CN114774084A - Photo-thermal shaping phase-change energy storage composite material and preparation method thereof - Google Patents
Photo-thermal shaping phase-change energy storage composite material and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention discloses a photo-thermal setting phase-change energy storage composite material and a preparation method thereof, wherein the photo-thermal setting phase-change energy storage composite material is prepared from 65-80 wt% of organic phase-change energy storage material and 20-35 wt% of frame structure material with photo-thermal and heat conduction functions, wherein the frame structure material realizes the setting and firming of a frame and the construction of a heat conduction path by virtue of coordination among metal ions, a two-dimensional sheet material and a high polymer material, electrostatic interaction and a hydrogen bond synergistic bridging effect among molecules. Decomposing ammonium bicarbonate to obtain the frame structure material; and immersing the frame structure material into the fused organic phase-change energy storage material for vacuum impregnation to prepare the photo-thermal setting phase-change energy storage composite material with excellent shape stability and stable and rapid heat transfer property. The preparation method is simple and efficient, energy-saving and environment-friendly, and has great significance for large-scale preparation of the composite material with the frame structure and practical application of the composite material in the field of solar photo-thermal conversion.
Description
Technical Field
The invention belongs to the field of new solar photo-thermal utilization materials, and particularly relates to a photo-thermal shaping phase-change energy storage composite material and a preparation method thereof.
Background
Solar energy has become an important component of energy with decreasing traditional energy and increasing environmental pollution. However, the solar energy is limited by the intermittency, low stability and low efficiency of solar irradiation, and the large-scale utilization of the solar energy is influenced. At present, the conversion of solar energy into thermal energy stored in a Phase Change Material (PCM) by using the heat absorption characteristic of the phase change material in the solid-liquid phase change process is a simple and convenient way to effectively utilize solar energy.
Among the numerous phase change materials, organic phase change materials (such as polyethylene glycol) have the advantages of large phase change enthalpy, proper phase change temperature, no toxicity, low cost, degradability, biocompatibility and the like, and thus have received extensive attention and research. However, the problem of leakage during the solid-liquid phase change becomes a major factor hindering its practical application; in addition, the practical application of the organic phase change energy storage material is greatly limited due to the problems of low thermal conductivity (about 0.2W/m.K) and lack of energy conversion capability of the organic phase change material (such as polyethylene glycol).
MXene(Mn+1XnTxT is a functional group, -O, -F, -OH), has a near 100% photothermal conversion efficiency, a wide absorption spectrum, a high thermal conductivity, and a simple and mass production method, and thus is one of the hot point materials for solar photothermal applications. After the electrons on the MXene surface capture photons from solar radiation, the photons are subjected to vibration frequencyThe rate is consistent with the vibration frequency of the absorbed photons to generate a plasmon resonance Effect (LSPR Effect), and then the absorbed solar radiation is converted into thermal energy by lattice scattering, thus having excellent photothermal conversion characteristics. At present, the photothermal property of MXene and the energy storage of an organic phase-change material are combined by technologies such as physical blending, microcapsule coating, porous material adsorption and the like to obtain a composite material with photothermal conversion and phase-change energy storage functions. Chinese patent CN109852349A discloses a light-heat energy conversion and heat energy storage shape-stabilized phase-change composite material and a preparation method thereof, wherein an organic phase-change material is added into MXene nanosheet dispersion liquid, and the light-heat energy conversion and heat energy storage shape-stabilized phase-change composite material is obtained by drying after ultrasonic mixing. Although the preparation technology is simple and rapid, the problem of poor heat conductivity of the phase-change material is still not solved. Chinese patent CN112588214A discloses a phase-change material microcapsule with photo-thermal conversion and energy storage properties and a preparation method thereof, and the phase-change material microcapsule is prepared in a system in which amphiphilic macromolecule 1, 1-diphenylethylene end-capped polyglycidyl methacrylate and MXene coexist synergistically and stably by a one-pot method. The microcapsule has a capsule core made of phase change material, an inner capsule wall made of polydivinylbenzene high polymer, and an outer capsule wall made of MXene. Although the multi-wall microcapsule has high encapsulation efficiency and higher thermal energy storage density and photothermal conversion efficiency, the preparation process is complex and high in cost, and large-scale production is difficult.
At present, in order to solve the problem of poor heat conductivity, researchers have also adopted a method for constructing a porous frame to prepare a phase-change composite material. Chinese patent CN110684510A discloses a heat-conduction-enhanced heat-energy-storage shaping phase-change composite material and a preparation method thereof, wherein MXene aerogel with a porous structure is constructed by an ice template method, and then the phase-change material is impregnated in vacuum to obtain the shaping phase-change composite material with a high enthalpy value. The phase-change composite material prepared by utilizing the aerogel frame has high enthalpy value and good photo-thermal effect, but the prepared frame structure material cannot form effective connection due to lack of strong interaction, so that the material is fragile under the action of external force, and the shape stability and the heat conductivity of the phase-change material cannot meet the practical application scene.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the objectives of the present invention is to provide a photo-thermal shape-stabilized phase-change energy-storage composite material, which integrates photo-thermal conversion (converting solar energy into thermal energy) and energy storage (storing through solid-liquid phase-change conversion), and has the advantages of good shape stability, low probability of breakage, stable heat transfer performance, and high heat transfer speed.
The second purpose of the invention is to provide a preparation method of the photo-thermal setting phase-change energy storage composite material, the preparation method is simple, efficient, energy-saving and environment-friendly, and the prepared photo-thermal setting phase-change energy storage composite material is stable in shape and good in heat transfer performance.
