CN115058058A - Preparation method of novel liquid metal-based photothermal phase change energy storage aerogel - Google Patents
Preparation method of novel liquid metal-based photothermal phase change energy storage aerogel Download PDFInfo
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 14
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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Abstract
The invention discloses a preparation method of a novel liquid metal-based photothermal phase change energy storage aerogel in the technical field of composite material preparation, aiming at solving the defects of low photothermal conversion performance, low thermal conductivity, easy leakage and the like of the traditional phase change energy storage material, and comprising the following steps of firstly preparing liquid metal-based photothermal phase change particles; carrying out alkylation modification on the cellulose gel to obtain alkylated cellulose aerogel; and melting the liquid metal-based photothermal phase change particles, and loading the melted liquid metal-based photothermal phase change particles into the alkylated cellulose aerogel through vacuum impregnation to obtain the liquid metal-based photothermal phase change energy storage aerogel. The liquid metal-based photothermal phase change energy storage aerogel prepared by the invention has the advantages of high-efficiency photothermal conversion, leakage prevention, enhanced heat conduction and high energy storage enthalpy value, so that the liquid metal-based photothermal phase change energy storage aerogel is widely applied to the field of photothermal phase change energy storage materials.
Description
Technical Field
The invention relates to a preparation method of a novel liquid metal-based photothermal phase change energy storage aerogel, and belongs to the technical field of composite material preparation.
Background
Along with the development of social economy, the human demand for energy is more and more, and due to the shortage of global energy, sustainable renewable environment-friendly energy is favored by people. Solar energy plays an important role in the field of energy as a sustainable renewable energy source. Therefore, the efficient utilization of solar energy resources has great significance for relieving global resource shortage. Among them, the photothermal conversion, i.e., the conversion of light energy into heat energy, is the most direct and the simplest way to use solar energy efficiently. Therefore, excellent photothermal conversion materials can efficiently use solar energy resources, such as conventional photothermal conversion materials such as: semiconductors, conjugated polymers, noble metal particles, and carbon materials, and the like.
Due to the characteristics of the solar east rising west drop, the solar energy resource has the problems of energy conversion, time and space mismatching, and the utilization rate of the solar energy is greatly reduced. Therefore, the development of the solar energy storage material is an effective way for improving the utilization efficiency of solar energy. The organic solid-liquid phase change energy storage material is a substance which changes the state of the material when the temperature of the material changes and provides latent heat, so that the material can be used as a solar energy storage material, but the traditional phase change energy storage material has the defects of low photo-thermal conversion performance, low thermal conductivity, easy leakage and the like.
Liquid metal is a novel metal material, the low melting point of the metal material enables phase change (namely, transformation from a solid state to a liquid state) to occur at a lower temperature, but the low light absorption performance and the energy storage enthalpy limit the application of the metal material in the field of photo-thermal phase change. Therefore, the light absorption capacity and the phase change energy storage performance of the liquid metal are improved, and the method has high scientific research significance and practical value for widening the application field of the liquid metal and improving the solar energy utilization rate.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a preparation method of a novel liquid metal-based photothermal phase change energy storage aerogel, which overcomes the defects of low photothermal conversion performance, low thermal conductivity, easy leakage and the like of the traditional phase change energy storage material, so that the novel liquid metal-based photothermal phase change energy storage aerogel is widely applied to the field of photothermal phase change energy storage materials.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
according to the first aspect of the invention, the preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel comprises the following steps,
s1, mixing liquid metal and stearic acid according to a certain proportion, carrying out first high-energy ball milling, mixing ball milling products with molybdenum disulfide, and carrying out second high-energy ball milling to obtain liquid metal-based photothermal phase change particles;
s2, freeze-drying the cellulose solution to obtain cellulose gel, and placing the cellulose gel in a mixed solution of petroleum ether, stearoyl chloride and triethylamine for alkylation modification to obtain alkylated cellulose aerogel;
s3, after the liquid metal-based photothermal phase change particles are melted, the liquid metal-based photothermal phase change particles are loaded into the alkylated cellulose aerogel through vacuum impregnation, and the liquid metal-based photothermal phase change energy storage aerogel is obtained.
Further, the mass ratio of the liquid metal to stearic acid is 1: 4-1: 19.
further, the time of the first high-energy ball milling is 10 hours, and the time of the second high-energy ball milling is 2 hours.
Further, the mass of the molybdenum disulfide is 5% of that of the first high-energy ball-milling product.
Further, the concentration of the cellulose solution was 2wt%, and the freezing time thereof was 48 hours.
Further, the mass ratio of the petroleum ether to the stearoyl chloride to the triethylamine is 26:2.4: 1.
Further, the alkylation modification in step S2 is carried out at a reaction temperature of 60 ℃ for a reaction time of 24 hours.
Further, in step S3, the melting temperature is 90 ℃ and the vacuum impregnation time is 2 h.
According to the second aspect of the invention, a novel liquid metal-based photothermal phase change energy storage aerogel is also provided, and is prepared by the preparation method of any one of the above.
