CN112094625A - Boron nitride nanotube aerogel/phase change heat conduction composite material and preparation method thereof - Google Patents
Boron nitride nanotube aerogel/phase change heat conduction composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a boron nitride nanotube aerogel/phase change heat conduction composite material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) mixing and dispersing a boron nitride nanotube raw material with a graphene oxide solution uniformly to obtain a uniform boron nitride nanotube/graphene oxide dispersion solution; (2) dropwise adding a reducing agent into the boron nitride nanotube/graphene oxide dispersion liquid, carrying out hydrothermal reduction under a heating condition to obtain hydrogel, and then carrying out vacuum freeze drying to obtain boron nitride nanotube aerogel; (3) under the heating condition, dropwise adding a melted solid-liquid organic phase change material into the boron nitride nanotube aerogel, then transferring the boron nitride nanotube aerogel into a vacuum condition to heat so as to remove residual bubbles, and cooling to room temperature to obtain the boron nitride nanotube aerogel/phase change heat conduction composite material. The phase-change composite material prepared by the invention has high heat-conducting property and heat-storing property.
Description
Technical Field
The invention relates to the technical field of phase-change heat-conducting composite materials, in particular to a preparation method of a phase-change composite material based on boron nitride nanotube aerogel.
Background
At present, the energy problem has become a bottleneck for further improvement of human material and mental life. The phase-change material can absorb or emit heat from the environment in the phase-change process, thereby storing and releasing heat energy and effectively improving the utilization rate of energy. Therefore, in recent years, phase change energy storage materials have become hot spots in energy utilization and material research. The solar heat collector can be widely applied to the fields of solar heat utilization, building energy conservation, heat management and the like. Organic phase change materials have many advantages such as small phase change temperature fluctuation, large phase change latent heat, stable chemical properties, and the like, and thus are widely researched. However, the organic phase-change material has the disadvantages of low heat conductivity, large volume change in the phase-change process, easy leakage and the like, so that the application process of the organic phase-change material is limited to a certain extent. The three-dimensional porous material formed by the organic phase-change material and the high-thermal-conductivity filler is compounded, can provide a thermal conduction path and simultaneously play a supporting role, and is one of effective means for improving the performance of the phase-change material.
The boron nitride nanotube has a crystal structure similar to that of carbon nanotube and is composed of B atom, N atom and SP atom2Hybridized into a tubular structure formed by bonding. The boron nitride nanotube has high thermal conductivity, high-temperature oxidation resistance, good chemical stability, excellent dielectric property and high elastic modulus, so that the boron nitride nanotube has very potential application value in the field of heat-conducting composite materials. Song et al prepared boron nitride nanotube/nanosheet hybrid porous aerogel using carbon aerogel as a template by chemical vapor deposition under high temperature and high pressure conditions. Due to the strong hydrophobicity and the lack of surface functional groups of the boron nitride nanotube, the construction of a three-dimensional porous structure based on the boron nitride nanotube by a simple method still has great challenges.
The organic phase change material and the three-dimensional boron nitride nanotube aerogel are compounded to realize stable shape and improve the heat transfer performance and the heat storage performance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a boron nitride nanotube aerogel/phase change heat conduction composite material.
The invention provides a boron nitride nanotube aerogel/phase-change heat-conducting composite material, which comprises a boron nitride nanotube aerogel framework and a solid-liquid organic phase-change material, wherein the boron nitride nanotube aerogel framework is composed of boron nitride nanotubes and graphene oxide, and the solid-liquid organic phase-change material is filled in and around the aerogel framework.
One aspect of the invention provides a preparation method of a boron nitride nanotube aerogel/phase change heat conduction composite material, which comprises the following steps:
(1) mixing and dispersing a boron nitride nanotube raw material and a graphene oxide solution uniformly to obtain a uniform boron nitride nanotube/graphene oxide dispersion solution;
(2) dropwise adding a reducing agent into the boron nitride nanotube/graphene oxide dispersion liquid, carrying out hydrothermal reduction under a heating condition to obtain hydrogel, and then carrying out vacuum freeze drying to obtain boron nitride nanotube aerogel;
(3) under the heating condition, adding a melted solid-liquid organic phase change material into the graphene-reinforced boron nitride nanotube aerogel, then transferring to a vacuum condition for heating to remove residual bubbles, and cooling to room temperature to obtain the boron nitride nanotube aerogel/phase change heat conduction composite material.