One of the purposes of the invention can be achieved by adopting the following technical scheme:
the photo-thermal setting phase change energy storage composite material is prepared from the following components in percentage by weight:
65% -80% of organic phase change energy storage material;
20% -35% of a frame structure material with photo-thermal and heat-conducting functions;
the organic phase change energy storage material is one or a composition of more than two of fatty acid, fatty acid ester or alcohol compounds;
the frame structure material with the photo-thermal and heat-conducting functions is made of metal ions, a macromolecular compound and a two-dimensional sheet material.
Further, the metal ions are one or a composition of more than two of chloride or nitrate of calcium ions, iron ions, cobalt ions, nickel ions, copper ions and zinc ions;
further, the high molecular compound is one or a composition of more than two of polyurethane, polyvinylpyrrolidone, starch, sodium alginate, chitosan, polydopamine, polyaniline or polyvinyl alcohol;
further, the two-dimensional sheet material is Ti2C nanosheet and Ti3C2Nano-meterSheet, Ti3CN nanosheet, V2C nanosheet and Nb2C nanosheet, TiNbC nanosheet and Nb4C3Nanosheet and Ta4C3Nanosheet, (Ti)0.5Nb0.5)2C nanosheet or (V)0.5Cr0.5)3C2One or a combination of any two or more of the nano sheets.
Further, the fatty acid is dodecanoic acid, tetradecanoic acid, pentadecanoic acid, palmitic acid, or stearic acid; the fatty acid ester is methyl stearate, methyl palmitate, hexadecahearate, octadecanoate, erythritol tetrastearate, erythritol tetrapalmitate or glycerol monostearate; the alcohol compound is dodecanol, tetradecanol, hexadecanol, octadecanol or polyethylene glycol with the molecular weight of 2000-20000.
Furthermore, the mass ratio of the metal ions to the high molecular compound to the two-dimensional sheet material is 1-2: 4-20: 20-50.
The second purpose of the invention can be achieved by adopting the following technical scheme:
a preparation method of a photo-thermal setting phase change energy storage composite material comprises the following steps:
the method comprises the following steps: fully grinding metal ions, a high molecular compound and a two-dimensional lamellar material with the formula ratio, ammonium bicarbonate and absolute ethyl alcohol, and then drying in vacuum until the absolute ethyl alcohol is completely volatilized to obtain a uniformly mixed prefabricated composite material;
step two: pressing and molding the uniformly mixed prefabricated composite material obtained in the step one; placing the materials under the sun illumination condition to completely decompose the ammonium bicarbonate to obtain a frame structure material with photo-thermal and heat conduction functions;
step three: and D, immersing the frame structure material with the photo-thermal and heat-conducting functions obtained in the step two into the molten organic phase-change energy storage material, carrying out vacuum impregnation, enabling the organic phase-change energy storage material to enter the frame under the assistance of vacuum, and filling the pores in the frame to obtain the photo-thermal sizing phase-change energy storage composite material.
Further, in the first step, the temperature of vacuum drying is 25-40 ℃; in the second step, the pressure for compression molding is 5-10T, and the compression time is 3-10 min.
Further, in the third step, the vacuum impregnation method comprises: and placing the frame structure material on the solid organic phase change material, keeping the pressure less than 20Pa, heating until the organic phase change material is completely melted, and keeping the temperature for vacuum impregnation for 6-12 h.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a photo-thermal setting phase-change energy storage composite material which is prepared from an organic phase-change energy storage material and a frame structure material with photo-thermal and thermal conductivity. The most critical of the materials is that metal ions, high molecular compounds and two-dimensional sheet materials form a stable frame structure material with photo-thermal and thermal conductivity.
One is as follows: two-dimensional slice layer Mn+1XnTxThe surface of the material contains abundant functional groups such as-F and-OH, and F and O have excellent coordination characteristics as atoms with large electronegativity; the macromolecular compound contains-COOH, -OH and-NH2The O and N atoms on the functional groups also have good coordination characteristics, and the metal ions have empty orbitals, so that the metal ions serve as coordination centers to form a two-dimensional sheet Mn+1XnTxThe polymer is effectively linked with a high molecular compound through a coordination covalent bond to form a three-dimensional space network structure and form a stable frame;
the second step is as follows: metal ions with positive charge, two-dimensional sheet layer Mn+1XnTxThe abundant-F and-OH on the surface lead F and O to have partial negative charges due to large electronegativity, and-COOH, -OH and NH in the macromolecular compound2O and N on the functional groups with the same polarity also have partial negative charges, so that certain electrostatic interaction exists among metal ions, high molecular compounds and the two-dimensional sheet material; the interaction has no directionality, and further strengthens the effective linkage of metal ions, the high molecular compound and the two-dimensional sheet material in the three-dimensional direction of the space; the stability of the frame is enhanced;
and thirdly: two-dimensional sheet layer Mn+1XnTxThe surface contains rich functional groups of-F, -OH and the like, and can be matched with-COOH, -OH and NH on a macromolecular compound2Complex and various intermolecular hydrogen bonds are formed among the polar functional groups, so that the stability of the framework is further enhanced, and meanwhile, the hydrogen bonds are also favorable for heat transfer, and the heat conductivity of the framework is improved.
In summary, the invention realizes the frame shaping and firming and the construction of the heat conduction path under the action of a certain pressure by virtue of the coordination electrostatic interaction of metal ions and the two-dimensional sheet material and the macromolecular compound material and the hydrogen bond synergistic bridging effect among molecules, so that the frame structure material has the functions of shaping, heat conduction path and photothermal conversion carrier, the problem that the frame material in the prior art is fragile under the action of external force is solved, and the problem that the heat conductivity cannot meet the actual application scene.
