CN111040737A - Shaped phase-change energy storage material and preparation method thereof - Google Patents
Shaped phase-change energy storage material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a qualitative phase change energy storage material and a preparation method thereof, wherein the shaped phase change energy storage material comprises a hydrous salt phase change material, a modified porous supporting material and a coating material, the coating material microscopically coats the hydrous salt phase change material and the modified porous supporting material, and the hydrous salt phase change material is adsorbed in the modified porous supporting material. According to the invention, hydrated salt is used as a phase change energy storage matrix material, and the preparation of the shaped phase change energy storage material is realized by dual means of porous adsorption and surface coating. The preparation method of the shaped phase-change energy storage material has the advantages of low cost, stable performance and simple and convenient operation, can completely prevent the phase-change material from micro-leakage, and can further expand the application field of the phase-change energy storage material.
Description
Technical Field
The invention relates to the technical field of phase-change materials, in particular to a shaped phase-change energy storage material and a preparation method thereof.
Background
Phase Change Materials (PCMs) are substances for storing, converting and utilizing heat by utilizing latent heat during phase change, and are widely applied to the fields of solar heat utilization, electric power peak regulation, waste heat utilization, building energy conservation, air conditioner energy conservation, aerospace and the like. Depending on the phase change mode, PCMs can be classified into solid-solid phase change materials, solid-liquid phase change materials, solid-gas phase change materials, and liquid-gas phase change materials. Among them, solid-gas phase change materials and liquid-gas phase change materials have very high latent heat of phase change, but gas is generated in the phase change process, so that the practical application is limited; the solid-liquid phase change material has larger phase change latent heat than the solid-solid phase change material, is the phase change energy storage material with the most practical value, but the material also has the defects of volume change, easy liquid leakage, low solid heat-conducting property and the like during system phase change.
The current solution can be divided into two aspects with respect to material leakage and stability: macro encapsulation and micro encapsulation (namely, shaping phase change energy storage materials). The macro packaging has certain limitation on the application of the phase change energy storage material; the shaped phase-change energy storage material has no flowability macroscopically in the phase-change process, can always keep a solid state without containing a container, so that the phase-change energy storage material is synergistically improved in phase-change performance, enhanced heat transfer, thermal stability and mechanical property, the service efficiency of the phase-change material is improved, and the application range of the phase-change energy storage material is widened.
The preparation method of the common shaped phase-change energy storage material mainly comprises the following steps of adsorbing by microcapsules and porous materials:
(1) microcapsule: the formation of particulate composite phase change materials by coating solid or liquid PCMs with a film-forming material is referred to as microencapsulated phase change materials (MCPMs). Among them, the coated film is called a capsule wall or wall material, and the coated solid or liquid is called a capsule core or core material. The coating of the wall material can effectively solve the problems of leakage, phase separation, corrosivity and the like of the PCMs, simultaneously increases the heat transfer area, prevents the reaction of the phase change material and the surrounding environment, controls the volume change during phase change, improves the service efficiency of the phase change material, can improve the application performance of the phase change material, expands the application field of the phase change material, and can provide a reliable way for compounding the solid-liquid phase change material and the high molecular structure material. Therefore, MCPCMs have become the most promising class of composite phase change heat storage materials.
(2) Adsorption of a porous material: the encapsulation reliability of the phase-change material in the porous medium is improved by means of the capillary effect, and the microscopic encapsulation of the phase-change material is realized. The porous medium is usually selected by considering its structural characteristics (pore size distribution, pore shape, pore-to-pore connectivity, etc.) and its compatibility with phase change energy storage materials. At present, natural porous materials, artificially synthesized porous materials, carbon carriers and the like can be selected.
However, according to the current research, the preparation and application of the microcapsule phase change material have the following problems that the coating rate of ① microcapsules is low, leakage exists to a certain extent, the preparation process of ② is complex, the cost is high, the application field of ③ is relatively exclusive, and the porous material absorbs the problem that the material leaks in the phase change process after multiple storage and heat release cycles because no chemical bond interaction exists between the phase change energy storage material and the porous material support.
