CN111909662B - Composite phase-change material and preparation method thereof - Google Patents
Composite phase-change material and preparation method thereof Download PDFInfo
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- CN111909662B CN111909662B CN202010886405.5A CN202010886405A CN111909662B CN 111909662 B CN111909662 B CN 111909662B CN 202010886405 A CN202010886405 A CN 202010886405A CN 111909662 B CN111909662 B CN 111909662B
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Abstract
The invention relates to the technical field of phase-change materials, in particular to a composite phase-change material and a preparation method thereof. The invention discloses a composite phase-change material, which takes a phase-change material as an inner core, a transparent high polymer material has good mechanical strength and fabric modulus, and a gel polymer is taken as a shell layer to protect the phase-change material in a limited domain, so that the leakage of the phase-change material can be prevented, the heat exchange area of the phase-change material can be increased, and the phase-change material is convenient to store and transport; the transparent high polymer material has high transmittance, the temperature-sensitive change of the color of cholesteric liquid crystal can be displayed, the change temperature of the color of the liquid crystal is matched with the phase transformation temperature range of the phase-change material, and the visualization of the phase-change material is realized; the one-dimensional heat conduction material has good heat conduction capability, is located in the array nanostructure radially arranged between the shell layer and the core layer, and the nanostructure of the array enables heat to be transmitted along the heat conduction material, so that the heat charging and discharging speed of the phase change material can be well improved, and the heat loss is reduced.
Description
Technical Field
The invention relates to the technical field of phase-change materials, in particular to a composite phase-change material and a preparation method thereof.
Background
The phase change energy storage is an energy storage mode with high research value and wide market research prospect in practical application, and is widely applied to the fields of energy conservation, environmental protection, novel buildings and the like at present. The phase change energy storage material has excellent latent heat capacity, the phase state of the phase change material is changed under different temperature environments, but the temperature of the material cannot be greatly changed. The phase change material changes the phase state including: solid-liquid, solid-gas, solid-solid, liquid-gas. The liquidity of gas state and liquid state is very strong, and the phase-change material is easy to leak in the phase state, which not only affects the phase-change material, but also pollutes the environment by the leaked phase-change material. Thus, this limits its application to some extent.
Disclosure of Invention
The invention provides a composite phase-change material and a preparation method thereof, which solve the problem that gaseous and liquid phase-change materials are easy to leak.
The specific technical scheme is as follows:
the invention provides a composite phase-change material, which is in a core-shell structure;
a shell layer in the core-shell structure is a gel polymer containing cholesteric liquid crystal, a core layer is a phase change material, and a one-dimensional heat conduction material is radially loaded between the shell layer and the core layer;
the gel polymer is made of a transparent high molecular material.
The composite phase-change material provided by the invention takes the phase-change material as the core, the transparent high polymer material has good mechanical strength and weaving modulus, the gel polymer is taken as the shell layer to protect the phase-change material in a limited domain, so that the leakage of the phase-change material can be prevented, and in addition, the heat exchange area of the phase-change material can be increased, so that the phase-change material is convenient to store and transport; the transparent high polymer material has high transmittance, the temperature-sensitive change of the color of cholesteric liquid crystal can be displayed, the change temperature of the color of the liquid crystal is matched with the phase transformation temperature range of the phase-change material, and the visualization of the phase-change material is realized; the one-dimensional heat conduction material has good heat conduction capability, the radial load of the one-dimensional heat conduction material is between the shell layer and the core layer, the array nano structures are arranged in the radial direction, the nano structures in the array can enable heat to be transmitted along the heat conduction material, the heat charging and discharging speed of the phase change material can be well improved, and the heat loss is reduced.
In the invention, the particle size of the core layer is 90-150 μm, the thickness of the shell layer is 10-30 μm, and the thickness of the one-dimensional heat conduction material is 20-30 μm.