In the technical scheme of the invention, the concentration of the graphene oxide solution in the step (1) is 2-6mg/ml, preferably 3-5mg/ml, and more preferably 4 mg/ml.
In the technical scheme of the invention, the mass ratio of the boron nitride nanotube to the graphene oxide in the step (1) is 1: (0.1-20), preferably 1: (0.5-15), more preferably 1: (1-9).
In the technical scheme of the invention, the step (1) of uniformly mixing and dispersing is to disperse by ultrasonic and stirring, preferably, after dispersing for 6-12h by low-power ultrasonic, the mixture is stirred by magnetic force for further dispersing for 1-2 h.
In the technical scheme of the invention, the reducing agent in the step (2) is selected from one or a mixture of at least two of hydrazine hydrate, hydrogen iodide, vitamin C, ammonium sulfide, tea polyphenol or ethylenediamine, preferably ethylenediamine; the volume ratio of the boron nitride nanotube/graphene oxide dispersion liquid to the boron nitride nanotube/graphene oxide dispersion liquid is 100-: 1.
in the technical scheme of the invention, the conditions of hydrothermal reduction under the heating condition in the step (2) are as follows: in a sealed environment, the heating temperature is 50-150 ℃, preferably 75-105 ℃, and more preferably 85-95 ℃; the heating time is 5-20h, preferably 6-15h, more preferably 8-12 h.
In the technical scheme of the invention, the freeze-drying process in the step (2) comprises the following steps: and taking out the reacted hydrogel, and freeze-drying the hydrogel for 24 to 48 hours under the vacuum condition by using a vacuum freeze dryer, wherein the freezing temperature is-20 to-80 ℃, the freezing temperature is preferably-50 ℃, and the vacuum degree is 10 to 100Pa, and the vacuum degree is preferably 33 Pa.
In the technical scheme of the invention, all operations in the step (3) are completed under the heating condition, and the heating temperature is 60-90 ℃, preferably 80-90 ℃, and more preferably 85 ℃.
In the technical scheme of the invention, the solid-liquid organic phase change material in the step (3) is one or more of polyethylene glycol, paraffin, polyols and fatty acids, preferably polyethylene glycol, and more preferably polyethylene glycol with a relative molecular weight of 4000-10000.
In the technical scheme of the invention, in the step (3), the operation time of switching to the vacuum condition for heating to remove the residual bubbles is 12-24 h.
In the technical scheme of the invention, in the step (3), in the operation of heating under vacuum condition to remove residual bubbles and then cooling, the cooling temperature is room temperature, and the cooling time is 10-20 min.
In another aspect, the invention provides a boron nitride nanotube aerogel/phase change heat conduction composite material prepared by the method.
In order to solve the problems of low thermal conductivity, electric insulation and the like of a phase change energy storage material in the prior art, graphene oxide is used as a dispersing agent and a cross-linking agent of a boron nitride nanotube, and a uniformly dispersed boron nitride nanotube/graphene oxide solution is subjected to hydrothermal reduction and freeze drying to obtain the boron nitride nanotube aerogel. And then, the phase-change material is filled in the three-dimensional structure of the stone boron nitride nanotube aerogel by a vacuum impregnation method, so that the seepage of the phase-change material is effectively prevented, and the heat-conducting property of the phase-change material is improved. The boron nitride nanotube makes the surface of the aerogel rough and hydrophobic, and the capillary force generated by the boron nitride nanotube can further improve the adsorption capacity on the phase-change material, so that the shape stability of the phase-change composite material is improved. In addition, due to the unique boron nitride nanotube hybrid structure, the phase change heat storage capacity of the composite material is also improved.