(2) The photo-thermal setting phase-change energy storage composite material provided by the invention has the effective effects that photo-thermal energy storage can be repeatedly carried out, the cycle performance is good, and the shape stability is good. The reason for this is that: on one hand, a stable framework formed by metal ions, high molecular compounds and two-dimensional sheet materials limits the flow of the liquid organic phase change material; on the other hand, fatty acids, fatty acid esters or alcohol compounds as organic phase change energy storage materials contain polar functional groups such as-COOH, -COOR or-OH, and these functional groups may be bonded to the two-dimensional sheet layer Mn+1XnTxThe surface of the polymer is rich in-F, -OH (or-COOH, -OH and NH of the polymer)2Among the polar functional groups), rich hydrogen bonds are formed, the interaction force between the polar functional groups and the hydrogen bonds is enhanced, and the photo-thermal cycle performance and the shape stability are improved;
in a word, the photothermal sizing phase-change energy storage composite material provided by the invention integrates photothermal conversion and energy storage, and has the advantages of excellent shape stability, stable heat transfer performance and high heat transfer speed; the maximum photo-thermal conversion efficiency can reach 95%, and the method has wide application prospects in the aspects of solar photo-thermal conversion, recycling and the like.
(3) According to the preparation method of the photo-thermal setting phase-change energy storage composite material, the photo-thermal effect of the two-dimensional lamellar material is utilized to quickly remove the ammonium bicarbonate template, and the framework structure material can be prepared without additional energy for heating. The method for efficiently removing the salt template has a simple preparation process (grinding, pressing and illumination), and is suitable for large-scale mass production.
(4) According to the preparation method of the photo-thermal setting phase-change energy storage composite material, the heat storage capacity can be regulated and controlled by simply regulating and controlling the mass fraction of the ammonium bicarbonate template agent, the mass fraction of the phase-change material can reach 80% at most, and the photo-thermal setting phase-change energy storage composite material can be applied to the fields with different heat capacity requirements.
(5) The preparation method of the photo-thermal setting phase change energy storage composite material has no solvation in the preparation process, and accords with the national advocated concepts of energy conservation, emission reduction, low carbon, environmental protection and greenization, so that the photo-thermal setting phase change energy storage composite material has wide application prospects in the aspects of solar photo-thermal conversion and the like.
Drawings
FIG. 1 is a view showing a state in which the frame structure materials produced in example 1(a) of the present invention and comparative example 1(b) were held by tweezers.
Fig. 2 is SEM images of the frame structure materials prepared in example 1(a) of the present invention and comparative example 1 (b).
FIG. 3 shows PEG8000 and Ti as raw materials in example 1 of the present invention3C2And XRD pattern of the prepared phase-change composite material.
Fig. 4 is a time-temperature graph of the phase change composite prepared in example 1 of the present invention and comparative example 2, and pure PEG8000 in a photothermal conversion storage test.
FIG. 5 is a diagram showing the state of the phase change composite materials prepared in examples 1 to 3 and comparative example 2 of the present invention and pure PEG8000 after heating at 30 deg.C, 50 deg.C, 70 deg.C, 90 deg.C, 110 deg.C for 5 min.
Detailed Description
The invention will be further described with reference to the accompanying drawings and the detailed description below:
the existing phase-change composite material obtained by vacuum impregnation of a phase-change material through a frame structure has a weak frame, is fragile under the action of external force, and the shape stability and the heat conductivity of the phase-change material cannot meet the practical application. Therefore, the invention provides the photo-thermal setting phase-change composite material with excellent shape stability, stable heat transfer performance and high heat transfer speed.
The photo-thermal setting phase change energy storage composite material is prepared from the following components in percentage by weight:
65% -80% of organic phase change energy storage material;
20% -35% of a frame structure material with photo-thermal and heat-conducting functions;
the organic phase change energy storage material is one or a composition of more than two of fatty acid, fatty acid ester or alcohol compounds;
the frame structure material with the photo-thermal and heat-conducting functions is made of metal ions, a high molecular compound and a two-dimensional sheet material.
As one embodiment of the invention, metal ions, a high molecular compound and a two-dimensional lamellar material are fully ground with ammonium bicarbonate and absolute ethyl alcohol according to a proportion, and then the mixture is dried in vacuum until the absolute ethyl alcohol is completely volatilized, so that a uniformly mixed prefabricated composite material is obtained; after compression molding, placing the mixture in the sun for irradiation, and obtaining a frame structure material with photo-thermal and heat conduction functions after ammonium bicarbonate is completely decomposed;
as an embodiment of the invention, the frame structure material is immersed into the molten organic phase-change material, vacuum impregnation is carried out, the organic phase-change material enters the frame structure material under the assistance of vacuum, and pores in the frame structure material are filled, so that the photo-thermal setting phase-change composite material is prepared.
In one embodiment of the present invention, the metal ion is one or a combination of two or more of chloride salts and nitrate salts of calcium ion, iron ion, cobalt ion, nickel ion, copper ion, and zinc ion.
In one embodiment of the present invention, the polymer compound is one or a combination of two or more of polyurethane, polyvinylpyrrolidone, starch, sodium alginate, chitosan, polydopamine, polyaniline, and polyvinyl alcohol.
As an embodiment of the invention, the two-dimensional lamellar material is Ti2C nanosheet and Ti3C2Nanosheet, Ti3CN nanosheet, V2C nanosheet and Nb2C nanosheet, TiNbC nanosheet and Nb4C3Nanosheet and Ta4C3Nanosheet, (Ti)0.5Nb0.5)2C nanosheet or (V)0.5Cr0.5)3C2One or a combination of any two or more of the nanosheets.
Under the action of certain pressure, the framework is shaped and firmed and a heat conduction passage is constructed by means of coordination of metal ions, a two-dimensional sheet material and a high polymer material, electrostatic interaction and hydrogen bond synergistic bridging among molecules.