In the invention, the phase-change material is a paraffin phase-change material, preferably tetradecane, octadecane or eicosane;
the one-dimensional heat conduction material is selected from copper nanowires, carbon fibers or carbon nanotubes;
the cholesteric liquid crystal comprises nematic liquid crystal and chiral dopant, wherein the nematic liquid crystal is BHR-59001, and the chiral dopant is S-811.
In the invention, the transparent high polymer material is gelatin and/or Arabic gum.
The invention provides a preparation method of the composite phase-change material, which comprises the following steps:
step 1: dispersing a phase change material and hexadecyl trimethyl ammonium bromide in a mixed solvent of water, ammonia water and alcohol by using a Stober method, and adding a silicon source to react to obtain a silicon dioxide coated phase change material;
step 2: immersing the phase-change material coated by the silicon dioxide into the one-dimensional heat conduction material dispersion liquid, stirring and drying to obtain the one-dimensional heat conduction material/silicon dioxide/phase-change material;
and step 3: soaking the one-dimensional heat conduction material/silicon dioxide/phase change material in hydrofluoric acid to obtain the one-dimensional heat conduction material/phase change material;
and 4, step 4: and mixing the transparent high polymer material, the one-dimensional heat conduction material/phase change material, the cholesteric liquid crystal and water, and freeze-drying to obtain the composite phase change material.
The method comprises the following steps that 1, a classical Stober method is adopted, cetyl trimethyl ammonium bromide is used as a mesoporous template, a layer of mesoporous silica is coated on the surface of the phase-change material, and the mesoporous silica confinement coated phase-change material is obtained;
the silicon source is preferably tetraethoxysilane;
the mass ratio of the phase-change material to the silicon source is (30-50): 1, preferably 30: 1;
in the mixed solvent, the alcohol is absolute ethyl alcohol, the water is deionized water, and the dosage ratio of the hexadecyl trimethyl ammonium bromide to the water to the alcohol is 1: (240-280): (50-60).
Step 2 of the invention, loading a one-dimensional heat conducting material in a pore channel of silicon dioxide in the phase change material coated by the silicon dioxide in the step 1;
the mass concentration of the one-dimensional heat conduction material dispersion liquid is 5-15 wt%;
the mass ratio of the one-dimensional heat conduction material to the phase change material is 1-3: 4.
the stirring is preferably magnetic stirring, the rotating speed of the stirring is 800rmp, and the time is 6 hours;
the drying is preferably carried out at 60 ℃ for 24h under vacuum.
Etching the mesoporous silica template by adopting hydrofluoric acid in step 3, and removing the one-dimensional heat conduction material which is not loaded in the mesoporous silica pore channel;
after the soaking, the one-dimensional heat conduction material/silicon dioxide/phase change material is obtained by vacuum drying for 24 hours at 60 ℃.
Step 4, coating a gel polymer containing cholesteric liquid crystal on the surface of a one-dimensional heat conduction material;
the transparent high polymer material, the one-dimensional heat conduction material/phase change material, the cholesteric liquid crystal and the water are mixed specifically as follows: transparent high molecular material, one-dimensional heat conduction material/phase change material, cholesteric liquid crystal and water are stirred into gel texture, and then the gel texture is put into an ultrasonic bath for stirring, so that the gel texture is fully dispersed. When the number of the transparent high polymer materials is more than two, the transparent high polymer materials are added step by step for dispersion.
The dosage ratio of the transparent high polymer material, the one-dimensional heat conduction material/phase change material, the cholesteric liquid crystal and the water is 8 g: (25-35) g: 5 g: 95mL, preferably 8 g: 30g of: 5 g: 95 mL;
the cholesteric liquid crystal comprises nematic liquid crystal and chiral dopants, and the nematic liquid crystal can reflect light with different colors under the illumination condition according to different addition amounts of the chiral dopants. In order to match the phase transition temperature of the phase change material, the addition amount of the chiral dopant is decreased as the phase transition temperature of the phase change material increases.
The mass ratio of the nematic liquid crystal to the chiral dopant is 5: (0.5 to 1.5).
