 nicotinic acid Substances 0.000 abstract description 2
- 230000008859 change Effects 0.000 description 17
- 239000012071 phase Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 238000007605 air drying Methods 0.000 description 3
- 239000000872 buffer Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000008055 phosphate buffer solution Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
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- 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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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
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Abstract
The invention discloses a preparation method of a composite phase-change material, which is characterized in that poly-dopamine nano-particles are synthesized by a bionic method and are used as carriers to prepare a novel composite shape-stabilized phase-change material.
Description
Technical Field
The invention relates to the technical field of composite material processing, in particular to a preparation method of a composite phase-change material.
Background
The organic phase change energy storage material absorbs or emits heat to realize the purpose of absorbing and releasing energy during phase change, has the advantages of high energy storage density, low corrosivity, low toxicity, low cost, convenient use, easy management, good control of system temperature in the phase change process and the like, and is widely applied to the field of energy storage; but the organic phase change material also has the defects of small heat conductivity coefficient, easy leakage and the like. In order to improve the phenomena that the existing organic phase change material and inorganic phase change material are easy to leak, have small heat conductivity coefficient and are easy to be supercooled, the composite phase change material is produced. The composite phase-change material is a new stable phase-change material formed by compounding a single organic or inorganic phase-change material and one or more other functional materials by a specific method, and is mainly divided into three categories of organic-inorganic, inorganic-inorganic and organic-organic according to the difference of the composite materials. Mesoporous materials such as mesoporous silicon and mesoporous carbon have the advantages of large specific surface area, good adsorption performance, high mechanical strength and the like, and the application of the mesoporous materials to the preparation of the shape-stabilized phase change material by using the organic phase change material carrier becomes a current research hotspot. However, the current mesoporous material preparation process still has the defects of complex preparation process, high cost and the like. Therefore, it is necessary to develop a composite phase change material to solve the above problems.
Disclosure of Invention
The invention aims to: a preparation method of the composite phase-change material is provided to solve the problems.
The technical scheme of the invention is as follows:
a preparation method of a composite phase-change material comprises the following steps:
(1) dissolving polydopamine in a phosphoric acid buffer solution at room temperature, stirring, performing suction filtration after reaction is completed to obtain a dark precipitate, and drying the dark precipitate to obtain black powdery polydopamine nanoparticles;
(2) dissolving polyethylene glycol in absolute ethyl alcohol, adding the polydopamine nano-particles after the polyethylene glycol is completely dissolved to form a suspension, carrying out vacuum impregnation on the suspension, stirring, drying, and completely evaporating ethanol to obtain the composite phase change material taking the polyethylene glycol as a core material and the polydopamine nano-particles as carriers.
Further, the preparation method of the phosphoric acid buffer solution in the step (1) comprises the following steps: sodium dihydrogen phosphate and disodium hydrogen phosphate were dissolved in water to prepare a phosphate buffer solution having a pH of 8.5.
Further, the rotating speed of the stirring in the step (1) is 500-700 rpm, and the reaction time is 12-24 h.
Further, the drying temperature in the step (1) is 45-75 ℃, and the drying time is 12-24 hours.
Further, in the step (1), before the drying, the dark-colored precipitate is washed with distilled water for 2 times.
Further, the mass ratio of the polyethylene glycol to the polyethylene glycol + polydopamine in the step (2) is 0.45-0.85.
Further, the dipping time in the step (2) is 1-2 h.
Further, in the step (2), the stirring temperature is 45 ℃, the rotating speed is 500-700 rpm, and the time is 4-8 h.
Further, in the step (2), the drying temperature is 45 ℃ and the drying time is 12-24 hours.
The invention provides a preparation method of a composite phase-change material, which is characterized in that poly-dopamine nano-particles are synthesized by a bionic method and are used as carriers to prepare a novel composite shape-stabilized phase-change material.
