CN110527495B - Preparation method of composite phase-change material - Google Patents

Preparation method of composite phase-change material Download PDF

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CN110527495B
CN110527495B CN201910600499.2A CN201910600499A CN110527495B CN 110527495 B CN110527495 B CN 110527495B CN 201910600499 A CN201910600499 A CN 201910600499A CN 110527495 B CN110527495 B CN 110527495B
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高军凯
唐茜
陈妍
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Zhejiang Ocean University ZJOU
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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

Preparation method of composite phase-change material
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
Figure BDA0002119070910000061
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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