The method comprises the steps of firstly, using the surface activity of the graphene oxide as a dispersing agent to disperse the boron nitride nanotube to obtain a uniformly dispersed boron nitride nanotube/graphene oxide solution. Therefore, boron nitride nanotubes with different mass can be added, but the mass ratio of the boron nitride nanotubes to the graphene oxide is not more than 1:1, otherwise, a uniformly dispersed boron nitride nanotube/graphene oxide dispersion cannot be formed. And preparing a solution with the mass ratio of the two being 0:1, namely, not adding the boron nitride nanotube, comparing the two, and comparing the influence of the graphene nanosheet on the composite material.
And dropwise adding a reducing agent ethylenediamine into the uniformly dispersed boron nitride nanotube/graphene oxide dispersion liquid, and then carrying out hydrothermal reduction at the temperature of 85-95 ℃ for 8-12 h. Due to poor thermal conductivity of graphene oxide, it can be reduced by hydrothermal reaction and form a three-dimensional network. In the experimental process, the gelation of the dispersion liquid is increased along with the increase of the content of the boron nitride nanotube, the reduction degree of the reaction is also related to the reaction temperature, and the graphene oxide can be effectively reduced by adopting the conditions in the invention.
Advantageous effects
(1) According to the invention, graphene oxide is used as a dispersing agent and a cross-linking agent to obtain a uniformly dispersed boron nitride nanotube/graphene oxide solution, and self-assembly is initiated under a hydrothermal condition through a reducing agent ethylenediamine, so that the boron nitride nanotube uniformly dispersed hybrid three-dimensional porous aerogel is obtained while the graphene oxide is reduced. The invention finds that the addition amount of the boron nitride nanotube can adjust the performance of the composite material, thereby obtaining the composite material with adjustable heat storage performance and heat conduction performance.
(2) Different from the three-dimensional graphene aerogel, the boron nitride nanotubes exist on the surface of the graphene sheet layer or between interlayers, and are mutually crosslinked to form a three-dimensional network structure. The boron nitride nanotube with excellent thermal conductivity can be used as a thermal conductive filler to improve the thermal conductivity of the phase-change material.
(3) The three-dimensional porous structure of the boron nitride nanotube aerogel can absorb the phase-change material, wherein the surface of the aerogel is hydrophobic and rough due to the addition of the boron nitride nanotube, so that the phase-change material can be adsorbed more favorably, and the shape stability of the phase-change material is improved. The phase-change composite material prepared by the invention not only improves the heat-conducting property, but also improves the heat-storing property.
(4) The preparation method is simple and has good repeatability. The boron nitride nanotube aerogel is used as a heat conducting framework and is compounded with a solid-liquid phase change organic material, so that the shape stability and the heat conductivity of the phase change composite material are effectively improved. Can effectively solve the technical problem of easy leakage and has good application prospect.
Drawings
Fig. 1 is a field emission scanning electron microscope image of the graphene aerogel prepared in example 1 at different magnifications;
FIG. 2 is a field emission scanning electron microscope image of the boron nitride nanotube aerogel prepared in example 2 under different magnifications;
FIG. 3 is a DSC plot of the composites prepared in examples 1-4 and polyethylene glycol;
fig. 4 is a graph of the thermal conductivity of the composite material and polyethylene glycol prepared in examples 1-4.
Detailed Description
The present invention is explained in detail by the following examples and the accompanying drawings. However, it is understood by those skilled in the art that the following examples are not intended to limit the scope of the present invention, and any modifications and variations based on the present invention are within the scope of the present invention.
Example 1
(1) 3ml of graphene oxide solution (4mg/ml) was placed in a sample bottle, and 20. mu.L of ethylenediamine was added as a reducing agent, followed by hydrothermal reduction at 95 ℃ for 12 hours. And (4) taking out the graphene columnar gel after the reaction is finished, and performing vacuum freeze-drying for 24 hours by using a vacuum freeze dryer to obtain the graphene aerogel.
(2) And (3) using polyethylene glycol as a phase-change material, heating and melting the phase-change material, slowly dripping the phase-change material on the graphene aerogel, transferring the graphene aerogel into a vacuum drying oven, heating for 12 hours under a vacuum condition at 85 ℃, removing residual bubbles, and cooling a sample to room temperature to obtain the graphene aerogel phase-change heat-conducting composite material.