Drawings
FIG. 1 is a scanning electron microscope image of polydopamine prepared by the method for preparing the composite phase change material according to the invention;
FIG. 2 is a scanning electron microscope image of a composite phase change material prepared by the method for preparing a composite phase change material according to the present invention;
FIG. 3 is a TEM image of the composite phase change material prepared by the method of the present invention;
FIG. 4 is a transmission electron microscope image of the composite phase change material prepared by the method of the present invention after further enlargement;
FIG. 5 is a wide-angle X-ray diffraction pattern of polyethylene glycol, poly-dopamine nanoparticles, and a composite phase change material in a method for preparing a composite phase change material according to the present invention;
FIG. 6 is a Differential Scanning Calorimetry (DSC) profile of a polyethylene glycol and a composite phase change material in a method for preparing the composite phase change material according to the present invention;
FIG. 7 is a Fourier infrared spectrum of the polyethylene glycol, the polydopamine nanoparticles and the composite phase change material in the preparation method of the composite phase change material.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
A preparation method of a composite phase-change material comprises the following steps:
the method comprises the following steps: dissolving polydopamine in a phosphoric acid buffer solution at room temperature, stirring, performing suction filtration after reaction is completed to obtain a dark precipitate, and drying the dark precipitate to obtain black powdery polydopamine nanoparticles;
this step may be specifically performed as follows: dissolving 0.25-0.5 g of polydopamine in 50-200 mL of phosphoric acid buffer solution as a reaction medium with the pH value of 8.5 in an open container, continuously stirring at the rotating speed of 500-700 rpm, reacting at room temperature (25 ℃) for 12-24 h, performing suction filtration, and drying the obtained dark precipitate (the drying temperature is 45-75 ℃ and the drying time is 12-24 h) to obtain black powdery polydopamine nanoparticles, wherein the preparation method of the phosphoric acid buffer solution comprises the following steps: sodium dihydrogen phosphate and disodium hydrogen phosphate were dissolved in water to prepare a phosphate buffer solution having a pH of 8.5.
Step two: dissolving polyethylene glycol in absolute ethyl alcohol, adding the polydopamine nano-particles after the polyethylene glycol is completely dissolved to form a suspension, carrying out vacuum impregnation on the suspension, stirring, drying, and completely evaporating ethanol to obtain the composite phase change material taking the polyethylene glycol as a core material and the polydopamine nano-particles as carriers.
This step may be specifically performed as follows: preparing a novel composite shape-stabilized phase change material by taking polyethylene glycol as a core material and polydopamine nano-particles as a carrier: dissolving 0.1-0.3 g of polyethylene glycol in 10-15 mL of absolute ethanol, adding 0.05-0.1 g of polydopamine nanoparticles after the polyethylene glycol and the polydopamine are completely dissolved, wherein the mass ratio of the polyethylene glycol to the polyethylene glycol and the polydopamine is 0.45-0.85, carrying out vacuum impregnation operation on suspension formed by the polyethylene glycol and the polydopamine for 1-2 h, stirring the suspension at the temperature of 45 ℃ for 4-8 h at the rotating speed of 500-700 rpm, drying the mixture in a constant-temperature drying oven at the temperature of 45 ℃ for 12-24 h after the suspension is finished, completely evaporating the ethanol, and finally obtaining a solid product, namely the composite phase change material.
The performance of the composite phase change material prepared by the above method is shown in fig. 1 to 7:
as can be seen from fig. 1, 2, 3 and 4, PEG was successfully complexed with the polydopamine carrier PDA.
As can be seen in fig. 5, pure PEG showed two strong diffraction peaks at 19.08 ° and 23.19 °, indicating the highly crystalline structure of the pure PEG material. The diffraction peak positions of the PEG/PDA material of the phase-change composite material are basically the same as those of the pure PEG material, and the peak values are respectively positioned at 19.06 degrees and 23.28 degrees, which shows that the introduction of the mesoporous material does not influence the crystal structure of the PEG, namely the crystallinity of the PEG.
As can be seen from FIG. 6, pure PEG showed an endothermic melting peak at 63.31 ℃ with a melting enthalpy of 195.36J/g, and an exothermic crystallization peak at 35.03 ℃ with a solidification enthalpy of 175.86J/g. Comparative example phase change composite PEG/PDA showed an endothermic melting peak at 63.49 deg.C with a melting enthalpy of 105.12J/g, an exothermic crystallization peak at 32.44 deg.C with a solidification enthalpy of 90.24J/g. Therefore, the phase change composite material PEG/PDA has a higher enthalpy value, which shows that the PEG is fixed by using polydopamine as a carrier to prepare the shape-stabilized phase change material, so that the PEG can be prevented from leaking in the phase change process, and the heat storage performance of the PEG cannot be influenced.
As can be seen from fig. 7, comparing the curve corresponding to the phase change composite PEG/PDA with the curve corresponding to the polydopamine carrier PDA, the curve corresponding to pure PEG, no significant new peak is observed in the curves, which indicates that the interaction between PEG and polydopamine PDA is physical and that the interaction can prevent the phase change composite from leaking out during the phase change process.
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying the present invention are further described below. The invention is not limited to the embodiments listed but also comprises any other known variations within the scope of the invention as claimed.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
The embodiment shows a preparation method of the composite phase-change material according to the following steps:
(1) preparation of phosphoric acid buffer solution
0.072g of sodium dihydrogen phosphate and 1.69g of disodium hydrogen phosphate were dissolved in a 50mL beaker, and the resulting solution was further placed in a 250mL volumetric flask to prepare a phosphoric acid buffer solution having a Ph of 8.5.
(2) Preparation of polydopamine
0.25g polydopamine was dissolved in 50mL phosphoric acid buffer at room temperature and stirred at 500rpm for 12h at room temperature. And after the reaction is finished, carrying out suction filtration, washing with distilled water for 2 times, and drying at 45 ℃ for 12 hours to obtain the polydopamine particles PDA.