Carbon atoms or nitrogen atoms are added into the metal lattice of the two-dimensional lamellar material, so that the MXene nanosheet can combine the characteristics of ceramics and metals, and has excellent light absorption capacity and local plasma resonance effect. After photons from solar radiation are captured by electrons on the MXene surface, a plasma resonance effect occurs due to the fact that the vibration frequency is consistent with the vibration frequency of the absorbed photons, the absorbed solar radiation is converted into heat energy through lattice scattering, and the heat energy is stored in the form of latent heat by the phase change material.
The two-dimensional sheet material has excellent photo-thermal conversion capability and has the photo-thermal conversion efficiency of 100% in a near infrared light region. And the two-dimensional sheet material is constructed into a frame structure, so that a heat conduction path is formed, and the heat transfer efficiency of the phase-change material is improved, so that the photo-thermal shaping phase-change material has high photo-thermal conversion efficiency.
As an embodiment of the present invention, the fatty acid is lauric acid, myristic acid, pentadecanoic acid, palmitic acid, or stearic acid. The fatty acid ester is methyl stearate, methyl palmitate, hexadecahearate, octadecanoate, erythritol tetrastearate, erythritol tetrapalmitate or glycerol monostearate; the alcohol compound is dodecanol, tetradecanol, hexadecanol, octadecanol or polyethylene glycol with molecular weight of 2000-20000.
According to one embodiment of the invention, the mass ratio of the metal ions, the high molecular compound and the two-dimensional sheet material is 1-2: 4-20: 20-50.
In the frame structure material, the two-dimensional sheet layer material plays a main frame structure role, the high molecular compound and metal ions enter the two-dimensional sheet layer material, and the frame is shaped and solidified under the assistance of certain pressure through coordination, electrostatic interaction and intermolecular hydrogen bond synergistic bridging, and a heat conduction passage is constructed at the same time. Therefore, the two-dimensional sheet material which plays the main framework structure accounts for the highest proportion, and the high molecular compound and the metal ions are arranged in the second place.
A preparation method of a photo-thermal setting phase change energy storage composite material comprises the following steps:
the method comprises the following steps: fully grinding metal ions, a high molecular compound and a two-dimensional lamellar material with a formula ratio with ammonium bicarbonate and absolute ethyl alcohol, and then drying in vacuum until the absolute ethyl alcohol is completely volatilized to obtain a uniformly mixed prefabricated composite material;
step two: pressing and molding the uniformly mixed prefabricated composite material obtained in the step one; placing the materials under the sun illumination condition to completely decompose the ammonium bicarbonate to obtain a frame structure material with photo-thermal and heat conduction functions;
step three: and D, immersing the frame structure material with the photo-thermal and heat-conducting functions obtained in the step two into the molten organic phase-change energy storage material, carrying out vacuum impregnation, enabling the organic phase-change energy storage material to enter the frame under the assistance of vacuum, and filling the pores in the frame to obtain the photo-thermal sizing phase-change energy storage composite material.
The photo-thermal effect of the two-dimensional lamellar material can be utilized to quickly remove the ammonium bicarbonate template agent, the frame structure material can be prepared without additional energy for heating, and the shape stability is excellent. The efficient salt template method and the simple preparation process (grinding, pressing, illumination and impregnation) thereof can be used for preparing the phase-change materials with different shapes according to needs, and have very important significance for large-scale preparation of frame structure materials and practical application thereof in the field of solar photo-thermal conversion.
The heat storage capacity can be regulated and controlled by simply regulating and controlling the mass fraction of the ammonium bicarbonate template agent, the mass fraction of the phase-change material can reach 80 percent at most, and the phase-change material can be applied to the fields with different heat capacity requirements
Preferably, the mass of the ammonium bicarbonate is 8.0-10.0 times of the mass of the two-dimensional sheet material.
Preferably, in the second step, the light irradiation is sunlight, and the time of the sunlight irradiation is 4 to 8 hours.
According to the embodiment of the invention, after the vacuum impregnation in the third step, the frame structure material filled with the organic phase change material is taken out and cooled to room temperature, so as to prepare the photo-thermal setting phase change energy storage composite material.
In one embodiment of the invention, in the first step, the temperature of vacuum drying is 25-40 ℃; in the second step, the pressure for compression molding is 5-10T, and the compression time is 3-10 min.
In the third step, the vacuum impregnation method is as follows: and (3) placing the frame structure material on the solid organic phase-change material, keeping the pressure less than 20Pa, heating until the organic phase-change material is completely molten, and keeping the temperature for vacuum impregnation for 6-12 h.
The following is further illustrated in connection with specific examples:
example 1
The photo-thermal setting phase change energy storage composite material is prepared from the following components in percentage by weight:
80 percent of organic phase change energy storage material
20% of frame structure material with photo-thermal and heat conduction functions;
in this embodiment, the organic phase change energy storage material is an alcohol compound, and the alcohol compound is polyethylene glycol (PEG8000) with an average molecular weight of 8000;
the frame structure material with the photo-thermal and heat-conducting functions is made of metal ions, a macromolecular compound and a two-dimensional sheet material;
in this example, the metal ion is calcium chloride (CaCl)2) (ii) a The high molecular compound is polyvinylpyrrolidone (PVP); the two-dimensional lamellar material is Ti3C2Nanosheets;
in this example, the mass ratio of the metal ions, the polymer compound, and the two-dimensional sheet material was 1: 2: 20.