According to the technical scheme, the invention has the following advantages:
the invention provides a composite phase-change material, which is in a core-shell structure; a shell layer in the core-shell structure is a gel polymer containing cholesteric liquid crystal, a core layer is a phase change material, and a one-dimensional heat conduction material is radially loaded between the shell layer and the core layer; the gel polymer is made of a transparent high molecular material.
The composite phase-change material provided by the invention takes the phase-change material as the core, the transparent high polymer material has good mechanical strength and weaving modulus, the gel polymer is taken as the shell layer to protect the phase-change material in a limited domain, so that the leakage of the phase-change material can be prevented, and in addition, the heat exchange area of the phase-change material can be increased, so that the phase-change material is convenient to store and transport; the transparent high polymer material has high transmittance, the temperature-sensitive change of the color of cholesteric liquid crystal can be displayed, the change temperature of the color of the liquid crystal is matched with the phase transformation temperature range of the phase-change material, and the visualization of the phase-change material is realized; the one-dimensional heat conduction material has good heat conduction capability, the radial load of the one-dimensional heat conduction material is between the shell layer and the core layer, the array nano structures are arranged in the radial direction, the nano structures in the array can enable heat to be transmitted along the heat conduction material, the heat charging and discharging speed of the phase change material can be well improved, and the heat loss is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of a composite phase change material according to an embodiment of the present invention;
FIG. 2 is SEM images of composite phase change materials of examples 1-3 and comparative example 1, wherein a-c correspond to the composite phase change materials of examples 1-3, d corresponds to the phase change material @ arrayed carbon nanotube of example 4, and e is an enlarged view of d;
FIG. 3 is a DSC of the composite phase change material in examples 1 to 4 of the present invention, wherein a) to d) correspond to examples 1 to 4 in sequence;
fig. 4 is a "visualization" diagram of the phase change process of the composite phase change material in embodiment 3 of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. 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
1. Preparing a phase-change material (phase-change material @ mesoporous silica) coated by mesoporous silica. Dispersing 20g of tetradecane in a mixed solvent of 100mL of deionized water, 20mL of absolute ethyl alcohol and 1.25g of hexadecyl trimethyl ammonium bromide, heating to 50 ℃, magnetically stirring for 1h, then adding 0.5mL of ammonia water and 0.583g of tetraethoxysilane into the mixture, mechanically stirring for six hours, carrying out suction filtration, extracting the deposit with ammonium nitrate for 3 times, standing at 80 ℃ for 6h to remove the soft template hexadecyl trimethyl ammonium bromide, and finally carrying out vacuum drying at 60 ℃ for 12h to obtain the phase change material @ mesoporous silica.
2. Preparing a phase change material @ mesoporous silica @ array copper nanowire. 5g of copper nanowires were added to a beaker, followed by 100mL of deionized water and magnetic stirring. And (2) immersing the phase change material @ mesoporous silica prepared in the step (1) into the solution in a vacuum environment, magnetically stirring for 2 hours, carrying out suction filtration to separate products after all the copper nanowires are loaded on a silica template, and drying in a vacuum oven at 60 ℃ for 24 hours to obtain the phase change material @ mesoporous silica @ array copper nanowire.
3. And preparing the phase change material @ array copper nanowire. And (3) adding the phase change material @ mesoporous silica @ array copper nanowire prepared in the step (2) into a beaker, adding 10mL of hydrofluoric acid, fully soaking for 2h to etch away the mesoporous silica template, and removing the copper nanowire which is not anchored and embedded in the mesopores. And (4) after the product is subjected to suction filtration and separation, putting the product into a vacuum oven to be dried for 24 hours at the temperature of 60 ℃, and obtaining the phase change material @ array copper nanowire.