Disclosure of Invention
In order to solve the problem that the shaped phase-change material in the prior art still has leakage to a certain extent, the invention provides a brand-new shaped phase-change energy storage material with a more stable structure and a preparation method thereof.
In order to achieve the purpose, the invention provides a shaped phase change energy storage material which comprises a hydrous salt phase change material, a modified porous support material and a coating material, wherein the coating material microcosmically coats the hydrous salt phase change material and the modified porous support material, and the hydrous salt phase change material is adsorbed in the modified porous support material.
Preferably, the hydrated salt phase change material is at least one of sodium acetate trihydrate, sodium thiosulfate pentahydrate, calcium chloride hexahydrate, magnesium nitrate hexahydrate, sodium sulfate decahydrate and sodium hydrogen phosphate dodecahydrate.
Preferably, the modified porous support material is obtained by pretreating a porous natural mineral material, an artificially synthesized porous material and a carbonaceous carrier.
Further preferably, the porous natural mineral material is at least one of diatomite, montmorillonite, kaolin, expanded perlite, halloysite and expanded vermiculite; the carbonaceous carrier is expanded graphite.
Preferably, the coating material is paraffin or polyvinylpyrrolidone.
The invention also provides a preparation method of the shaped phase-change energy storage material, which comprises the following steps:
pretreating the porous support material to obtain a modified porous support material;
adsorbing the hydrated salt phase change material into the modified porous support material to obtain a composite phase change energy storage material;
and (3) microcosmically coating the composite phase change energy storage material by adopting a coating material to obtain the shaped phase change energy storage material.
Preferably, the pre-treatment comprises: calcining and carrying out acid treatment, wherein the calcining temperature is 350-550 ℃, and the calcining time is 1-3 h.
Further preferably, the acid treatment is carried out by using hydrochloric acid or sulfuric acid, the concentration of the acid is 60-80%, and the acid treatment time is 2-6 h.
Preferably, the adsorption mode is vacuum adsorption, and the vacuum degree is 0.04-0.07 MPa.
Preferably, the temperature of the vacuum adsorption is 40-60 ℃, and the adsorption time is 20-100 min.
According to the invention, hydrated salt is used as a phase change energy storage matrix material, and the preparation of the shaped phase change energy storage material is realized by dual means of porous adsorption and surface coating. The method has the advantages of low cost, stable performance and simple and convenient operation, can completely prevent the phase-change material from micro-leakage, and can further expand the application field of the phase-change energy storage material.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. This invention may, however, be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and its practical application to thereby enable others skilled in the art to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated.
The inventor of the invention provides a brand-new shaped phase-change energy storage material with excellent thermal stability and a preparation method thereof based on the problem that the shaped phase-change material in the prior art still has leakage to a certain extent.
The embodiment of the invention provides a preparation method of a shaped phase change energy storage material, which comprises the following steps:
and step A, pretreating the porous support material to obtain the modified porous support material.
The specific surface area of the internal micropores of the porous supporting material is large, the adsorption effect is strong, and the porous supporting material is an ideal sizing material. The porous support material can be selected from porous natural mineral materials, artificially synthesized porous materials or carbon carriers. Further preferably at least one of diatomaceous earth, montmorillonite, kaolin, expanded perlite, halloysite, expanded vermiculite and expanded graphite.
The pretreatment comprises the following steps: calcination and acid treatment, the porous material being subjected to calcination and acid treatment in order to: the natural minerals contain impurities such as clay minerals and organic matters, and are modified before use in order to improve the porosity, facilitate the adsorption of the phase-change material and further improve the utilization value of the phase-change material.
Preferably, the calcining temperature is 350-550 ℃ and the time is 1-3 h.
