CN113105871A - Phase-change heat storage material with bionic structure and preparation method and application thereof - Google Patents
Phase-change heat storage material with bionic structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a phase-change heat storage material with a bionic structure, and a preparation method and application thereof, and belongs to the technical field of phase-change heat storage materials. The phase-change heat storage material provided by the invention comprises a composite core and a shell layer coated on the surface of the composite core; the composite core comprises a porous material and a phase change substance filled in pores and gaps of the porous material. According to the invention, by imitating fruits with high water content such as watermelon and towel gourd and using the network-shaped cytoplasm partition wall structure in the fruits, firstly, phase change substances are filled in holes and gaps of porous materials to form a composite core, then, by using the epidermis structure of the fruits with high water content, a shell layer is coated on the surface of the composite core, and the phase change substances are fixed by the cooperation of the adsorption and shaping effects of the porous networks in the porous materials and the coating effect of the shell layer, so that the phase change substances are prevented from leaking in the solid/liquid conversion process; meanwhile, the porous material with the network structure can also obviously improve the heat conduction capability of the phase change substance.
Description
Technical Field
The invention belongs to the technical field of phase-change heat storage materials, and particularly relates to a phase-change heat storage material with a bionic structure, and a preparation method and application thereof.
Background
The phase-change material can absorb/release a large amount of heat when phase transition (solid/liquid, liquid/gas and the like) occurs, and meanwhile, the temperature fluctuation is small, so the phase-change energy storage technology utilizing the phase-change material has unique advantages and wide application prospects in the aspects of heat energy storage and utilization.
In the actual use process, the phase change material is often used after being packaged, for example, the organic phase change material is coated into a micro capsule, for example, researchers use organic polymers such as polymethyl methacrylate (PMMA) as shell materials, and organic matters such as paraffin/alkane fatty acid are sealed inside to form a heat storage microcapsule. The patent with the application number of 201510143894.4 discloses a phase change heat storage micro-capsule coated by an organic shell, which is prepared by taking fatty acid as a core material and polymethyl methacrylate as a shell through suspension polymerization, photocuring and other methods; the tremajeff (functional material 2016,1(47): 01199-. The packaging technology of the method is mature, but the volume fraction of the coating material (namely, organic matter shell) in the whole is too high, so that the effective content of the phase change material is low; the thermal conductivity of the organic shell is not high, and the phase change material is coated by the organic shell, so that the thermal response speed of the phase change material cannot be increased.
Disclosure of Invention
The invention provides a phase-change heat storage material with a bionic structure, and a preparation method and application thereof, aiming at overcoming the defects of the prior art and solving the technical problems that the volume fraction of a coating material in a phase-change heat storage material with a core-shell structure in the whole is too high and the thermal response speed of a phase-change material is low.
The invention is realized by the following technical scheme.
The phase-change heat storage material with the bionic structure comprises a composite core and a shell layer coated on the surface of the composite core, wherein the composite core comprises a porous material and a phase-change substance filled in holes and gaps of the porous material.
Further, the phase change material is paraffin.
Further, the porous material is graphite foam or graphene foam, and the density of the porous material is 0.1-0.5 g/cm3The porosity is 70-95%.
Furthermore, the shell layer is made of graphene oxide.
Furthermore, the diameter of the composite core is 20-50 μm, and the thickness of the shell layer is 10-100 nm.
Further, the content of a phase-change substance in the phase-change heat storage material is 50-80 wt.%, and the mass ratio of the phase-change substance to the porous material is (1-9): 1.
A preparation method of a phase-change heat storage material with a bionic structure comprises the following steps: firstly, impregnating or vacuum-absorbing a porous material in a liquid phase-change substance, and crushing an obtained product after cooling to obtain a composite core; and then, depositing a shell layer on the surface of the prepared composite core, and drying to obtain the phase-change heat storage material.
Further, the pressure of the dipping environment is more than or equal to 0.08KPa, and the time is 2-8 h;
the vacuum adsorption comprises vacuum heat preservation and pressure maintaining which are sequentially carried out; the vacuum heat preservation environment pressure is more than or equal to 0.06KPa, the temperature is 80-120 ℃, and the heat preservation time is 2-3 h; the pressure maintaining environment is 0.3-0.5 MPa, and the pressure maintaining time is 2-3 h.
