CN109266314B - Flexible composite phase change material and preparation method thereof - Google Patents
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Abstract
The invention provides a preparation method of a flexible composite phase-change material, and belongs to the field of phase-change heat storage materials. According to the invention, ice crystals formed by water in a freeze drying process are used as a template to prepare the carbon nanotube-based aerogel carrier with a loose and porous three-dimensional network structure, so that a flexible structure is obtained, more phase change core materials can be loaded due to strong hydrogen bond action among polyvinyl alcohol, chitosan and the phase change core materials, the loading capacity of the phase change core materials is increased, the energy storage density of the material is improved, the flexibility of the material can still be maintained due to the matching property between the phase change core materials and the pore channels of the carbon nanotube-based material, and the thermal conductivity of the material is better due to the high thermal conductivity of the carbon nanotube.
Description
Technical Field
The invention belongs to the technical field of phase change heat storage materials, and particularly relates to a flexible composite phase change material and a preparation method thereof.
Background
With the development of electronic technology, the heat dissipation power and the heat dissipation density of an electronic chip are increasingly improved, and the requirement on the thermal control of the electronic chip is also increasingly higher. Phase change energy storage thermal control has become one of the most important passive thermal control means of electronic devices due to the advantages of high energy storage density, small temperature fluctuation, simple system, convenient operation and the like. However, the problems of difficult installation, easy leakage and the like caused by solid-liquid change in the phase change process of the solid-liquid phase change materials commonly adopted at present become key factors for restricting the phase change thermal control. Although researchers have proposed solutions to the above problems with shaped phase change materials, there are still many key problems that are not solved, mainly: the low energy storage density and the lack of flexibility make the installation of the phase change thermal control component on the thermal control surface with a complex shape difficult.
Disclosure of Invention
In view of this, the present invention aims to provide a flexible composite phase change material, and a preparation method and an application thereof. The flexible composite phase change material prepared by the invention has super-good flexibility and high energy storage density.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a flexible composite phase change material, which comprises the following steps:
providing a chitosan acetic acid solution;
providing an aqueous polyvinyl alcohol solution;
mixing carbon nanotubes with water to obtain a carbon nanotube suspension;
adding the carbon nano tube suspension into a chitosan acetic acid solution to obtain a mixed solution;
mixing the mixed solution with a polyvinyl alcohol aqueous solution to obtain a precursor solution;
freeze-drying the precursor solution to obtain a carbon nanotube-based aerogel carrier;
and (3) dipping the carbon nanotube-based aerogel carrier by using a phase-change core material solution to obtain the flexible composite phase-change material, wherein the phase-change core material solution is a polyethylene glycol solution, an octadecanol solution or an octadecylamine solution.
Preferably, the mass ratio of the carbon nanotubes in the carbon nanotube suspension to the chitosan in the chitosan acetic acid solution is 1: 1-1: 10.
Preferably, the concentration of the carbon nanotube suspension is 4-35 mg/mL, and the mass fraction of the chitosan acetic acid solution is 1-5%.
Preferably, the mass ratio of the carbon nanotubes in the carbon nanotube suspension to the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 1: 1-1: 20.
Preferably, the mass fraction of the polyvinyl alcohol aqueous solution is 2-25%.
Preferably, the mass ratio of the phase-change core material to the carbon nanotube-based aerogel carrier in the phase-change core material solution is 0.5: 9.5-5: 5.
Preferably, the molecular weight of the polyethylene glycol is 2000-20000.
Preferably, the temperature of the freeze drying is-20 to-196 ℃, the time is 2 to 12 hours, and the pressure is 25 to 95 mT.
The invention also provides the flexible composite phase-change material prepared by the preparation method in the technical scheme, wherein the flexible composite phase-change material comprises a phase-change core material and a carbon nanotube-based aerogel carrier, and the phase-change core material is loaded in the three-dimensional holes of the carbon nanotube-based aerogel carrier.
Preferably, the loading capacity of the phase change core material is 50-95%.