Preferably, hydrochloric acid or sulfuric acid is used for acid treatment, the concentration of the acid is 60% -80%, and the acid treatment time is 2-6 h.
B. And adsorbing the hydrated salt phase change material into the modified porous support material to obtain the composite phase change energy storage material.
The choice of hydrated salt phase change material is not limited and only a few commonly used are listed here: sodium acetate trihydrate, sodium thiosulfate pentahydrate, calcium chloride hexahydrate, magnesium nitrate hexahydrate, sodium sulfate decahydrate, and sodium hydrogen phosphate dodecahydrate.
The preferred adsorption mode is vacuum adsorption, the preferred vacuum degree is 0.04-0.07 MPa, the adsorption temperature is 40-60 ℃, and the adsorption time is 20-100 min. The adsorption temperature is ensured to be above the phase transition temperature of the hydrous salt phase change material, so that the hydrous salt phase change material can be ensured to be in a liquid state, and in addition, the problem that if the adsorption temperature is too high, the crystal water in the hydrous salt phase change material can be dehydrated is also considered.
The specific operation is as follows: placing the modified porous support material in a closed conical flask, vacuumizing, and adding the hydrated salt phase-change material into the conical flask through a separating funnel for vacuum adsorption; and after adsorption, carrying out suction filtration, and grinding and dispersing the solid subjected to suction filtration at a low temperature (at the temperature of 5-15 ℃) to obtain the composite phase change energy storage material.
C. And (3) coating the composite phase change energy storage material by a coating material to obtain the shaped phase change energy storage material.
Compared with macroscopic encapsulation and encapsulation, the microscopic encapsulation is more beneficial to the application of the shaped phase change energy storage material, the composite phase change energy storage material encapsulated by the microscopic encapsulation can be better mixed with a base material such as a cement base material, the dispersity is better, and the strength of the base material is not easy to weaken. The coating material is selected from materials capable of coating a film, and the preferred material is paraffin or polyvinylpyrrolidone (PVP).
The specific operation is as follows: fully dissolving high-temperature paraffin in a solvent such as normal hexane to form a paraffin normal hexane solution, wherein the melting point of the paraffin is more than 60 ℃, and the mass fraction of the paraffin is 3-5%; adding the composite phase change energy storage material in the step B into a paraffin n-hexane solution, and stirring for 4-6 hours at room temperature; and carrying out suction filtration and low-temperature drying for 1-2 h to obtain the qualitative phase change energy storage material.
The invention also provides a shaped phase change energy storage material which comprises a hydrous salt phase change material, a modified porous supporting material and a coating material, wherein the coating material microscopically coats the hydrous salt phase change material and the modified porous supporting material, and the hydrous salt phase change material is adsorbed in the modified porous supporting material.
For the purposes of the present invention, the selection of the hydrous salt phase-change material influences physical parameters of the shaped phase-change energy storage material, such as phase-change latent heat, phase-change temperature and the like, but the parameters are the characteristics of the hydrous salt phase-change material. The selection of the hydrated salt phase change material has no substantial effect on the effectiveness of the micro encapsulation, and therefore, the selection of the hydrated salt phase change material is not limited in the present invention. Only a few of the commonly used are listed here: sodium acetate trihydrate, sodium thiosulfate pentahydrate, calcium chloride hexahydrate, magnesium nitrate hexahydrate, sodium sulfate decahydrate, and sodium hydrogen phosphate dodecahydrate.
The modified porous supporting material is obtained by pretreating the porous supporting material. The pretreatment operation comprises calcination and acid treatment, and the obtained modified porous support material has higher porosity. The specific surface area of the internal micropores of the porous supporting material is large, the adsorption effect is strong, and the porous supporting material is an ideal sizing material. The porous support material can be selected from porous natural mineral materials, artificially synthesized porous materials or carbon carriers. Further preferably at least one of diatomaceous earth, montmorillonite, kaolin, expanded perlite, halloysite, expanded vermiculite and expanded graphite.