Further, the deposition method of the shell layer comprises the following steps: coating the water dispersion of the shell material on the surface of the composite core; the coating method is spraying or fluidized coating; the concentration of the aqueous dispersion of the shell material is 2-4 mg/mL.
The phase-change heat storage material or the phase-change heat storage material prepared by the preparation method is applied to the fields of solar energy, buildings, constant-temperature drying or electronic device heat management.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, by imitating fruits with high water content such as watermelon and towel gourd and using the network-shaped cytoplasm partition wall structure in the fruits, firstly, the phase change substances are filled in the holes and gaps of the porous material to form a composite core, and then, by using the epidermis structure of the fruits with high water content, the surface of the composite core is coated with a shell layer. According to the invention, the phase change substance is synergistically fixed by the adsorption and shaping effects of the porous network in the porous material and the coating effect of the shell layer, so that the phase change substance is prevented from leaking in the solid/liquid conversion process, the loss of the phase change substance is reduced, and the higher phase change enthalpy of the phase change material is kept; meanwhile, the porous material with the network structure can also obviously improve the heat conduction capability of the phase change material, and is beneficial to the obtained phase change heat storage material to have higher heat conductivity.
The test results of the embodiment show that the content of the heat storage substance in the phase-change heat storage material provided by the invention reaches 50-78 wt.%, and the content of the heat storage substance is high; the thermal conductivity reaches 1.9-6.5W/mK, and the thermal conductivity is high; the leakage rate is 1.8-4.1% after the material is placed for 200 hours at the temperature of 60 ℃, and the leakage rate is low.
Drawings
Fig. 1 is a flow chart of a preparation method of a phase-change heat storage material with a bionic structure.
Detailed Description
The invention provides a phase-change heat storage material with a bionic structure, which comprises a composite core and a shell layer coated on the surface of the composite core, wherein the composite core comprises a porous material and a phase-change substance filled in holes and gaps of the porous material.
In the present invention, the phase change material is preferably a solid-liquid phase change material, and more preferably includes paraffin. In the invention, the solid/liquid phase transition temperature of the paraffin is preferably 30-80 ℃.
In the present invention, the porous material preferably includes graphite foam or graphene foam. In the invention, the density of the porous material is preferably 0.1-0.5 g/cm3More preferably 0.15 to 0.45g/cm3. In the present invention, the porosity of the porous material is preferably 70 to 95%, more preferably 75 to 90%, and most preferably 85%.
In the invention, the diameter of the composite core is preferably 20-50 μm; more preferably 25 to 45 μm. In the invention, the mass ratio of the phase change substance to the porous material is preferably (1-9): 1, more preferably (2-8): 1; the content of the phase-change substance in the phase-change heat storage material is preferably 50-80 wt.%, and more preferably 55-75 wt.%.
In the present invention, the material of the shell layer is preferably graphene oxide. In the invention, the thickness of the shell layer is preferably 10-100 nm, and more preferably 35-60 nm.
The invention also provides a preparation method of the phase-change heat storage material in the technical scheme, which comprises the following steps:
soaking or vacuum adsorbing the porous material in a liquid phase-change substance, and cooling and crushing the obtained product to obtain a composite core;
and after a shell layer is deposited on the surface of the composite core, drying to obtain the phase-change heat storage material.
In the present invention, unless otherwise specified, each component in the preparation method is a commercially available product well known to those skilled in the art.
The porous material is soaked or vacuum-absorbed in the liquid phase-change substance, and the obtained product is cooled and then crushed to obtain the composite core.
The impregnation is not particularly limited in the present invention, so as to enable filling of the phase change substance into the pores and pores of the porous material.
In the invention, the environmental pressure of the impregnation is preferably more than or equal to 0.08KPa, and more preferably 0.08 KPa-0.3 MPa; the time is preferably 2 to 8 hours, and more preferably 2 to 7 hours.
Before the impregnation, the invention also comprises melting the phase-change substance to ensure that the phase-change substance is in a liquid state.