A preparation method of a photo-thermal setting phase change energy storage composite material comprises the following steps:
the method comprises the following steps: weighing metal ions, a high molecular compound, a two-dimensional lamellar material and ammonium bicarbonate according to the mass ratio of 1: 2: 20: 200, transferring the weighed materials into a mortar, adding a proper amount of absolute ethyl alcohol into the mortar, fully grinding the materials, transferring the mortar and the mixture into a vacuum oven, and drying the mortar and the mixture at the temperature of 40 ℃ for 1 hour until the absolute ethyl alcohol is completely volatilized to obtain a uniformly mixed prefabricated composite material;
step two: transferring the uniformly mixed prefabricated composite material obtained in the first step into a mold, pressing for 5min by using a press machine under the pressure of 8T, pressing into a wafer, placing the prepared wafer under the sunlight for 6h, and obtaining a frame structure material after ammonium bicarbonate is completely decomposed;
step three: immersing the frame structure material prepared in the second step into the organic phase-change material in a molten state, placing the frame structure material on the solid organic phase-change material, keeping the pressure at less than 20Pa, heating the system until the organic phase-change material is completely molten, and keeping the temperature for vacuum impregnation for 10 hours; making the organic phase-change material enter the frame structure material under the assistance of vacuum so as to fill the pores in the frame structure material;
step four: and taking out the frame structure material filled with the organic phase change material in the third step, and cooling to room temperature to obtain the photo-thermal setting phase change energy storage composite material.
Example 2
The mass ratio of the metal ions, the high molecular compound, the two-dimensional lamellar material and the ammonium bicarbonate was changed to 1: 2: 20: 180, and the other conditions were the same as in example 1.
Example 3
The mass ratio of the metal ions, the high molecular compound, the two-dimensional lamellar material and the ammonium bicarbonate was changed to 1: 2: 20: 160, and the other conditions were the same as in example 1.
Example 4
The photo-thermal setting phase-change composite material is prepared from the following components in percentage by weight:
70 percent of organic phase change energy storage material
30% of frame structure material with photo-thermal and heat conduction functions;
in this embodiment, the organic phase change material is fatty acid, and the fatty acid is stearic acid.
The frame structure material is made of metal ions, high polymers and a two-dimensional sheet material;
in this embodiment, the metal ion is copper chloride (CuCl)2) (ii) a The macromolecular compound is chitosan; the two-dimensional lamellar material is Nb2C nano-sheet;
in this example, the mass ratio of the metal ions, the polymer compound, and the two-dimensional sheet material was 1: 2: 20.
A preparation method of a photo-thermal setting phase change energy storage composite material comprises the following steps:
the method comprises the following steps: weighing metal ions, a high molecular compound, a two-dimensional lamellar material and ammonium bicarbonate according to the mass ratio of 1: 2: 20: 175, transferring the weighed materials into a mortar, adding a proper amount of absolute ethyl alcohol into the mortar, fully grinding the materials, transferring the mortar and the mixture of the mortar into a vacuum oven, and drying the mortar and the mixture at 25 ℃ for 5 hours until the absolute ethyl alcohol is completely volatilized to obtain a uniformly mixed prefabricated composite material;
step two: transferring the prefabricated composite material uniformly mixed in the step one into a mold, pressing for 10min by using a press machine under the pressure of 5T, pressing into a wafer, placing the prepared wafer under sunlight for illumination for 4h, and obtaining a frame structure material after ammonium bicarbonate is completely decomposed;
step three: immersing the frame structure material prepared in the second step into the organic phase-change material in a molten state, placing the frame structure material on the solid organic phase-change material, keeping the pressure at less than 20Pa, heating the system until the organic phase-change material is completely molten, and keeping the temperature for vacuum impregnation for 6 hours; making the organic phase-change material enter the frame structure material under the assistance of vacuum so as to fill the pores in the frame structure material;
step four:
and taking out the frame structure material filled with the organic phase change material in the third step, and cooling to room temperature to obtain the photo-thermal setting phase change energy storage composite material.
Example 5
The photo-thermal setting phase change energy storage composite material is prepared from the following components in percentage by weight:
80% of organic phase change energy storage material;
20% of frame structure material with photo-thermal and heat conduction functions;
in the embodiment, the organic phase change material is fatty acid, and the fatty acid is a composition of pentadecanoic acid and palmitic acid according to the mass ratio of 1: 1;
the frame structure material is made of metal ions, high polymers and a two-dimensional sheet material;
in this example, the metal ion is zinc chloride (ZnCl)2) (ii) a The polymer is a composition of chitosan and polyaniline according to the mass ratio of 1: 1; the two-dimensional lamellar material is Ti2C nanosheet and V2C nano-sheet is a composition with the mass ratio of 1: 1.
In this example, the mass ratio of the metal ions, the polymer, and the two-dimensional sheet material was 1: 2: 20.
A preparation method of a photo-thermal setting phase change energy storage composite material comprises the following steps:
the method comprises the following steps: weighing metal ions, a high molecular compound, a two-dimensional lamellar material and ammonium bicarbonate according to the mass ratio of 1: 2: 20: 190, transferring the weighed materials into a mortar, adding a proper amount of absolute ethyl alcohol into the mortar, fully grinding the materials, transferring the mortar and the mixture of the mortar into a vacuum oven, and drying the mortar and the mixture at 33 ℃ for 2.5 hours until the absolute ethyl alcohol is completely volatilized to obtain a uniformly mixed prefabricated composite material;
step two: transferring the uniformly mixed prefabricated composite material obtained in the first step into a mold, pressing for 3min by using a press machine under the pressure of 10T, pressing into a wafer, placing the prepared wafer under the sunlight for illumination for 4h, and obtaining a frame structure material after ammonium bicarbonate is completely decomposed;
step three: immersing the frame structure material prepared in the second step into the organic phase-change material in a molten state, placing the frame structure material on the solid organic phase-change material, keeping the pressure at less than 20Pa, heating the system until the organic phase-change material is completely molten, and keeping the temperature for vacuum impregnation for 12 hours; making the organic phase-change material enter the frame structure material under the assistance of vacuum so as to fill the pores in the frame structure material;
step four:
and (4) taking out the frame structure material filled with the organic phase change material in the third step, and cooling to room temperature to obtain the photo-thermal setting phase change energy storage composite material.