4. Preparing a composite phase change material (the phase change material coated by gelatin/Arabic shell glue containing cholesteric liquid crystal @ array copper nanowire). 3g of gelatin, 5g of nematic liquid crystal BHR-59001 and 0.5g of chiral dopant S-811 are added into a beaker, and 50mL of deionized water is added and stirred for 2h to form gel texture. And (2) putting the mixture into an ultrasonic bath, adding 20g of the phase change material @ array copper nanowire aqueous solution prepared in the step (3), stirring for half an hour, slowly adding 50mL of gum arabic solution, continuously performing ultrasonic treatment for two hours, mechanically stirring at room temperature for about twenty hours, adding 150mL of diethyl ether into the prepared product to dissolve the product obtained after stirring, shaking vigorously by hand, centrifuging at 2000rmp for 10min, extracting precipitate, and freeze-drying for 24 hours to obtain the composite phase change material @ array copper nanowire coated by the gelatin/gum arabic shell layer containing cholesteric liquid crystal.
As shown in fig. 2(a), the composite phase change material prepared by the embodiment has a uniform size, a core layer with a thickness of 100 microns, and a smooth shell layer, and has a good protection effect. As shown in FIG. 3(c), the enthalpy of the composite phase change material is 166J g-1The heat release rate is 232J g-1·min-1And 226 J.g-1·min-1Comparison with figure 3(a) pure octadecane (enthalpy 232J g)-1) And FIG. 3(b) a composite phase change material containing no heat conductive material (the heat release rate is 162J g each)-1·min-1And 157J. g-1·min-1) Although the enthalpy value is reduced, the heat charging and discharging rate is obviously improved.
Example 2
1. Preparing a phase-change material (phase-change material @ mesoporous silica) coated by mesoporous silica. Dispersing 20g of octadecane in a mixed solvent of 120mL of deionized water, 25mL of absolute ethyl alcohol and 1.50g of hexadecyl trimethyl ammonium bromide, heating to 50 ℃, magnetically stirring for 1h, then adding 0.5mL of ammonia water and 0.667g of tetraethoxysilane into the mixture, mechanically stirring for six hours, carrying out suction filtration, extracting the deposit with ammonium nitrate for 3 times, standing at 80 ℃ for 6h to remove the soft template hexadecyl trimethyl ammonium bromide, and finally carrying out vacuum drying at 60 ℃ for 12h to obtain the phase change material @ mesoporous silica.
2. Preparing a phase change material @ mesoporous silica @ array copper nanowire. 10g of copper nanowires were added to a beaker, followed by 100mL of deionized water and magnetic stirring. And (2) immersing the phase change material @ mesoporous silica prepared in the step (1) into the solution in a vacuum environment, magnetically stirring for 2 hours, carrying out suction filtration to separate products after all the copper nanowires are loaded on a silica template, and drying in a vacuum oven at 60 ℃ for 24 hours to obtain the phase change material @ mesoporous silica @ array copper nanowire.
3. And preparing the phase change material @ array copper nanowire. And (3) adding the phase change material @ mesoporous silica @ array copper nanowire prepared in the step (2) into a beaker, adding 10mL of hydrofluoric acid, fully soaking for 2h to etch away the mesoporous silica template, and removing the copper nanowire which is not anchored and embedded in the mesopores. And after the product is subjected to suction filtration and separation, putting the product into a vacuum oven to be dried for 24 hours at the temperature of 60 ℃ to obtain the phase change material @ array copper nanowire.
4. Preparing a composite phase change material (the phase change material coated by gelatin/Arabic shell glue containing cholesteric liquid crystal @ array copper nanowire). 3g of gelatin, 5g of nematic liquid crystal BHR-59001 and 1.0g of chiral dopant S-811 are added into a beaker, and 50mL of deionized water is added and stirred for 2h to form gel texture. And (2) putting the mixture into an ultrasonic bath, adding 20g of the phase change material @ array copper nanowire aqueous solution prepared in the step (3), stirring for half an hour, slowly adding 50mL of gum arabic solution, continuously performing ultrasonic treatment for two hours, mechanically stirring at room temperature for about twenty hours, adding 150mL of diethyl ether into the prepared product to dissolve the product obtained after stirring, shaking vigorously by hand, centrifuging at 2000rmp for 10min, extracting precipitate, and freeze-drying for 24 hours to obtain the gelatin/arabic shell layer gum-coated phase change material @ array copper nanowire containing cholesteric liquid crystal.