In the present invention, the vacuum adsorption comprises the steps of: covering the surface of the porous material with a solid phase-change material, and then sequentially carrying out vacuum heat preservation and pressure maintaining. In the invention, the environment pressure of the vacuum heat preservation is preferably not less than 0.06KPa, the temperature is preferably 80-120 ℃, and the heat preservation time is preferably 2-3 h; the pressure maintaining environment is preferably 0.3-0.5 MPa, and more preferably 0.3-0.4 MP a; the pressure maintaining time is preferably 2 to 3 hours, and more preferably 2 to 2.5 hours.
The cooling is not particularly limited in the present invention, and may be any cooling known to those skilled in the art, specifically, natural cooling. In the present invention, the crushing is preferably mechanical crushing, air stream crushing or ball milling. The specific process of mechanical crushing, gas stream crushing or ball milling is not particularly limited in the present invention, and processes well known to those skilled in the art may be used.
After the composite core is obtained, the shell layer is deposited on the surface of the composite core, and then the composite core is dried to obtain the phase-change heat storage material.
In the present invention, the deposition method of the shell layer is preferably: and coating the water dispersion of the shell material on the surface of the composite core. In the present invention, the coating method is preferably spray or fluidized coating. In the invention, the concentration of the aqueous dispersion of the shell material is preferably 2-4 mg/mL, and more preferably 2-3.5 mg/mL. The spray and fluidized coating of the present invention is not particularly limited, and those known to those skilled in the art can be used.
In the present invention, the drying is preferably vacuum drying. In the invention, the drying temperature is preferably 35-45 ℃, and more preferably 35-40 ℃; the vacuum degree is preferably more than or equal to 0.06 KPa; the time is preferably 24 to 48 hours, and more preferably 24 to 36 hours. In the present invention, the drying apparatus is preferably a drying oven, more preferably a vacuum drying oven.
Fig. 1 is a flow chart of a preparation method of a phase-change heat storage material with a bionic structure, and as can be seen from fig. 1, the preparation method provided by the invention is that a phase-change substance and a porous material are mixed, impregnated and then crushed, so that the phase-change substance fills holes and gaps of the porous material to obtain a composite core, and a shell material is deposited on the surface of the obtained composite core to obtain the phase-change heat storage material.
The invention also provides the application of the phase-change heat storage material in the technical scheme or the phase-change heat storage material prepared by the preparation method in the technical scheme in the fields of solar energy, buildings, constant-temperature drying and electronic device heat management.
For further illustration of the present invention, the following describes in detail a phase change heat storage material with a biomimetic structure, and a preparation method and application thereof with reference to the following embodiments, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Placing 80g paraffin with phase transition temperature of 40 deg.C in 80 deg.C oven until paraffin is completely melted, and adding 5mg paraffin with density of 0.1g/cm3The graphite foam is soaked in melted paraffin for 8 hours under normal pressure, and the graphite foam absorbed with the paraffin is naturally cooled and then crushed to obtain a composite core with the particle size of 10 mu m;
and spraying 30mL of aqueous dispersion of 4mg/mL graphene oxide on the surface of the 5g composite core, placing the obtained product in a vacuum drying oven, and drying for 24 hours at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 10 nm.
Example 2
80g of paraffin with the phase transition temperature of 60 ℃ is placed in a drying oven with the temperature of 100 ℃ until the paraffin is completely melted, and the density of 5mg is 0.1g/cm3The graphite foam is soaked in melted paraffin for 5 hours under the condition that the negative pressure is more than or equal to 0.08KPa, and the graphite foam absorbed with the paraffin is naturally cooled and then crushed to obtain a composite core with the grain diameter of 30 mu m;
and spraying 100mL of aqueous dispersion of 4mg/mL graphene oxide on the surface of the 5g composite core, placing the obtained product in a vacuum drying oven, and drying for 24h at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 35 nm.
Example 3
80g of paraffin with the phase transition temperature of 30 ℃ is placed in a 70 ℃ oven until the paraffin is completely melted, and 10mg of paraffin with the density of 0.2g/cm is added3The graphite foam is soaked in melted paraffin for 5 hours under the condition that the negative pressure is more than or equal to 0.08KPa, and the graphite foam absorbed with the paraffin is naturally cooled and then crushed to obtain a composite core with the grain diameter of 50 mu m;
and spraying 100mL of aqueous dispersion of 4mg/mL graphene oxide on the surface of the 5g composite core, placing the obtained product in a vacuum drying oven, and drying for 24h at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 38 nm.