The coating material is selected from materials capable of coating a film, and the preferred material is paraffin or PVP.
The phase change temperature of the shaped phase change energy storage material is 20-35 ℃, and the latent heat of phase change is 90-120 kJ/kg: the phase change latent heat of the shaped phase change energy storage material obtained in the embodiment is higher than 100kJ/kg, and the shaped phase change energy storage material has good thermal stability: the initial weight loss temperature is 50-60 ℃.
The invention adopts the dual means of porous adsorption and surface coating to encapsulate the phase-change material, can completely prevent the phase-change material from micro-leakage in the solid-liquid conversion process, and the obtained novel shaped phase-change energy storage material has better thermal stability and cycling stability.
The above-mentioned shaped phase-change energy storage material and the preparation method thereof according to the present invention will be described with reference to specific examples, and it will be understood by those skilled in the art that the following examples are only specific examples of the above-mentioned shaped phase-change energy storage material and the preparation method thereof according to the present invention, and are not intended to limit the entirety thereof.
Example 1
1. Calcining diatomite and modifying by sulfuric acid treatment, wherein the calcining temperature is 350 ℃, and the calcining time is 3 hours; the acid treatment concentration is 80%, and the acid soaking treatment time is 6 h.
2. Placing the modified diatomite in a closed coneVacuumizing in a bottle, adding liquid CaCl2·6H2And adding the O into the conical flask through a separating funnel for vacuum adsorption. Wherein the adsorption temperature is 40 ℃ and the adsorption time is 100 min. And after adsorption, carrying out suction filtration, and grinding and dispersing the solid subjected to suction filtration at a low temperature of 5 ℃ to obtain the porous adsorbed phase change energy storage material.
3. And (3) fully dissolving high-temperature paraffin in the normal hexane, wherein the mass fraction of the paraffin is 5%.
4. And adding the phase change energy storage material subjected to porous adsorption into a solution of n-hexane, stirring for 4 hours at room temperature, and then carrying out suction filtration treatment. Drying the obtained solid at low temperature for 1h to obtain the shaped phase change energy storage material.
The shaped phase change energy storage material obtained in example 1 was tested by Differential Scanning Calorimetry (DSC), and the test results showed that the latent heat of phase change of the material was 103.6kJ/kg, the phase change temperature was 29.3 ℃, and the initial weight loss temperature of the shaped phase change energy storage material was 57.2 ℃.
Example 2
1. Calcining diatomite and modifying by sulfuric acid treatment, wherein the calcining temperature is 550 ℃, and the calcining time is 1 h; the acid treatment concentration is 60 percent, and the acid soaking treatment time is 2 hours.
2. Placing the modified diatomite in a closed conical flask, vacuumizing, and adding liquid CaCl2·6H2And adding the O into the conical flask through a separating funnel for vacuum adsorption. Wherein the adsorption temperature is 60 ℃ and the adsorption time is 20 min. And after adsorption, carrying out suction filtration, and grinding and dispersing the solid subjected to suction filtration at low temperature of 15 ℃ to obtain the porous adsorbed phase change energy storage material.
3. The high-temperature paraffin was sufficiently dissolved in n-hexane at a concentration of 30 g/mL.
4. And adding the phase change energy storage material subjected to porous adsorption into a solution of n-hexane, stirring for 6 hours at room temperature, and then carrying out suction filtration treatment. Drying the obtained solid at low temperature for 2h to obtain the shaped phase change energy storage material.
DSC (differential scanning calorimetry) test is carried out on the shaped phase change energy storage material obtained in example 2, and the test result shows that the phase change latent heat of the material is 106.1kJ/kg, and the phase change temperature is 29.5 ℃. The initial weight loss temperature of the sizing phase change energy storage material is 57.8 ℃.