The invention provides a preparation method of a flexible composite phase change material, which comprises the following steps: providing a chitosan acetic acid solution; providing an aqueous polyvinyl alcohol solution; mixing carbon nanotubes with water to obtain a carbon nanotube suspension; adding the carbon nano tube suspension into a chitosan acetic acid solution to obtain a mixed solution; mixing the mixed solution with a polyvinyl alcohol aqueous solution to obtain a precursor solution; freeze-drying the precursor solution to obtain a carbon nanotube-based aerogel carrier; and (3) dipping the carbon nanotube-based aerogel carrier by using a phase-change core material solution to obtain the flexible composite phase-change material, wherein the phase-change core material solution is a polyethylene glycol solution, an octadecanol solution or an octadecylamine solution. According to the invention, ice crystals formed by water in a freeze drying process are used as a template to prepare a loose and porous carbon nanotube-based aerogel carrier with a three-dimensional network structure, so that a flexible structure is obtained, and strong hydrogen bond action among polyvinyl alcohol, chitosan and a phase change core material enables the phase change core material to enter a pore channel of the three-dimensional network structure and is bound in the pore channel to prevent leakage; controlling the size of the pore diameter by utilizing freeze drying; the thickness and flexibility of the composite phase-change material are controlled by the carbon nano tube suspension, more phase-change core materials can be loaded, the loading capacity of the phase-change core materials is increased, the energy storage density of the material is improved, the flexibility of the material can be still maintained by utilizing the matching property between the phase-change core materials and the pore channels of the carbon nano tube base material, and the thermal conductivity of the material is better by utilizing the high thermal conductivity of the carbon nano tube. The preparation method provided by the invention has the advantages of low cost, simple and convenient operation and the like. The data of the embodiment shows that the maximum compression amount of the flexible composite phase change material prepared by the invention can reach 99% and can be restored to the original 99% through a compression resilience test; through flexibility test, the composite phase change material is respectively bent, folded and twisted, and can completely recover the original shape under the action of external force; the carbon nanotube-based carrier material obtained by a nitrogen adsorption and desorption curve through a BET test is a hierarchical pore, has more micron pore ratio, is very beneficial to packaging of a phase-change material, and has phase-change enthalpy up to 149J/g.
Drawings
Fig. 1 is an SEM image of the carbon nanotube-based aerogel support of example 1;
FIG. 2 is an SEM image of a flexible composite phase change material of example 1;
FIG. 3 is a DSC graph of the flexible composite phase change material of example 1;
FIG. 4 is a photograph of a flexible composite phase change material of example 1 showing a bending property test;
FIG. 5 is an SEM image of a flexible composite phase change material of example 3;
FIG. 6 is an SEM image of a flexible composite phase change material of example 4;
FIG. 7 is a DSC graph of the flexible composite phase change material of example 5;
FIG. 8 is a DSC graph of the flexible composite phase change material of example 6.
Detailed Description
The invention provides a preparation method of a flexible composite phase change material, which comprises the following steps:
providing a chitosan acetic acid solution;
providing an aqueous polyvinyl alcohol solution;
mixing carbon nanotubes with water to obtain a carbon nanotube suspension;
adding the carbon nano tube suspension into a chitosan acetic acid solution to obtain a mixed solution;
mixing the mixed solution with a polyvinyl alcohol aqueous solution to obtain a precursor solution;
freeze-drying the precursor solution to obtain a carbon nanotube-based aerogel carrier;
and (3) dipping the carbon nanotube-based aerogel carrier by using a phase-change core material solution to obtain the flexible composite phase-change material, wherein the phase-change core material solution is a polyethylene glycol solution, an octadecanol solution or an octadecylamine solution.
The invention provides a chitosan acetic acid solution. In the invention, the mass fraction of the chitosan acetic acid solution is preferably 1-5%, and more preferably 2-4%. The invention preferably adds chitosan into acetic acid to prepare the chitosan acetic acid solution. In the invention, the molar concentration of the acetic acid is preferably 1-5 mol/L. In the invention, the chitosan has good solubility and good flexibility.
In the invention, the preparation of the chitosan acetic acid solution is preferably carried out under the condition of ultrasonic stirring, the time of ultrasonic stirring treatment is preferably 60min, and the speed of ultrasonic stirring is preferably 600 r/min.
The present invention provides an aqueous polyvinyl alcohol solution. In the invention, the mass fraction of the polyvinyl alcohol aqueous solution is preferably 2-25%, and more preferably 15%. In the present invention, the preparation of the aqueous polyvinyl alcohol solution is preferably carried out under stirring conditions, the stirring treatment is preferably carried out for 60min, and the stirring speed is preferably 600 r/min.
The invention mixes the carbon nano tube with water to obtain the carbon nano tube suspension. In the invention, the mixing is preferably carried out under ultrasonic conditions, the ultrasonic treatment time is preferably 60min, and the ultrasonic power is preferably 500-1000W.