Example 4
10mg of the powder was mixed at a density of 0.25g/cm3The graphite foam is placed in a cuboid tray, the size of the cuboid tray is 500mm multiplied by 300mm multiplied by 200mm, 80g of paraffin with the phase transition temperature of 40 ℃ is covered on the surface of the graphite foam, the graphite foam covered with the paraffin is placed in an autoclave and vacuumized until the vacuum degree is more than or equal to 0.06KPa, the temperature is kept at 80 ℃ for 3 hours, then the autoclave is pressurized to 0.3MPa, the pressure is maintained for 2 hours, and the graphite foam is taken out and naturally cooled and crushed to obtain a composite core with the particle size of 30 mu m;
and spraying 100mL of aqueous dispersion of 4mg/mL graphene oxide on the surface of the 5g composite core, placing the obtained product in a vacuum drying oven, and drying for 24h at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 45 nm.
Example 5
25mg of the mixture was mixed at a density of 0.5g/cm3The graphite foam is placed in a cuboid tray, the size of the cuboid tray is 500mm multiplied by 300mm multiplied by 200mm, 80g of paraffin with the phase transition temperature of 80 ℃ is covered on the surface of the graphite foam, the graphite foam covered with the paraffin is placed in an autoclave and vacuumized until the vacuum degree is more than or equal to 0.06KPa, the temperature is kept at 120 ℃ for 2 hours, then the autoclave is pressurized to 0.3MPa, the pressure is maintained for 2 hours, and the graphite foam is taken out and naturally cooled and crushed to obtain a composite core with the particle size of 30 mu m;
and spraying 230mL of aqueous dispersion of 4mg/mL graphene oxide on the surface of the 5g composite core, placing the obtained product in a vacuum drying oven, and drying for 24 hours at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 100 nm.
Example 6
80g of paraffin with the phase transition temperature of 30 ℃ is placed in a 70 ℃ oven until the paraffin is completely melted, and the density of 20mg is 0.4g/cm3The graphite foam is soaked in melted paraffin for 5 hours under the condition that the negative pressure is more than or equal to 0.08KPa, and the graphite foam absorbed with the paraffin is naturally cooled and then crushed to obtain a composite core with the grain diameter of 50 mu m;
and spraying 140mL of aqueous dispersion of 4mg/mL graphene oxide on the surface of the 5g composite core, placing the obtained product in a vacuum drying oven, and drying for 24 hours at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 53 nm.
Example 7
15mg of the mixture was mixed at a density of 0.3g/cm3The graphite foam is placed in a cuboid tray, the size of the cuboid tray is 500mm multiplied by 300mm multiplied by 200mm, 80g of paraffin with the phase transition temperature of 50 ℃ is covered on the surface of the graphite foam, the graphite foam covered with the paraffin is placed in an autoclave and vacuumized until the vacuum degree is more than or equal to 0.06KPa, the temperature is kept at 90 ℃ for 2 hours, then the autoclave is pressurized to 0.3MPa, the pressure is maintained for 2 hours, and the graphite foam is taken out and naturally cooled and crushed to obtain a composite core with the particle size of 20 mu m;
and spraying 100mL of graphene oxide aqueous dispersion with the concentration of 2mg/mL on the surface of the composite core obtained by 5g, placing the obtained product in a vacuum drying oven, and drying for 24 hours at the temperature of 35 ℃ and the vacuum degree of less than or equal to 0.06KPa to obtain the phase-change heat storage material with the shell thickness of 41 nm.
The phase change heat storage materials of the biomimetic structures obtained in examples 1-7 were tested as follows:
1. content of phase change material:
calculating according to the formula (1) to obtain the content of the phase change material in the phase change heat storage material with the bionic structure,
in the formula (1), Δ Hm,compositeAnd Δ Hf,compositeRespectively the melting enthalpy value and the crystallization enthalpy value, delta H, of the prepared bionic phase-change particlesm,PAAnd Δ Hf,PARespectively, the melting enthalpy and the crystallization enthalpy of the paraffin, which are obtained by DSC of the test sample.