According to a third aspect of the invention, the application of the novel liquid metal-based photothermal phase change energy storage aerogel in photothermal phase change energy storage is also provided.
Compared with the prior art, the invention has the following beneficial effects:
the liquid metal-based photothermal phase change energy storage particles prepared firstly have excellent photothermal conversion performance and higher phase change energy storage enthalpy value, and are greatly improved compared with the original liquid metal; and then the liquid metal-based photothermal phase change energy storage aerogel is prepared by combining the liquid metal-based photothermal phase change energy storage aerogel with the alkylated cellulose aerogel, so that the defects of low photothermal conversion efficiency, easy leakage and poor thermal conductivity of the traditional phase change energy storage material are overcome, and the application of liquid metal in the field of photothermal phase change is widened.
Drawings
FIG. 1 shows the product a of the example of the present invention 1 、a 2 And a 3 Schematic view of a DSC image of (a);
FIG. 2 shows the product a of the example of the present invention 1 、a 2 And a 3 A schematic diagram of an absorbance image of (a);
FIG. 3 shows product A in an example of the present invention 1 And A 2 A light reflectance in the spectral range of 250-2500 nm;
FIG. 4 shows product A in an example of the present invention 1 And A 2 At 1 Kw/m 2 Schematic diagram of temperature change under light source irradiation;
FIG. 5 shows product A in an example of the present invention 1 And A 2 A schematic of thermal conductivity of (a);
FIG. 6 shows product A in an example of the present invention 2 A schematic view of a DSC image of (a);
FIG. 7 shows product A in an example of the present invention 2 The leakage-proof performance test of (2) is shown schematically.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
For the purposes of the present specification and appended claims, unless otherwise indicated, all numbers expressing quantities, percentages or proportions, and other numerical values used in the specification and appended claims, are to be understood as being modified in all instances by the term "about". Moreover, all ranges disclosed herein are inclusive of the endpoints and independently combinable.
Example 1:
respectively mixing liquid metal and stearic acid in a mass ratio of 1: 4, placing the mixture in a ball milling tank, and carrying out high-energy mechanical ball milling for 10 hours to obtain a product a 1 。
Example 2:
respectively mixing liquid metal and stearic acid in a mass ratio of 1: 19, placing the mixture into a ball milling tank, and carrying out high-energy mechanical ball milling for 10 hours to obtain a product a 2 Adding molybdenum disulfide into the solution A 2 Ball-milling in a ball-milling tank for 2 hours to obtain liquid metal-based photothermal phase change particles a 3 Wherein the molybdenum disulfide is a 2 5% by mass.
Example 3:
s1, mixing the liquid metal and stearic acid in a mass ratio of 1: 19, placing the mixture into a ball milling tank, and carrying out high-energy mechanical ball milling for 10 hours to obtain a product a 2 。
S2, placing a 2wt% cellulose solution into a cylindrical/square container, carrying out freeze drying for 48h to obtain cellulose aerogel, then placing the cellulose aerogel into a mixed solution of petroleum ether, stearoyl chloride and triethylamine (the mass ratio of the petroleum ether, the stearoyl chloride and the triethylamine is 26:2.4: 1), and carrying out alkylation modification at 60 ℃ for 24h to obtain alkylated cellulose aerogel;
s3, mixing a 2 Is placed in a container and put intoMelting in an oven, and impregnating a by vacuum 2 Loading into alkylated cellulose aerogel to obtain aerogel product A 1 。
Example 4:
s1, mixing the liquid metal and stearic acid in a mass ratio of 1: 19, placing the mixture into a ball milling tank, and carrying out high-energy mechanical ball milling for 10 hours to obtain a product a 2 . Adding molybdenum disulfide into the solution A 2 Ball milling pot (molybdenum disulfide is a) 2 5 percent of the mass) is subjected to ball milling for 2 hours to obtain liquid metal-based photothermal phase change particles a 3 。
S2, placing a 2wt% cellulose solution into a cylindrical/square container, carrying out freeze drying for 48 hours to obtain cellulose aerogel, placing the cellulose aerogel into a mixed solution of petroleum ether, stearoyl chloride and triethylamine (the mass ratio is 26:2.4: 1), and carrying out alkylation modification at 60 ℃ for 24 hours to obtain alkylated cellulose aerogel;
s3, mixing a 2 Placing in a container, putting in an oven for melting, and performing vacuum impregnation on the mixture 3 Loading into alkylated cellulose aerogel to obtain aerogel product A 2 。
The properties of the products obtained in the examples of the present invention will be analyzed with reference to the drawings.
First, the product a obtained in example 1-2 was subjected to 1 、a 2 And a 3 The performance is analyzed, and the product a can be obtained by calculation according to the DSC image schematic diagram of three products shown in figure 1 and figure 1 1 、a 2 And a 3 Respectively 165.5J/g, 205.5J/g and 190.6J/g, and respectively 169.9J/g, 211.5J/g and 195.8J/g. From the results, it can be seen that by adjusting the ratio of liquid metal and stearic acid, a 2 The melting enthalpy and the cold crystallization enthalpy are both higher than a 1 It is demonstrated that as the stearic acid content increases, the melting enthalpy and the cold crystallization enthalpy of the product increase accordingly.