In the invention, the concentration of the carbon nanotube suspension is preferably 4-35 mg/mL, and more preferably 5-10 mg/mL. In the invention, the carbon nano tube has the best dispersibility in the chitosan, the agglomeration phenomenon of the carbon nano tube is reduced to the greatest extent, and the flexibility and the high thermal conductivity of the carbon nano tube can be fully exerted. The source of the carbon nanotubes in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used.
The carbon nano tube suspension is added into a chitosan-acetic acid solution to obtain a mixed solution. In the invention, the mass ratio of the carbon nanotubes in the carbon nanotube suspension to the chitosan in the chitosan acetic acid solution is preferably 1: 1-1: 10, and more preferably 1: 3-1: 7.
In the present invention, the carbon nanotube suspension is preferably subjected to ultrasonic treatment after being added to the chitosan acetic acid solution. The parameters of the ultrasonic treatment are not specially limited, and the carbon nano tube suspension and the chitosan acetic acid solution can be uniformly mixed.
After the mixed solution is obtained, the mixed solution is mixed with a polyvinyl alcohol aqueous solution to obtain a precursor solution. In the invention, the mass ratio of the carbon nanotubes in the carbon nanotube suspension to the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is preferably 1: 1-1: 20, and more preferably 1: 5-1: 15. In the present invention, the polyvinyl alcohol aqueous solution can bind the carbon nanotube.
After the mixing is completed, the invention preferably carries out ultrasonic crushing on the obtained mixed system to obtain a precursor solution. In the invention, the time of ultrasonic crushing is preferably 45-60 min, and the power of ultrasonic crushing is preferably 500-1000W.
After the precursor solution is obtained, the precursor solution is subjected to freeze drying to obtain the carbon nanotube-based aerogel carrier. In the present invention, the temperature of the freeze-drying is preferably-20 to-196 ℃, more preferably-60 to-196 ℃; the freeze drying time is preferably 2-12 hours, and more preferably 2-10 hours; the pressure of freeze drying is preferably 25-95 mT, and more preferably 36 mT. According to the invention, ice crystals formed by water in a freeze drying process are used as a template to prepare the loose and porous carbon nanotube-based aerogel carrier with the three-dimensional network structure, so that the flexible structure is obtained.
After the carbon nanotube-based aerogel carrier is obtained, the carbon nanotube-based aerogel carrier is soaked by a phase-change core material solution to obtain the flexible composite phase-change material, wherein the phase-change core material solution is a polyethylene glycol solution, an octadecanol solution or an octadecylamine solution. In the invention, the mass ratio of the phase-change core material to the carbon nanotube-based aerogel carrier in the phase-change core material solution is preferably 0.5: 9.5-5: 5.
The solvent of the phase-change core material solution is not specially limited, and polyethylene glycol, octadecanol and octadecylamine can be completely dissolved.
In the invention, the molecular weight of the polyethylene glycol is preferably 2000-20000.
The invention also provides the flexible composite phase-change material prepared by the preparation method in the technical scheme, wherein the flexible composite phase-change material comprises a phase-change core material and a carbon nanotube-based aerogel carrier, and the phase-change core material is loaded in the three-dimensional holes of the carbon nanotube-based aerogel carrier.
In the invention, the loading capacity of the phase change core material is preferably 50-95%.
The following will describe the flexible composite phase change material and the preparation method thereof in detail with reference to the examples, but they should not be construed as limiting the scope of the invention.
Example 1
(1) Putting chitosan into acetic acid solution with the molar concentration of 5mol/L, and carrying out ultrasonic stirring treatment for 60min at the stirring speed of 600r/min to obtain uniform chitosan solution with the mass fraction of 1%;
(2) adding 20mL of 5mg/mL carbon nanotube suspension liquid subjected to ultrasonic treatment for 60min into 100mL of the chitosan solution, and performing ultrasonic stirring for 60min to obtain a mixed solution for later use;
(3) adding 10mL of prepared polyvinyl alcohol aqueous solution with the mass fraction of 15% into the mixed solution, and performing ultrasonic crushing to prepare precursor solution;
(4) putting the precursor solution into liquid nitrogen for freezing at the temperature of-196 ℃ for 2h under the freeze-drying pressure of 36 mT; after completely freezing, putting the mixture into a freeze dryer for drying to prepare a carbon nanotube-based aerogel carrier with a loose porous structure;
(5) dissolving polyethylene glycol-2000 (PEG), and preparing the final flexible composite phase change material by using an impregnation method, wherein the mass ratio of the polyethylene glycol to the carbon nanotube-based aerogel carrier material is 95: 5.