Example 6
The photo-thermal shaping phase-change energy storage composite material is characterized in that: is prepared from the following components in percentage by weight:
65% of organic phase change energy storage material;
35% of frame structure material with photo-thermal and heat conduction functions;
in the embodiment, the organic phase change energy storage material is a mixture of fatty acid and fatty acid ester according to the mass ratio of 1: 1, the fatty acid is pentadecanoic acid, and the fatty acid ester is methyl stearate;
the frame structure material is made of metal ions, high polymers and a two-dimensional sheet material;
in this example, the metal ion was cobalt chloride (CoCl)2) (ii) a The polymer is a composition of starch and polydopamine according to the mass ratio of 1: 1; the two-dimensional lamellar material is Ti3C2Nanosheet and Ta4C3The nano-sheets are in a mass ratio of 1: 1.
In this example, the mass ratio of the metal ions, the polymer, and the two-dimensional sheet material was 1: 2: 20.
The preparation method of the photo-thermal setting phase-change energy storage composite material is the same as that of the embodiment 1.
Example 7
The mass ratio of the metal ions, the high molecular compound, the two-dimensional lamellar material and the ammonium bicarbonate was changed to 1: 5: 10: 180, and the other conditions were the same as in example 1.
Example 8
The mass ratio of the metal ions, the high molecular compound, the two-dimensional lamellar material and the ammonium bicarbonate was changed to 1: 3.5: 50: 160, and the other conditions were the same as in example 1.
Comparative example 1
Mixing Ti3C2Weighing the nanosheets and the ammonium bicarbonate according to the mass ratio of 20: 90, and then transferring the nanosheets and the ammonium bicarbonate into a mortar for full grinding; grinding the Ti uniformly3C2Transferring the mixture of the nanosheets and ammonium bicarbonate into a mold, and tabletting by using a press machine, wherein the pressure and the time are 8T and 5min respectively to obtain a hard wafer; placing the prepared wafer under sunlight for illumination for 6h, and obtaining a frame structure material after ammonium bicarbonate is completely decomposed;
comparative example 2
Adding CaCl2PVP and Ti3C2The nano-sheets are weighed and dispersed in ethanol according to the mass ratio of 1: 2: 20, and are ultrasonically dispersed for 30min to obtain dispersion liquid; and (3) heating the obtained dispersion to 90 ℃, adding 1.5g of polyethylene glycol with the average molecular weight of 8000 into the system, continuously stirring for 1h, transferring the mixture into a mold, and placing the mold in a vacuum oven to dry until the temperature is constant, thereby obtaining the phase-change composite material.
Comparative example 3
The metal ions, the high molecular compound, the two-dimensional lamellar material and the ammonium bicarbonate are weighed in a mass ratio of 1: 20: 200, and other conditions are the same as those in example 1. It is worth noting that during the grinding process, it is found that the viscosity of the mixture is obviously increased, the time required for vacuum drying is longer, and the frame after decomposing the ammonium bicarbonate is relatively flexible due to the high polymer content, so that the frame is obviously shrunk, and the pouring of PEG is not facilitated.
Comparative example 4
The metal ions, the polymer, the two-dimensional lamellar material and the ammonium bicarbonate were weighed in a mass ratio of 1: 2: 20: 250, and the other conditions were the same as in example 1. It should be noted that after the template agent ammonium bicarbonate is decomposed, the frame is also damaged by being carefully clamped by forceps, so that the frame with an excessive ammonium bicarbonate content is fragile and is not beneficial to pouring of PEG.
Comparative example 5
The metal ions, the polymer, the two-dimensional lamellar material and the ammonium bicarbonate were weighed in a mass ratio of 1: 2: 20: 130, and the other conditions were the same as in example 1. It should be noted that after decomposition of the templating agent ammonium bicarbonate, the frame was very strong and did not break even when dropped from a height. Ammonium bicarbonate content is low, framework stability is enhanced, but void volume is significantly reduced, which is not conducive to absorbing more PEG.
Comparative analysis of appearance and properties of examples and comparative examples:
(1) experimental example 1 and comparative example 1
The frame structure materials obtained in example 1 and comparative example 1 were held by tweezers and subjected to appearance observation, and the results are shown in fig. 1:
as can be seen from fig. 1(a), the frame structure material prepared from metal ions and polymers can withstand the clamping of tweezers and has certain flexibility. As can be seen from FIG. 1(b), a similar preparation process is adopted, after the template ammonium bicarbonate is decomposed, Ti3C2The frame structure material constructed by the nanosheets is very fragile, and the frame is very easy to damage without being clamped by tweezers. The metal ions and the high molecular compounds play an important role in preparing the shaped frame structure material, and the small amount of the metal ions and the high molecular compounds ensures that the shape of the frame structure material is firm.
The frame structure materials of example 1 and comparative example 1 were subjected to Scanning Electron Microscope (SEM) image analysis, and the results are shown in fig. 2:
as shown in the SEM image of the frame structure material prepared in example 1 in FIG. 2(a), the frame structure material of example 1 is decomposed by ammonium bicarbonate, and a large number of pores are formed in the frame due to the template effect, and the pores are formed due to the presence of metal ions and high moleculesThe function of the bridge is similar to that of a bridge, so that the gaps are communicated with each other. Comparative example 1 pure Ti as shown in FIG. 2(b)3C2Gaps of the framework constructed by the nano sheets are not communicated with each other, so that the framework structure is loose and fragile.
(2) XRD characterization of composites prepared in example 1
For the phase change composite material prepared in the embodiment 1 of the invention, the organic phase change materials PEG8000 and two-dimensional Mxene Ti3C2The XRD characterization was performed separately, and the results are shown in FIG. 3.