And, the product a 3 Enthalpy of stored energy compared to a 2 This is mainly due to the fact that molybdenum disulfide does not have phase change energy storage properties. With reference to FIG. 2, FIG. 2 is a schematic diagram of absorbance images of three productsIt can be seen from FIG. 2 that after addition of molybdenum disulphide, a 3 Exhibits a ratio of 2 The excellent light absorption properties are required mainly because molybdenum disulfide is a semiconductor having excellent light absorption properties and a wide light absorption range, and exhibits a flower-like microstructure that causes multiple reflections of light to enhance light absorption thereof.
Next, the product A obtained in example 3-4 was subjected to 1 And A 2 The performance was analyzed. FIG. 3 shows product A 1 And A 2 Light reflectance in the spectral range of 250-2500nm, from which A can be derived 1 ，A 2 The lower light reflectance was shown, again due primarily to the broad light absorption range of molybdenum disulfide and multiple reflections of light. Then, in conjunction with FIG. 4, at 1 Kw/m 2 Under the irradiation of a light source, A 1 And A 2 All have different degree of rise of surface temperature, wherein A 1 And A 2 The surface temperatures of (a) can reach 52.2 ℃ and 54.6 ℃, respectively, which is consistent with the results described in fig. 3.
FIG. 5 shows product A 1 And A 2 The thermal conductivity of (2) to obtain A 1 And A 2 Respectively 0.2861W/m and 0.3095W/m, it is evident that the introduction of molybdenum disulphide can improve the heat transfer performance of the phase change energy storage material, wherein a 2 Ratio A 1 The higher thermal conductivity is probably that the molybdenum disulfide has good wetting property, and can reduce A 2 Internal thermal resistance.
FIG. 6 shows product A 2 The melting enthalpy and the cold crystallization enthalpy are 187.5J/g and 192.6J/g respectively, and the DSC image has a higher phase change energy storage enthalpy value. FIG. 7 is A 2 The leakage-proof test of (1) is schematically illustrated, wherein block-shaped pure stearic acid is used as a comparison, pure stearic acid is placed on a heating table at 90 ℃ for heating, and it can be seen from FIG. 7 that a sample of pure stearic acid melts into a colorless liquid within 4 minutes, and the shape stability and leakage-proof performance are poor, in contrast to A 2 The sample showed excellent shape stability and leakage-proof property, and no significant leakage occurred even after heating for 80 minutes. This is mainly due to the surface of the alkylated cellulose aerogelsThe tension and the capillary force promote a 3 Good dispersion in 3D aerogel porous framework, make A 2 And the phase transition process shows good shape stability and leakage-proof performance.
The novel liquid metal-based photothermal phase change particles are prepared by a simple mechanical ball milling method, and the cellulose aerogel is introduced as a matrix to prepare the liquid metal-based photothermal phase change energy storage aerogel with high-efficiency photothermal conversion, leakage prevention, enhanced heat conduction and high energy storage enthalpy value.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a novel liquid metal-based photothermal phase change energy storage aerogel is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
s1, mixing liquid metal and stearic acid according to a certain proportion, carrying out first high-energy ball milling, mixing ball milling products with molybdenum disulfide, and carrying out second high-energy ball milling to obtain liquid metal-based photothermal phase change particles;
s2, freeze-drying the cellulose solution to obtain cellulose gel, and placing the cellulose gel into a mixed solution of petroleum ether, stearoyl chloride and triethylamine for alkylation modification to obtain alkylated cellulose aerogel;
s3, after the liquid metal-based photothermal phase change particles are melted, the liquid metal-based photothermal phase change particles are loaded into the alkylated cellulose aerogel through vacuum impregnation, and the liquid metal-based photothermal phase change energy storage aerogel is obtained.
2. The preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein: the mass ratio of the liquid metal to the stearic acid is 1: 4-1: 19.
3. the preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein: the time of the first high-energy ball milling is 10 hours, and the time of the second high-energy ball milling is 2 hours.
4. The preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein: the mass of the molybdenum disulfide is 5% of that of the first high-energy ball-milling product.
5. The preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein the preparation method comprises the following steps: the concentration of the cellulose solution was 2wt%, and the freezing time was 48 h.
6. The preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein: the mass ratio of the petroleum ether to the stearoyl chloride to the triethylamine is 26:2.4: 1.
7. The preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein: the reaction temperature for alkylation modification in step S2 was 60 ℃ and the reaction time was 24 hours.
8. The preparation method of the novel liquid metal-based photothermal phase change energy storage aerogel according to claim 1, wherein the preparation method comprises the following steps: in step S3, the melting temperature is 90 ℃, and the vacuum impregnation time is 2 h.
9. The utility model provides a novel liquid metal base light and heat phase transition energy storage aerogel which characterized in that: is produced by the production method according to any one of claims 1 to 8.
10. The novel liquid metal-based photothermal phase change energy storage aerogel according to claim 9, for use in photothermal phase change energy storage.
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