SEM tests were performed on the carbon nanotube-based aerogel support, as shown in fig. 1. As can be seen from fig. 1, the prepared carbon nanotube-based aerogel carrier has an oriented layered structure, and carbon nanotubes are connected into a three-dimensional network structure by using an end-to-end mechanism, so that the porosity is high.
SEM testing was performed on the flexible composite phase change material as shown in fig. 2. As can be seen from fig. 2, after the phase-change core material is loaded, the surface of the composite phase-change material becomes smooth, which indicates that the phase-change core material successfully enters the pore channel.
Fig. 3 is a DSC graph of a flexible composite phase change material, where the enthalpy of phase change is an important parameter of the heat storage performance of the phase change material, and is directly related to the heat storage density of the phase change material. As can be seen from FIG. 3, the mass fraction of PEG of 95% has a very high loading amount, the enthalpy of phase change is 149J/g, and the enthalpy of phase change of pure PEG is 156J/g, which is obtained by integral calculation of the heat absorption and release peaks in the DSC curve, and is consistent with the result.
The flexible composite phase change material of example 1 was subjected to a bending property test, and the results are shown in fig. 4, and it can be seen from fig. 4 that the prepared flexible composite phase change material has good flexibility and excellent mechanical properties.
Example 2
The same as example 1, except that: the carbon nanotube concentration was varied to 10 mg/mL.
(1) Putting chitosan into acetic acid solution with the molar concentration of 10mol/L, and carrying out ultrasonic stirring treatment for 60min at the stirring speed of 600r/min to obtain uniform chitosan solution with the mass fraction of 1%;
(2) adding 20mL of 10mg/mL carbon nanotube suspension liquid subjected to ultrasonic treatment for 60min into 100mL of the chitosan solution, and performing ultrasonic stirring for 60min to obtain a mixed solution for later use;
(3) adding 10mL of prepared polyvinyl alcohol aqueous solution with the mass fraction of 15% into the mixed solution, and performing ultrasonic crushing to prepare precursor solution;
(4) putting the precursor solution into liquid nitrogen for freezing at the temperature of-196 ℃ for 2h under the freeze-drying pressure of 36 mT; after completely freezing, putting the mixture into a freeze dryer for drying to prepare a carbon nanotube-based aerogel carrier with a loose porous structure;
(5) dissolving polyethylene glycol-2000 (PEG), and preparing the final flexible composite phase change material by using an impregnation method, wherein the mass ratio of the polyethylene glycol to the carbon nanotube-based aerogel carrier material is 95: 5.
Example 3
The same as example 1, except that: the freezing temperature was changed to-60 ℃.
(1) Putting chitosan into acetic acid solution with the molar concentration of 5mol/L, and carrying out ultrasonic stirring treatment for 60min at the stirring speed of 600r/min to obtain uniform chitosan solution with the mass fraction of 1%;
(2) adding 20mL of 5mg/mL carbon nanotube suspension liquid subjected to ultrasonic treatment for 60min into 100mL of the chitosan solution, and performing ultrasonic stirring for 60min to obtain a mixed solution for later use;
(3) adding 10mL of prepared polyvinyl alcohol aqueous solution with the mass fraction of 15% into the mixed solution, and performing ultrasonic crushing to prepare precursor solution;
(4) putting the precursor solution into liquid nitrogen for freezing at-60 ℃ for 10h under the pressure of 36 mT; after completely freezing, putting the mixture into a freeze dryer for drying to prepare a carbon nanotube-based aerogel carrier with a loose porous structure;
(5) dissolving polyethylene glycol-2000 (PEG), and preparing the final flexible composite phase change material by using an impregnation method, wherein the mass ratio of the polyethylene glycol to the carbon nanotube-based aerogel carrier material is 95: 5.
Example 4
The same as example 1, except that: the freezing temperature was changed to-20 ℃. The other steps were the same as in example 1.
Examples 3 to 4 study the influence of the freezing temperature on the pore size, fig. 5 is an SEM spectrogram of the composite phase change material prepared in example 3, and fig. 6 is an SEM spectrogram of the composite phase change material prepared in example 4, and it can be seen by comparing scanning electron micrographs (fig. 2, 5, and 6) that the pore size becomes smaller and smaller with the decrease of the freezing temperature, and it is found that the pore size is too large at the freezing temperature of-20 ℃, which is not favorable for the loading of the phase change material.