As shown in fig. 2(b), the composite phase change material prepared by the embodiment has a uniform size, a core layer with a thickness of 120 microns, and a smooth shell layer, and has a good protection effect.
Example 3
1. Preparing a phase-change material (phase-change material @ mesoporous silica) coated by mesoporous silica. Dispersing 20g of eicosane in a mixed solvent of 140mL of deionized water, 30mL of anhydrous ethanol and 1.75g of hexadecyl trimethyl ammonium bromide, heating to 50 ℃, magnetically stirring for 1h, then adding 0.5mL of ammonia water and 0.748g of tetraethoxysilane into the mixture, mechanically stirring for six hours, carrying out suction filtration, extracting the deposit with ammonium nitrate for 3 times, standing at 80 ℃ for 6h to remove the soft template hexadecyl trimethyl ammonium bromide, and finally carrying out vacuum drying at 60 ℃ for 12h to obtain the phase change material @ mesoporous silica.
2. Preparing a phase change material @ mesoporous silica @ array copper nanowire. 15g of copper nanowires were added to a beaker, followed by 100mL of deionized water and magnetic stirring. And (2) immersing the phase change material @ mesoporous silica prepared in the step (1) into the solution in a vacuum environment, magnetically stirring for 2 hours, carrying out suction filtration to separate products after all the copper nanowires are loaded on a silica template, and drying in a vacuum oven at 60 ℃ for 24 hours to obtain the phase change material @ mesoporous silica @ array copper nanowire.
3. And preparing the phase change material @ array copper nanowire. And (3) adding the phase change material @ mesoporous silica @ array copper nanowire prepared in the step (2) into a beaker, adding 10mL of hydrofluoric acid, fully soaking for 2h to etch the mesoporous silica template, and removing the copper nanowire which is not anchored and embedded in the mesopores. And after the product is subjected to suction filtration and separation, putting the product into a vacuum oven to be dried for 24 hours at the temperature of 60 ℃ to obtain the phase change material @ array copper nanowire.
4. Preparing a composite phase change material (the phase change material coated by gelatin/Arabic shell glue containing cholesteric liquid crystal @ array copper nanowire). 3g of gelatin, 5g of nematic liquid crystal BHR-59001 and 1.5g of chiral dopant S-811 are added into a beaker, and 50mL of deionized water is added and stirred for 2h to form gel texture. And (2) putting the mixture into an ultrasonic bath, adding 20g of the phase change material @ array copper nanowire aqueous solution prepared in the step (3), stirring for half an hour, slowly adding 50mL of gum arabic solution, continuously performing ultrasonic treatment for two hours, mechanically stirring at room temperature for about twenty hours, adding 150mL of diethyl ether into the prepared product to dissolve the product obtained after stirring, shaking vigorously by hand, centrifuging at 2000rmp for 10min, extracting precipitate, and freeze-drying for 24 hours to obtain the gelatin/arabic shell layer gum-coated phase change material @ array copper nanowire containing cholesteric liquid crystal.
As shown in fig. 2(c), the composite phase change material prepared by the embodiment has a uniform size, a core layer with a thickness of 110 microns, and a smooth shell layer, and has a good protection effect. As shown in FIG. 4, when the composite phase-change material is not subjected to phase change at a temperature lower than 30 ℃, blue light is reflected, when the composite phase-change material absorbs heat and is heated, phase transition occurs, and when the temperature is higher than 30 ℃, the light is not reflected, and the process has reversibility, so that the visualization of the phase-change process is realized.