(3) Preparation of phase change composite material
And (3) placing 0.3g of PEG in a conical flask, adding 15mL of ethanol solution, adding 0.1g of polydopamine particles, carrying out vacuum impregnation for 1h, then placing the suspension in a 45-DEG C constant-temperature water bath, stirring at the speed of 500rpm for 4h, and drying in a 45-DEG C forced air drying oven for 24h to obtain the phase change composite material PEG/PDA.
Example 2
The embodiment shows a preparation method of the composite phase-change material according to the following steps:
(1) preparation of phosphoric acid buffer solution
0.072g of sodium dihydrogen phosphate and 1.69g of disodium hydrogen phosphate were dissolved in a 50mL beaker, and the resulting solution was further placed in a 250mL volumetric flask to prepare a phosphoric acid buffer solution having a Ph of 8.5.
(2) Preparation of polydopamine
0.4g polydopamine was dissolved in 150mL phosphoric acid buffer at room temperature and stirred at 600rpm for 18h at room temperature. And after the reaction is finished, carrying out suction filtration, washing with distilled water for 2 times, and drying at 60 ℃ for 12 hours to obtain the poly-dopamine particles PDA.
(3) Preparation of phase change composite material
And (3) placing 0.2g of PEG in a conical flask, adding 12mL of ethanol solution, adding 0.08g of polydopamine particles, carrying out vacuum impregnation for 1.5h, then placing the suspension in a 45-DEG C constant-temperature water bath kettle, stirring at the speed of 600rpm for 6h, and drying in a 45-DEG C forced air drying oven for 18h to obtain the phase-change composite material PEG/PDA.
Example 3
The embodiment shows a preparation method of the composite phase-change material according to the following steps:
(1) preparation of phosphoric acid buffer solution
0.072g of sodium dihydrogen phosphate and 1.69g of disodium hydrogen phosphate were dissolved in a 50mL beaker, and the resulting solution was further placed in a 250mL volumetric flask to prepare a phosphoric acid buffer solution having a Ph of 8.5.
(2) Preparation of polydopamine
0.5g polydopamine was dissolved in 200mL phosphoric acid buffer at room temperature and stirred at 700rpm for 24h at room temperature. And after the reaction is finished, carrying out suction filtration, washing with distilled water for 2 times, and drying at 75 ℃ for 18h to obtain the poly-dopamine particles PDA.
(3) Preparation of phase change composite material
And (3) placing 0.1g of PEG in a conical flask, adding 10mL of ethanol solution, adding 0.05g of polydopamine particles, carrying out vacuum impregnation for 2h, then placing the suspension in a 45-DEG C constant-temperature water bath, stirring at 700rpm for 8h, and drying in a 45-DEG C forced air drying oven for 12h to obtain the phase change composite material PEG/PDA.
TABLE 1 comparison of the composite materials of the types
Compared with the prior art, the invention has the beneficial effects that: the preparation method has the advantages of simple operation, mild conditions, no toxicity, low cost and the like.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. The preparation method of the composite phase-change material is characterized by comprising the following steps of:
(1) dissolving dopamine in a phosphoric acid buffer solution at room temperature, stirring, performing suction filtration after reaction is completed to obtain a dark-colored precipitate, and drying the dark-colored precipitate to obtain black powdery polydopamine nanoparticles, wherein the preparation method of the phosphoric acid buffer solution comprises the following steps: dissolving sodium dihydrogen phosphate and disodium hydrogen phosphate in water to prepare a phosphoric acid buffer solution with the pH value of 8.5;
(2) dissolving polyethylene glycol in absolute ethyl alcohol, adding the polydopamine nano-particles after the polyethylene glycol is completely dissolved to form a suspension, carrying out vacuum impregnation on the suspension, stirring, drying, and completely evaporating ethanol to obtain the composite phase change material taking the polyethylene glycol as a core material and the polydopamine nano-particles as carriers.
2. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: in the step (1), the stirring speed is 500-700 rpm, and the reaction time is 12-24 h.
3. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: the drying temperature in the step (1) is 45-75 ℃, and the drying time is 12-24 hours.
4. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: in the step (1), before drying, the dark precipitate is washed for 2 times by distilled water.
5. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: in the step (2), the mass ratio of the polyethylene glycol to the polyethylene glycol + polydopamine is 0.45-0.85.
6. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: and (3) soaking for 1-2 h in the step (2).
7. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: in the step (2), the stirring temperature is 45 ℃, the rotating speed is 500-700 rpm, and the time is 4-8 h.
8. The method for preparing the composite phase-change material according to claim 1, wherein the method comprises the following steps: and (3) drying at the temperature of 45 ℃ for 12-24 hours in the step (2).
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