From the analysis of the figure, in the XRD pattern of the phase change composite material prepared in example 1, the characteristic crystallization peak of pure PEG8000 and Ti exist simultaneously3C2Characteristic peak of (2); with Ti 302The diffraction peak in the composite material is obviously shifted to the left compared with the diffraction peak at the position of 10 degrees, which shows that PEG8000 enters two-dimensional Ti during the vacuum impregnation process3C2Causing an increase in the interlayer spacing; the intercalation of PEG8000 is favorable to PEG8000 and two-dimensional Ti3C2The interaction force between the two is enhanced, and the shape stability of the phase change material is further enhanced.
(3) Comparative shape stability between examples 1 to 3 and comparative example 2
The phase change composite materials prepared in the embodiments 1-3 and the comparative example 2 and the pure PEG8000 are placed on a heating table, and are heated at constant temperature of 30 ℃, 50 ℃, 70 ℃, 90 ℃ and 110 ℃ for 5min respectively, the melting, overflowing and flowing characteristics of the organic phase change material are contrastingly observed, the shape stability of the composite material is judged, and the test experiment result is shown in figure 5.
As can be seen, pure PEG8000 and comparative example 2 (phase change composite prepared by melt blending method) were substantially completely melted into liquid by heating at 70 ℃ for 5 min; while the original state of the samples 1-3 is basically maintained after heating at 70 ℃ for 5 min; when heated at 90 ℃ for 5min, a small amount of PEG8000 on the surface of the sample 1 begins to melt, but the samples 2 and 3 basically keep the original state; even if the phase change material is heated at 110 ℃ for 5min, PEG8000 which is obviously melted on the surfaces of the embodiment 2 and the embodiment 3 is not observed, which shows that the frame structure prepared by adopting metal ions, high molecular compounds and two-dimensional sheet materials is stable, and the technical problem that the phase change material is easy to leak in the phase change process can be effectively solved.
(4) Comparison of thermal conductivity, energy storage property, and photothermal conversion property of examples 1 to 3 and comparative examples 2 to 5.
Thermal conductivity test method: the thermal conductivity of the sample was calculated according to the formula λ ═ α × ρ × Cp, where a is the thermal diffusivity of the sample, and the thermal diffusivity of the phase change composite was measured using an LFA467 type laser thermal conductivity tester manufactured by NETZSCH, germany, and the sample was cut to the size required by the tester and uniformly coated with a graphite layer before the test. ρ is the density of the sample, measured by gravimetric method. Cp is the specific heat capacity of the sample, and is measured by a differential scanning calorimeter model DSC3 from METTLER and by the sapphire specific heat method.
Energy storage performance test method
The DSC3 model differential scanning calorimeter of METTLER company is adopted at N2And repeatedly measuring for 20 times under the atmosphere to obtain the fusion enthalpy of the PEG8000 and the phase-change composite material.
The test method of the photothermal conversion performance comprises the following steps: the sample was placed on a PET foam plate, irradiated with a xenon lamp light source loaded with an AM1.5 filter, and the temperature of the sample surface was recorded with an infrared thermal imager to generate a temperature-time curve. The photothermal efficiency of the phase change composite material is calculated according to the formula η ═ m Δ Hm/(P (ts-te)), where m is the mass of the sample, Δ Hm is the melting enthalpy of the sample, P is the power of the simulated solar radiation, ts is the time to start the melting process, and te is the end time of the melting process (ts and te are obtained by the tangent method).
The phase change composite materials of example 1 and comparative example 2 and pure PEG8000 were irradiated under a xenon lamp, and the change in temperature of the materials with time was measured, and the result is shown in fig. 4. As can be seen from fig. 4, when the xenon lamp is turned on, all samples start to heat up, and the sample corresponding to example 1 heats up fastest, which can illustrate that the heat transfer performance of the frame in the sample is good; subsequently, both example 1 and comparative example 2 underwent a marked melting behavior; when the xenon lamp was turned off after 1000s of irradiation, all samples rapidly cooled, and the temperature of example 1 and comparative example 2 remained substantially constant for a period of time due to the exothermic heat of solidification of PEG, while the temperature of pure PEG8000 was slowly cooled to room temperature. The more latent heat stored, the longer the heat release lasts under the same environmental conditions. It can be seen that when example 1 is cooled to the phase transition temperature after turning off the lamp, latent heat starts to be released, and the heat release lasts for 250s, while that of comparative example 2 lasts for 187s, which shows that example 1 has better heat storage capacity under the same irradiation intensity and time.
The thermal conductivity, melting enthalpy, photothermal efficiency and shape stability of examples 1 to 3 and comparative examples 2 to 5 are shown in table 1.
As can be seen from Table 1, the phase change composite materials of examples 1-3, which were prepared by the salt templating method and contain metal ions and high molecular compounds, had thermal conductivity, photo-thermal efficiency, and shape stability, which were significantly superior to those of comparative example 2 (prepared by melt blending), and the thermal conductivity was 4.84-7.9 times that of pure PEG 8000. In addition, the phase change enthalpy value of the phase change composite material in the embodiment 1 is 133.1J/g, 80% of the enthalpy value of PEG8000(166.4J/g) can be reserved, and the obtained composite phase change energy storage material has good heat transfer capacity, higher phase change enthalpy value and excellent photo-thermal conversion and storage capacity.
Comparing the performances of examples 1 to 3 with comparative examples 4 and 5, it can be seen that when a frame structure material is designed and prepared, the amount of template agent ammonium bicarbonate is reduced, the structure and shape stability of the frame is better, the heat conductivity coefficient of the frame is increased, and the photo-thermal efficiency is enhanced, but the heat storage performance is reduced along with the reduction of the relative amount of the organic phase change material, the reduction of the melting enthalpy; when the amount of ammonium bicarbonate is reduced to 85.0 wt% of the frame material, the melting enthalpy of comparative example 5 is reduced to less than 100J/g, and the basic requirement of phase change energy storage cannot be met; when the relative amount of ammonium bicarbonate is increased and the templating agent is decomposed, the stability of the framework is somewhat affected, and when the amount of ammonium bicarbonate is increased to 91.6 wt%, comparative example 4 forms a very fragile framework even though the interaction is enhanced by the addition of the metal ion and the high molecular compound.