Example 2
(1) Putting 3ml of graphene oxide solution (4mg/ml) into a sample bottle, and adding a certain amount of boron nitride nanotubes, wherein the mass ratio of the boron nitride nanotubes to the graphene oxide is 1: and 9, performing ultrasonic treatment for 6 hours, and stirring for 1 hour to obtain the boron nitride nanotube/graphene oxide dispersion liquid.
(2) The mixture was placed in a sample bottle, and 20. mu.L of ethylenediamine as a reducing agent was added to conduct hydrothermal reduction at 95 ℃ for 12 hours. And (3) taking out the boron nitride nanotube/graphene columnar gel after the reaction is finished, and performing vacuum freeze-drying for 24 hours by using a vacuum freeze dryer to obtain the boron nitride nanotube aerogel.
(3) And (2) using polyethylene glycol as a phase-change material, heating and melting the phase-change material, slowly dripping the phase-change material on the boron nitride nanotube aerogel, transferring the boron nitride nanotube aerogel into a vacuum drying oven, heating for 12 hours under a vacuum condition at 85 ℃, removing residual bubbles, and cooling a sample to room temperature to obtain the boron nitride nanotube aerogel phase-change heat-conducting composite material.
Fig. 1 and 2 are scanning electron micrographs of the graphene aerogel in example 1 and the boron nitride nanotube aerogel in example 2, respectively. The prepared graphene aerogel and the boron nitride nanotube aerogel can be observed to be of a three-dimensional porous honeycomb structure, but the boron nitride nanotube aerogel can be observed to be uniformly distributed on the surface of a graphene sheet layer or in an interlayer.
Example 3
(1) Putting 3ml of graphene oxide solution (4mg/ml) into a sample bottle, adding a certain amount of boron nitride nanotubes, wherein the mass ratio of the boron nitride nanotubes to the graphene oxide is 3:7, performing ultrasonic treatment for 6 hours, and stirring for 1 hour to obtain the boron nitride nanotube/graphene oxide dispersion solution.
(2) The mixture was placed in a sample bottle, and 20. mu.L of ethylenediamine as a reducing agent was added to conduct hydrothermal reduction at 95 ℃ for 12 hours. And (3) taking out the boron nitride nanotube/graphene columnar gel after the reaction is finished, and performing vacuum freeze-drying for 24 hours by using a vacuum freeze dryer to obtain the boron nitride nanotube aerogel.
(3) And (2) using polyethylene glycol as a phase-change material, heating and melting the phase-change material, slowly dripping the phase-change material on the boron nitride nanotube aerogel, transferring the boron nitride nanotube aerogel into a vacuum drying oven, heating for 12 hours under a vacuum condition at 85 ℃, removing residual bubbles, and cooling a sample to room temperature to obtain the boron nitride nanotube aerogel phase-change heat-conducting composite material.
Example 4
(1) Putting 3ml of graphene oxide solution (4mg/ml) into a sample bottle, and adding a certain amount of boron nitride nanotubes, wherein the mass ratio of the boron nitride nanotubes to the graphene oxide is 1: and (3) carrying out ultrasonic treatment for 6h, and stirring for 1h to obtain the boron nitride nanotube/graphene oxide dispersion liquid.
(2) The mixture was placed in a sample bottle, and 20. mu.L of ethylenediamine as a reducing agent was added to conduct hydrothermal reduction at 95 ℃ for 12 hours. And (3) taking out the boron nitride nanotube/graphene columnar gel after the reaction is finished, and performing vacuum freeze-drying for 24 hours by using a vacuum freeze dryer to obtain the boron nitride nanotube aerogel.
(3) And (2) using polyethylene glycol as a phase-change material, heating and melting the phase-change material, slowly dripping the phase-change material on the boron nitride nanotube aerogel, transferring the boron nitride nanotube aerogel into a vacuum drying oven, heating for 12 hours under a vacuum condition at 85 ℃, removing residual bubbles, and cooling a sample to room temperature to obtain the boron nitride nanotube aerogel phase-change heat-conducting composite material.
The DSC curve of the prepared boron nitride nanotube aerogel phase-change thermal conductive composite in examples 1 to 4 is shown in fig. 3, which shows that the phase-change temperature of the composite is almost unchanged and the phase-change enthalpy is not lost.