Example 3
1. Calcining diatomite and modifying by sulfuric acid treatment, wherein the calcining temperature is 450 ℃, and the calcining time is 3 hours; the acid treatment concentration is 60 percent, and the acid soaking treatment time is 4 hours.
2. Placing the modified diatomite in a closed conical flask, vacuumizing, and adding liquid CaCl2·6H2And adding the O into the conical flask through a separating funnel for vacuum adsorption. Wherein the adsorption temperature is 40 ℃ and the adsorption time is 60 min. And after adsorption, carrying out suction filtration, and grinding and dispersing the solid subjected to suction filtration at low temperature of 15 ℃ to obtain the porous adsorbed phase change energy storage material.
3. The high-temperature paraffin was sufficiently dissolved in n-hexane at a concentration of 30 g/mL.
4. And (3) adding the material obtained in the step (2) into a normal hexane solution, stirring for 6 hours at room temperature, and then carrying out suction filtration treatment. Drying the obtained solid at low temperature for 1h to obtain the shaped phase change energy storage material.
DSC (differential scanning calorimetry) test is carried out on the shaped phase change energy storage material obtained in the embodiment 3, and the test result shows that the phase change latent heat of the material is 108.2kJ/kg, the phase change temperature is 28.9 ℃, and the initial weight loss temperature of the shaped phase change energy storage material is 58.6 ℃.
Comparative example 1
1. Calcining diatomite and modifying by sulfuric acid treatment, wherein the calcining temperature is 350 ℃, and the calcining time is 3 hours; the acid treatment concentration is 80%, and the acid soaking treatment time is 6 h.
2. Placing the modified diatomite in a closed conical flask, vacuumizing, and adding liquid CaCl2·6H2And adding the O into the conical flask through a separating funnel for vacuum adsorption. Wherein the adsorption temperature is 40 ℃ and the adsorption time is 100 min. And after adsorption, carrying out suction filtration, and grinding and dispersing the solid subjected to suction filtration at a low temperature of 5 ℃ to obtain the porous adsorbed phase change energy storage material.
DSC (differential scanning calorimetry) test is carried out on the phase change energy storage material obtained in the comparative example 1, and the test result shows that the phase change latent heat of the material is 114.6kJ/kg, the phase change temperature is 28.7 ℃, and the initial weight loss temperature of the sizing phase change energy storage material is 52.1 ℃.
The comparative example 1 is compared with the example 1, the difference is whether surface coating is adopted, and the data result shows that the phase change latent heat of the shaped phase change energy storage material subjected to surface coating by adopting paraffin is reduced by 11kJ/kg, the phase change temperature change is less than 1 ℃, and the initial weight loss temperature is increased by 5.1 ℃.
Comparative example 2
1. Calcining diatomite and modifying by sulfuric acid treatment, wherein the calcining temperature is 550 ℃, and the calcining time is 1 h; the acid treatment concentration is 60 percent, and the acid soaking treatment time is 2 hours.
2. Placing the modified diatomite in a closed conical flask, vacuumizing, and adding liquid CaCl2·6H2And adding the O into the conical flask through a separating funnel for vacuum adsorption. Wherein the adsorption temperature is 60 ℃ and the adsorption time is 20 min. And after adsorption, carrying out suction filtration, and grinding and dispersing the solid subjected to suction filtration at low temperature of 15 ℃ to obtain the porous adsorbed phase change energy storage material.
DSC (differential scanning calorimetry) test is carried out on the phase change energy storage material obtained in the comparative example 2, and the test result shows that the phase change latent heat of the material is 115.2kJ/kg, the phase change temperature is 29.7 ℃, and the initial weight loss temperature of the sizing phase change energy storage material is 51.8 ℃.
The comparative example 2 is compared with the example 2, the difference is whether surface coating is adopted, and the data result shows that the phase change latent heat of the shaped phase change energy storage material subjected to surface coating by adopting paraffin is reduced by 9.1kJ/kg, the phase change temperature change is less than 0.5 ℃, and the initial weight loss temperature is increased by 6.0 ℃.