Example 5
The same as example 1, except that: the phase change core material was changed to octadecylamine.
(1) Putting chitosan into acetic acid solution with the molar concentration of 5mol/L, and carrying out ultrasonic stirring treatment for 60min at the stirring speed of 600r/min to obtain uniform chitosan solution with the mass fraction of 1%;
(2) adding 20mL of 5mg/mL carbon nanotube suspension liquid subjected to ultrasonic treatment for 60min into 100mL of the chitosan solution, and performing ultrasonic stirring for 60min to obtain a mixed solution for later use;
(3) adding 10mL of prepared polyvinyl alcohol aqueous solution with the mass fraction of 15% into the mixed solution, and performing ultrasonic crushing to prepare precursor solution;
(4) putting the precursor solution into liquid nitrogen for freezing at the temperature of-196 ℃ for 2h under the freeze-drying pressure of 36 mT; after completely freezing, putting the mixture into a freeze dryer for drying to prepare a carbon nanotube-based aerogel carrier with a loose porous structure;
(5) dissolving octadecylamine, and preparing the final flexible composite phase change material by using an immersion method, wherein the mass ratio of polyethylene glycol to the carbon nanotube-based aerogel carrier material is 95: 5.
Example 5 studies the effect of loading different phase-change core materials on the phase-change enthalpy, and it is found by DSC test (fig. 7) that the phase-change enthalpy after loading octadecylamine is reduced relative to polyethylene glycol having a molecular weight of 2000, and it is studied that the size of polyethylene glycol having a molecular weight of 2000 is more matched with the pore size of the carrier material.
Example 6
The same as example 1, except that: the phase change core material was changed to octadecanol. The other steps were the same as in example 1.
Example 6 is to study the effect of phase change core materials loaded differently on phase change enthalpy, and DSC test shows (fig. 8) that the phase change enthalpy after loading octadecanol is increased compared with that of octadecylamine, and the hydrogen bonding effect of octadecanol and the carrier material is stronger.
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 (7)
1. The preparation method of the flexible composite phase-change material is characterized by comprising the following steps of:
providing a chitosan acetic acid solution;
providing an aqueous polyvinyl alcohol solution;
mixing carbon nanotubes with water to obtain a carbon nanotube suspension;
adding the carbon nano tube suspension into a chitosan acetic acid solution to obtain a mixed solution; the mass ratio of the carbon nanotubes in the carbon nanotube suspension to the chitosan in the chitosan acetic acid solution is 1: 1-1: 10;
mixing the mixed solution with a polyvinyl alcohol aqueous solution to obtain a precursor solution; the mass ratio of the carbon nanotubes in the carbon nanotube suspension to the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 1: 1-1: 20;
freeze-drying the precursor solution to obtain a carbon nanotube-based aerogel carrier;
dipping the carbon nanotube-based aerogel carrier by using a phase-change core material solution to obtain a flexible composite phase-change material, wherein the phase-change core material solution is a polyethylene glycol solution, an octadecanol solution or an octadecylamine solution; the mass ratio of the phase-change material in the phase-change core material solution to the carbon nanotube-based aerogel carrier is 0.5: 9.5-5: 5.
2. The preparation method of claim 1, wherein the concentration of the carbon nanotube suspension is 4-35 mg/mL, and the mass fraction of the chitosan acetic acid solution is 1-5%.
3. The method according to claim 1, wherein the polyvinyl alcohol aqueous solution is present in an amount of 2 to 25% by mass.
4. The method according to claim 1, wherein the polyethylene glycol has a molecular weight of 2000 to 20000.
5. The method according to claim 1, wherein the freeze-drying temperature is-20 to-196 ℃, the time is 2 to 12 hours, and the pressure is 25 to 95 mT.
6. The flexible composite phase-change material prepared by the preparation method of any one of claims 1 to 5, wherein the flexible composite phase-change material comprises a phase-change core material and a carbon nanotube-based aerogel carrier, and the phase-change core material is loaded in three-dimensional holes of the carbon nanotube-based aerogel carrier.
7. The flexible composite phase change material as claimed in claim 6, wherein the loading amount of the phase change core material is 50-95%.
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| CN113621348B (en) * | 2021-08-16 | 2023-08-15 | 山东建筑大学 | High-heat-conductivity phase change material based on chitin derived carbon, preparation method and heat storage application thereof |
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