Comparing the properties of example 1 and comparative example 3 it can be seen that the addition of PVP in a proper amount results in a relatively viscous pre-formed composite material, a difficult processing to prepare a frame material, and a reduced thermal conductivity of the composite material if the PVP is added in an amount exceeding 8.2 wt%, indicating that a proper range of the amount of the polymeric compound is required.
In summary, the present invention provides a photo-thermal setting phase-change energy-storage composite material made of an organic phase-change material and a frame structure material. By utilizing the characteristic that ammonium bicarbonate is easy to decompose at low temperature and the photo-thermal effect of the two-dimensional lamellar material, metal ions and a small amount of high polymer material are prepared into the frame structure material with the photo-thermal and heat-conducting functions by a salt template method. Under the action of a certain pressure, the frame is shaped and firmed and a heat conduction passage is constructed by virtue of the synergistic bridging effect among metal ions, a high polymer material and a two-dimensional sheet material; and loading the phase change material into a porous frame by a vacuum impregnation method to finally prepare the shaped phase change energy storage composite material. The phase-change composite material has the advantages of excellent shape stability, high heat transfer speed and integration of light-heat conversion and energy storage; the heat storage capacity can be regulated by simply regulating the mass fraction of the ammonium bicarbonate template agent, the mass fraction of the phase-change material can reach 80 percent at most, and the phase-change material can be applied to the fields with different heat capacity requirements. In addition, the phase-change composite material also has excellent photo-thermal conversion effect, the photo-thermal conversion efficiency can reach 95 percent at most, and the phase-change composite material can be used in the fields of solar photo-thermal conversion and the like.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (9)
1. The photo-thermal setting phase change energy storage composite material is characterized by being prepared from the following components in percentage by weight:
65% -80% of organic phase change energy storage material;
20% -35% of frame structure material with photo-thermal and heat-conducting functions;
the organic phase change energy storage material is one or a composition of more than two of fatty acid, fatty acid ester or alcohol compounds;
the frame structure material with the photo-thermal and heat-conducting functions is made of metal ions, a macromolecular compound and a two-dimensional sheet material.
2. The photothermal fixed phase change energy storage composite material as claimed in claim 1, wherein the metal ion is one or a combination of two or more of chloride and nitrate of calcium ion, iron ion, cobalt ion, nickel ion, copper ion and zinc ion.
3. The photothermal typing phase change energy storage composite material as claimed in claim 1, wherein the high molecular compound is one or a composition of more than two of polyurethane, polyvinylpyrrolidone, starch, sodium alginate, chitosan, polydopamine, polyaniline and polyvinyl alcohol.
4. The photothermal stereotyped phase change energy storage composite material as claimed in claim 1, wherein said two-dimensional sheet material is Ti2C nanosheet and Ti3C2Nanosheet, Ti3CN nanosheet, V2C nanosheet and Nb2C nanosheet, TiNbC nanosheet and Nb4C3Nanosheet and Ta4C3Nanosheet, (Ti)0.5Nb0.5)2C nano sheet, (V)0.5Cr0.5)3C2One or a combination of any two or more of the nanosheets.
5. The photothermal fixing phase change energy storage composite material as claimed in claim 1, wherein the fatty acid is one or a combination of any two or more of lauric acid, myristic acid, pentadecanoic acid, palmitic acid, and stearic acid; the fatty acid ester is one or a composition of more than two of methyl stearate, methyl palmitate, hexadecahearate, octadecanoate, erythritol tetrastearate, erythritol tetrapalmitate and glycerin monostearate; the alcohol compound is one or a composition of more than two of dodecanol, tetradecanol, hexadecanol, octadecanol and polyethylene glycol with the molecular weight of 2000-20000.
6. The photothermal sizing phase change energy storage composite material as claimed in claim 1, wherein the mass ratio of the metal ions, the high molecular compound and the two-dimensional sheet material is 1-2: 4-20: 20 to 50.
7. The preparation method of the photo-thermal setting phase change energy storage composite material is characterized by comprising the following steps of:
the method comprises the following steps: fully grinding metal ions, a high molecular compound and a two-dimensional lamellar material with the formula ratio, ammonium bicarbonate and absolute ethyl alcohol, and then drying in vacuum until the absolute ethyl alcohol is completely volatilized to obtain a uniformly mixed prefabricated composite material;
step two: pressing and molding the uniformly mixed prefabricated composite material obtained in the step one; placing the materials under the sun illumination condition to completely decompose the ammonium bicarbonate to obtain a frame structure material with photo-thermal and heat conduction functions;
step three: and D, immersing the frame structure material with the photo-thermal and heat-conducting functions obtained in the step two into the molten organic phase-change energy storage material, carrying out vacuum impregnation, enabling the organic phase-change energy storage material to enter the frame under the assistance of vacuum, and filling the pores in the frame to obtain the photo-thermal sizing phase-change energy storage composite material.
8. The preparation method of the photothermal stereotyped phase change energy storage composite material as claimed in claim 7, wherein in the first step, the temperature of vacuum drying is 25-40 ℃; in the second step, the pressure for compression molding is 5-10T, and the compression time is 3-10 min.
9. The method for preparing the photothermal stereotyped phase change energy storage composite material according to claim 7, wherein in the third step, the vacuum impregnation method comprises the following steps: placing a frame structure material with photo-thermal and heat-conducting functions on a solid organic phase-change energy storage material, keeping the pressure less than 20Pa, heating until the organic phase-change energy storage material is completely molten, and keeping the temperature for vacuum impregnation for 6-12 h.
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