Example 4
1. Preparing a phase-change material (phase-change material @ mesoporous silica) coated by mesoporous silica. Dispersing 20g of octadecane in a mixed solvent of 120mL of deionized water, 25mL of absolute ethyl alcohol and 1.50g of hexadecyl trimethyl ammonium bromide, heating to 50 ℃, magnetically stirring for 1h, then adding 0.5mL of ammonia water and 0.667g of tetraethoxysilane into the mixture, mechanically stirring for six hours, carrying out suction filtration, extracting the deposit with ammonium nitrate for 3 times, standing at 80 ℃ for 6h to remove the soft template hexadecyl trimethyl ammonium bromide, and finally carrying out vacuum drying at 60 ℃ for 12h to obtain the phase change material @ mesoporous silica.
2. Preparing a phase change material @ mesoporous silica @ array carbon nanotube. Adding 10g of carbon nano tubes into a beaker, then adding 100mL of deionized water, magnetically stirring for 30min, and continuing to perform ultrasonic treatment for 30min to further disperse the carbon nano tubes. And (2) immersing the phase change material @ mesoporous silica prepared in the step (1) into the solution in a vacuum environment, magnetically stirring for 2 hours, carrying out suction filtration on a separated product after all the carbon nanotubes are loaded on a silica template, and drying in a vacuum oven at 60 ℃ for 24 hours to obtain the phase change material @ mesoporous silica @ array carbon nanotubes.
3. And preparing the phase-change material @ array carbon nanotube. And (3) adding the phase change material @ mesoporous silica @ array carbon nano tube prepared in the step (2) into a beaker, adding 10mL of hydrofluoric acid, fully soaking for 2h to etch away the mesoporous silica template, and removing the carbon nano tube which is not anchored and embedded in the mesopores. And after the product is subjected to suction filtration and separation, putting the product into a vacuum oven to be dried for 24 hours at the temperature of 60 ℃ to obtain the phase change material @ array carbon nanotube.
4. Preparing a composite phase-change material (the phase-change material coated by gelatin/Arabic shell glue containing cholesteric liquid crystal @ array carbon nano tubes). 3g of gelatin, 5g of nematic liquid crystal BHR-59001 and 1.0g of chiral dopant S-811 are added into a beaker, and 50mL of deionized water is added and stirred for 2h to form gel texture. And (2) putting the mixture into an ultrasonic bath, adding 20g of the phase change material @ array carbon nanotube aqueous solution prepared in the step (3), stirring for half an hour, slowly adding 50mL of gum arabic solution, continuously performing ultrasonic treatment for two hours, mechanically stirring at room temperature for about twenty hours, adding 150mL of diethyl ether into the prepared product to dissolve the product obtained after stirring, shaking vigorously by hand, centrifuging at 2000rmp for 10min, extracting precipitate, and freeze-drying for 24 hours to obtain the gelatin/arabic shell glue coated phase change material @ array carbon nanotube containing cholesteric liquid crystal.
As shown in fig. 2(d) and 2(e), the phase change material @ array carbon nanotube prepared in step 3 of this embodiment has a plurality of array carbon nanotubes loaded therein. As shown in FIG. 3(d), the enthalpy of the composite phase change material is 175J g-1The respective charge and discharge rates were 253 J.g-1·min-1And 238 J.g-1·min-1Comparison with figure 3(a) pure octadecane (enthalpy 232J g)-1) And FIG. 3(b) a composite phase change material containing no heat conductive material (the heat release rate is 162J g each)-1·min-1And 157J. g-1·min-1) Although the enthalpy value is reduced, the heat charging and discharging rate is obviously improved.
Example 5
1. Preparing a phase-change material (phase-change material @ mesoporous silica) coated by mesoporous silica. Dispersing 20g of octadecane in a mixed solvent of 120mL of deionized water, 25mL of absolute ethyl alcohol and 1.50g of hexadecyl trimethyl ammonium bromide, heating to 50 ℃, magnetically stirring for 1h, then adding 0.5mL of ammonia water and 0.667g of tetraethoxysilane into the mixture, mechanically stirring for six hours, carrying out suction filtration, extracting the deposit with ammonium nitrate for 3 times, standing at 80 ℃ for 6h to remove the soft template hexadecyl trimethyl ammonium bromide, and finally carrying out vacuum drying at 60 ℃ for 12h to obtain the phase change material @ mesoporous silica.