2. Thermal conductivity:
calculating the heat conductivity of the phase-change heat storage material with the bionic structure according to the formula (2),
k is α · ρ · cp, formula (2)
In the formula (2), K is the sample thermal conductivity and has the unit of W/m.K; alpha is the sample thermal diffusivity in mm2S; ρ is the density of the sample in g/cm3(ii) a cp is the specific heat of the sample, in J/Kg. multidot.K.
The thermal diffusion coefficient of the phase change heat storage material is tested by a German NETZSCH LFA 447/2-2InSb Nano Flash laser thermal conductivity meter; specific heat was tested using a german NETZSCH STA 409PC thermal analysis system.
3. Leakage rate:
calculating the leakage rate (Lr) of the phase change heat storage material with the bionic structure according to the formula (3),
in formula (3), M0For the pre-heating mass of the phase-change heat storage material, MnThe mass of the phase-change heat storage material after being heated for 200 hours at 60 ℃.
The test results obtained are shown in Table 1.
TABLE 1 Performance test results of phase-change heat storage materials of biomimetic structures obtained in examples 1-7
As can be seen from table 1, the content of the heat storage substance in the phase change heat storage material provided by the present invention can be up to 78 wt.%, and the heat storage substance content is high; the thermal conductivity can reach 6.5W/mK, and the thermal conductivity is high; the leakage rate can be as low as 1.8 percent after the heat storage material is placed for 200 hours at the temperature of 60 ℃, and the leakage of the heat storage material can be effectively prevented.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The utility model provides a phase transition heat-retaining material with bionic structure which characterized in that: the composite core comprises a porous material and a phase change substance filled in holes and gaps of the porous material.
2. The phase-change heat storage material with a bionic structure as claimed in claim 1, wherein: the phase change material is paraffin.
3. The phase-change heat storage material with a bionic structure as claimed in claim 1, wherein: the porous material is graphite foam or graphene foam, and the density of the porous material is 0.1-0.5 g/cm3The porosity is 70-95%.
4. The phase-change heat storage material with a bionic structure as claimed in claim 1, wherein: the shell layer is made of graphene oxide.
5. The phase-change heat storage material with a bionic structure as claimed in any one of claims 1 to 4, characterized in that the diameter of the composite core is 20 to 50 μm, and the thickness of the shell layer is 10 to 100 nm.
6. The phase-change heat storage material with a bionic structure as claimed in claim 1, wherein: the content of a phase-change substance in the phase-change heat storage material is 50-80 wt.%, and the mass ratio of the phase-change substance to the porous material is (1-9): 1.
7. The preparation method of the phase-change heat storage material with the bionic structure as claimed in claim 1, characterized by comprising the following steps: firstly, impregnating or vacuum-absorbing a porous material in a liquid phase-change substance, and crushing an obtained product after cooling to obtain a composite core; and then, depositing a shell layer on the surface of the prepared composite core, and drying to obtain the phase-change heat storage material.
8. The method for preparing the phase-change heat storage material with the bionic structure according to claim 7, wherein the method comprises the following steps: the impregnation environmental pressure is more than or equal to 0.08KPa, and the time is 2-8 h;
the vacuum adsorption comprises vacuum heat preservation and pressure maintaining which are sequentially carried out; the vacuum heat preservation environment pressure is more than or equal to 0.06KPa, the temperature is 80-120 ℃, and the heat preservation time is 2-3 h; the pressure maintaining environment is 0.3-0.5 MPa, and the pressure maintaining time is 2-3 h.
9. The method for preparing the phase-change heat storage material with the bionic structure according to claim 7, wherein the method comprises the following steps: the deposition method of the shell layer comprises the following steps: coating the water dispersion of the shell material on the surface of the composite core; the coating method is spraying or fluidized coating; the concentration of the aqueous dispersion of the shell material is 2-4 mg/mL.
10. The phase-change heat storage material as claimed in claim 1 or the phase-change heat storage material prepared by the preparation method as claimed in any one of claims 7 to 9 is applied to the fields of solar energy, buildings, constant temperature drying or electronic device heat management.
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