Comparative example 3
1. Calcining diatomite and modifying by sulfuric acid treatment, wherein the calcining temperature is 450 ℃, and the calcining time is 3 hours; the acid treatment concentration is 60 percent, and the acid soaking treatment time is 4 hours.
2. Placing the modified diatomite in a closed conical flask, vacuumizing, and adding liquid CaCl2·6H2And adding the O into the conical flask through a separating funnel for vacuum adsorption. Wherein the adsorption temperature is 40 ℃ and the adsorption time is 60 min. Carrying out suction filtration after the adsorption is finished, and carrying out low temperature treatment on the solid after the suction filtrationGrinding and dispersing at 15 ℃ to obtain the porous adsorbed phase change energy storage material.
DSC (differential scanning calorimetry) test is carried out on the phase change energy storage material obtained in the comparative example 3, and the test result shows that the phase change latent heat of the material is 117.1kJ/kg, the phase change temperature is 28.7 ℃, and the initial weight loss temperature of the sizing phase change energy storage material is 52.9 ℃.
The comparison example 3 and the example 3 form a single variable comparison, the difference is whether surface coating is adopted, and the data result shows that the phase change latent heat of the sizing phase change energy storage material subjected to surface coating by adopting paraffin is reduced by 8.9kJ/kg, the phase change temperature change is less than 0.5 ℃, and the initial weight loss temperature is increased by 5.7 ℃.
While the invention has been shown and described with reference to certain embodiments, those skilled in the art will understand that: various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (10)
1. The shaping phase-change energy storage material is characterized by comprising a hydrated salt phase-change material, a modified porous supporting material and a coating material, wherein the coating material microcosmically coats the hydrated salt phase-change material and the modified porous supporting material, and the hydrated salt phase-change material is adsorbed in the modified porous supporting material.
2. The shaped phase change energy storage material of claim 1, wherein the hydrated salt phase change material is at least one of sodium acetate trihydrate, sodium thiosulfate pentahydrate, calcium chloride hexahydrate, magnesium nitrate hexahydrate, sodium sulfate decahydrate, and sodium hydrogen phosphate dodecahydrate.
3. The shaped phase-change energy storage material as claimed in claim 1, wherein the modified porous support material is obtained by pretreating a porous natural mineral material, an artificially synthesized porous material or a carbonaceous carrier; the coating material is a material capable of forming a film.
4. The shaped phase change energy storage material of claim 3, wherein the porous natural mineral material is at least one of diatomaceous earth, montmorillonite, kaolin, expanded perlite, halloysite, and expanded vermiculite; the carbonaceous carrier is expanded graphite.
5. The shaped phase change energy storage material as claimed in claim 3, wherein the coating material is paraffin or polyvinylpyrrolidone.
6. A method for preparing the shaped phase change energy storage material as claimed in any one of claims 1 to 5, comprising:
pretreating the porous support material to obtain a modified porous support material;
adsorbing the hydrated salt phase change material into the modified porous support material to obtain a composite phase change energy storage material;
and (3) microcosmically coating the composite phase change energy storage material by adopting a coating material to obtain the shaped phase change energy storage material.
7. The method of manufacturing according to claim 6, wherein the pre-treatment comprises: calcining and acid treatment, wherein the calcining temperature is 350-550 ℃, and the time is 1-3 h.
8. The method according to claim 7, wherein the acid treatment is carried out using hydrochloric acid or sulfuric acid, the acid concentration is 60% to 80%, and the acid treatment time is 2 to 6 hours.
9. The method according to any one of claims 6 to 8, wherein the adsorption is performed by vacuum adsorption at a vacuum degree of 0.04 to 0.07 MPa.
10. The method according to claim 9, wherein the temperature of the vacuum adsorption is 40 to 60 ℃ and the adsorption time is 20 to 100 min.
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Application publication date: 20200421 |