2. Preparing a phase change material @ mesoporous silica @ array carbon fiber. 10g of carbon fibers are added into a beaker, then 100mL of deionized water is added, and the magnetic stirring is carried out for 30min, and then the ultrasonic treatment is continued for 30min, so that the carbon fibers are further dispersed. And (2) immersing the phase change material @ mesoporous silica prepared in the step (1) into the solution in a vacuum environment, magnetically stirring for 2 hours, filtering and separating a product after all carbon fibers are loaded on a silica template, and drying in a vacuum oven at 60 ℃ for 24 hours to obtain the phase change material @ mesoporous silica @ array copper carbon fibers.
3. Preparing the phase change material @ array carbon fiber. And (3) adding the phase change material @ mesoporous silica @ array carbon fiber prepared in the step (2) into a beaker, adding 10mL of hydrofluoric acid, fully soaking for 2 hours to etch away the mesoporous silica template, and removing the carbon fiber which is not anchored and embedded in the mesopores. And (3) after the product is subjected to suction filtration and separation, putting the product into a vacuum oven, and drying the product for 24 hours at the temperature of 60 ℃ to obtain the phase change material @ array carbon fiber.
4. Preparing a composite phase change material (the phase change material coated by gelatin/Arabic shell glue containing cholesteric liquid crystal @ array carbon fiber). 3g of gelatin, 5g of nematic liquid crystal BHR-59001 and 1.0g of chiral dopant S-811 are added into a beaker, and 50mL of deionized water is added and stirred for 2h to form gel texture. And (2) putting the mixture into an ultrasonic bath, adding 20g of the phase change material @ array carbon fiber aqueous solution prepared in the step (3), slowly adding 50mL of gum arabic solution after stirring for half an hour, continuing ultrasonic treatment for two hours, then mechanically stirring for about twenty hours at room temperature, adding 150mL of diethyl ether into the prepared product to dissolve the product obtained after stirring, shaking vigorously by hand, centrifuging at 2000rmp for 10min, extracting precipitate, and freeze-drying for 24 hours to obtain the phase change material @ array carbon fiber coated by gelatin/Arabic shell layer gum containing cholesteric liquid crystal.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The composite phase change material is characterized in that the composite phase change material is of a core-shell structure;
a shell layer in the core-shell structure is a gel polymer containing cholesteric liquid crystal, a core layer is a phase change material, and a one-dimensional heat conduction material is radially loaded between the shell layer and the core layer;
the gel polymer is made of a transparent high molecular material.
2. The composite phase change material as claimed in claim 1, wherein the core layer has a particle size of 90-150 μm, the shell layer has a thickness of 10-30 μm, and the one-dimensional heat conductive material has a thickness of 20-30 μm.
3. The composite phase change material of claim 1, wherein the phase change material is a paraffin-type phase change material;
the one-dimensional heat conduction material is selected from copper nanowires, carbon fibers or carbon nanotubes;
the cholesteric liquid crystal includes a nematic liquid crystal and a chiral dopant.
4. The composite phase-change material of claim 3, wherein the nematic liquid crystal is BHR-59001 and the chiral dopant is S-811.
5. The composite phase change material of claim 3, wherein the paraffin-type phase change material is tetradecane, octadecane, or eicosane.
6. The composite phase change material of claim 5, wherein the transparent polymer material is gelatin and/or gum arabic.