The thermal conductivity of the composite material is shown in fig. 4, and the thermal conductivity of the composite material is obviously improved.
The boron nitride nanotube aerogel phase-change thermal conductive composite materials prepared in the above examples 1-4.
And the thermal properties of polyethylene glycol are specified in table 1 below.
TABLE 1
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should understand that they can make improvements and modifications without departing from the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The preparation method of the boron nitride nanotube aerogel/phase change heat conduction composite material is characterized by comprising the following steps of:
(1) mixing and dispersing a boron nitride nanotube raw material with a graphene oxide solution uniformly to obtain a uniform boron nitride nanotube/graphene oxide dispersion solution;
(2) dropwise adding a reducing agent into the boron nitride nanotube/graphene oxide dispersion liquid, carrying out hydrothermal reduction under a heating condition to obtain hydrogel, and then carrying out vacuum freeze drying to obtain boron nitride nanotube aerogel;
(3) under the heating condition, dropwise adding a melted solid-liquid organic phase change material into the boron nitride nanotube aerogel, then transferring the boron nitride nanotube aerogel into a vacuum condition to heat so as to remove residual bubbles, and cooling to room temperature to obtain the boron nitride nanotube aerogel/phase change heat conduction composite material.
2. The method for preparing boron nitride nanotube aerogel/phase change thermal conductive composite material according to claim 1, wherein the mass ratio of the boron nitride nanotubes to the graphene oxide in the step (1) is 1: (0.1-20), preferably 1: (0.5-15), more preferably 1: (1-9).
3. The method is characterized in that the concentration of the graphene oxide in the step (1) is 1-10mg/ml, preferably 3-5mg/ml, and more preferably 4 mg/ml.
4. The method for preparing boron nitride nanotube aerogel/phase-change thermal conductive composite material as claimed in claim 1, wherein the reducing agent in the step (2) is ethylenediamine, and the volume ratio of ethylenediamine to the boron nitride nanotube/graphene oxide dispersion is 100-: 1.
5. the preparation method of the boron nitride nanotube aerogel/phase change thermal conductive composite material as claimed in claim 1, wherein the hydrothermal reduction under heating in the step (2) comprises: in a sealed environment, the heating temperature is 50-150 ℃, the heating temperature is preferably 75-105 ℃, the heating time is preferably 85-95 ℃, and the heating time is 5-20h, preferably 6-15h, and the heating time is preferably 8-12 h.
6. The preparation method of the boron nitride nanotube aerogel/phase change thermal conductive composite material as claimed in claim 1, wherein the freeze-drying process in the step (2) comprises: and taking out the reacted hydrogel, and freeze-drying for 24-48h under a vacuum condition, wherein the freezing temperature is-50 ℃, and the vacuum degree is 33 Pa.
7. The method for preparing boron nitride nanotube aerogel/phase change thermal conductive composite material as claimed in claim 1, wherein the solid-liquid organic phase change material in step (3) is one or more of polyethylene glycol, paraffin, polyol and fatty acid, preferably polyethylene glycol, more preferably polyethylene glycol having a relative molecular weight of 4000-10000.
8. The preparation method of the boron nitride nanotube aerogel/phase change thermal conductive composite material as claimed in claim 1, wherein all operations in step (3) are performed under heating conditions, wherein the heating temperature is 60-90 ℃, preferably 80-90 ℃, and more preferably 85 ℃.
9. The boron nitride nanotube aerogel/phase-change thermal conductive composite material prepared by the method for preparing the boron nitride nanotube aerogel/phase-change thermal conductive composite material according to any one of claims 1 to 8.
10. A boron nitride nanotube aerogel/phase change heat conduction composite material comprises a boron nitride nanotube aerogel framework composed of boron nitride nanotubes and graphene oxide, and a solid-liquid organic phase change material filled in and around the aerogel framework;
preferably, the mass ratio of the boron nitride nanotubes to the graphene oxide is 1: (0.1-20); the solid-liquid organic phase change material is one or more of polyethylene glycol, paraffin, polyalcohol and fatty acid.
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