7. The method for preparing the composite phase change material according to any one of claims 1 to 6, comprising the steps of:
step 1: adding a silicon source into a phase-change material and hexadecyl trimethyl ammonium bromide in a mixed solvent of water and alcohol by using a Stober method to react to obtain a silicon dioxide coated phase-change material;
step 2: immersing the phase-change material coated by the silicon dioxide into the one-dimensional heat conduction material dispersion liquid, stirring and drying to obtain the one-dimensional heat conduction material/silicon dioxide/phase-change material;
and step 3: soaking the one-dimensional heat conduction material/silicon dioxide/phase change material in hydrofluoric acid to obtain the one-dimensional heat conduction material/phase change material;
and 4, step 4: and mixing the transparent high polymer material, the one-dimensional heat conduction material/phase change material, the cholesteric liquid crystal and water, and freeze-drying to obtain the composite phase change material.
8. The preparation method according to claim 7, wherein the mass ratio of the phase-change material to the silicon source is (30-50): 1;
the mass ratio of the one-dimensional heat conduction material to the phase change material is 1-3: 4.
9. the preparation method according to claim 7, wherein the ratio of the transparent polymer material, the one-dimensional heat conductive material/phase change material, the cholesteric liquid crystal and the water is 8 g: (25-35) g: 5 g: 95 mL.
10. The method according to claim 7, wherein the cholesteric liquid crystal comprises a nematic liquid crystal and a chiral dopant;
the mass ratio of the nematic liquid crystal to the chiral dopant is 5: (0.5 to 1.5).
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4131158A (en) * | 1976-01-23 | 1978-12-26 | Institut Fur Kerntechnik Und Energiewandlung E.V. | Storage arrangement for thermal energy |
| CN101343529A (en) * | 2007-07-13 | 2009-01-14 | 中国科学院大连化学物理研究所 | Method for preparing composite phase-changing material |
| CN101768427A (en) * | 2009-01-07 | 2010-07-07 | 清华大学 | Thermal interface material and preparation method thereof |
| CN102388018A (en) * | 2009-04-10 | 2012-03-21 | 应用纳米结构方案公司 | Fiber sizing comprising nanoparticles |
| CN103571062A (en) * | 2012-07-25 | 2014-02-12 | 哈金森公司 | Rubber composition based on at least one EPDM and a phase-change material, pipe incorporating same and process for preparing this composition |
| CN109321212A (en) * | 2018-10-28 | 2019-02-12 | 西南电子技术研究所（中国电子科技集团公司第十研究所） | The preparation method of the compound PCM combined phasetransform temperature control component of nanotube |
| CN111234502A (en) * | 2020-03-31 | 2020-06-05 | 南京理工大学 | Efficient and uniform heat conduction polymer-based heat conduction material and preparation method thereof |
-
2020
- 2020-08-28 CN CN202010886405.5A patent/CN111909662B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4131158A (en) * | 1976-01-23 | 1978-12-26 | Institut Fur Kerntechnik Und Energiewandlung E.V. | Storage arrangement for thermal energy |
| CN101343529A (en) * | 2007-07-13 | 2009-01-14 | 中国科学院大连化学物理研究所 | Method for preparing composite phase-changing material |
| CN101768427A (en) * | 2009-01-07 | 2010-07-07 | 清华大学 | Thermal interface material and preparation method thereof |
| CN102388018A (en) * | 2009-04-10 | 2012-03-21 | 应用纳米结构方案公司 | Fiber sizing comprising nanoparticles |
| CN103571062A (en) * | 2012-07-25 | 2014-02-12 | 哈金森公司 | Rubber composition based on at least one EPDM and a phase-change material, pipe incorporating same and process for preparing this composition |
| CN109321212A (en) * | 2018-10-28 | 2019-02-12 | 西南电子技术研究所（中国电子科技集团公司第十研究所） | The preparation method of the compound PCM combined phasetransform temperature control component of nanotube |
| CN111234502A (en) * | 2020-03-31 | 2020-06-05 | 南京理工大学 | Efficient and uniform heat conduction polymer-based heat conduction material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 可逆热致变色相变微胶囊的制备与性能研究;石李明;《中国优秀硕士学位论文全文数据库（电子期刊）工程科技I辑》;20140415(第04期);第B020-69页 * |
| 胆甾相液晶的应用;赵静等;《品牌》;20140630;第119页 * |
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