CN107586537B - Composite phase-change material and preparation method thereof - Google Patents
Composite phase-change material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a composite phase-change material and a preparation method thereof, wherein three-dimensional sleeve-shaped graphene is prepared by a hydrothermal method, the three-dimensional sleeve-shaped graphene is compounded with mixed salt by a vacuum impregnation method to obtain the composite phase-change material, and the mixed salt comprises borax and Na2SO4·10H2O, mixed saltsBorax and Na2SO4·10H2The mass ratio of O is (0-1): 25, the mass ratio of the three-dimensional graphene to the mixed salt is 1: (7-10). Compared with the prior art, the three-dimensional sleeve-shaped graphene structure is applied to compounding with inorganic hydrated salt, a new thought is provided for solving the problems of phase separation, supercooling and the like, the application field of the inorganic hydrated salt is greatly widened, the application prospect is wide, and the three-dimensional graphene/inorganic hydrated salt composite phase-change material can be used as a phase-enlarging capsule to be applied to the fields of building ecological energy conservation and the like.
Description
Technical Field
The invention relates to the field of composite phase-change materials, in particular to a composite phase-change material and a preparation method thereof.
Background
Graphene has a series of advantages, and is paid keen attention by researchers. The two-dimensional graphene has the characteristics of large specific surface area and high surface energy, is easy to agglomerate, and limits the application and popularization of the two-dimensional graphene in actual production. The three-dimensional graphene (3D-rGO) has stable mechanical properties, and retains some excellent properties of the two-dimensional graphene, so that the three-dimensional graphite and the composite material thereof have wide application prospects.
The inorganic hydrated salt used as the phase-change material has the advantages of high latent heat of phase change, low phase-change temperature, small environmental pollution and the like, and can be applied to the fields of cold chain transportation, ecological building energy conservation and the like. Na (Na)2SO4·10H2O is a typical low-temperature phase change material, has the melting point of 32.4 ℃, has higher phase change latent heat, good chemical stability, no toxicity, easily obtained raw materials and low price, and can be applied to the storage of solar energy and industrial waste heat. However, the inorganic hydrated salt has phase separation phenomenon and large supercooling degree, which severely limits the wide application.
Disclosure of Invention
The present invention is directed to overcome the above-mentioned drawbacks of the prior art and to provide a composite phase change material with excellent mechanical properties and thermal conductivity and a method for preparing the same.
The purpose of the invention can be realized by the following technical scheme: the composite phase-change material comprises three-dimensional graphene and mixed salt filled between the three-dimensional graphene, wherein the mixed salt comprises borax and Na2SO4·10H2O, borax and Na in the mixed salt2SO4·10H2The mass ratio of O is (0-1): 25, the mass ratio of the three-dimensional graphene to the mixed salt is 1: (7-10), wherein the amount of borax is not 0.
In the material, the three-dimensional graphene provides excellent mechanical property and structural stability, meanwhile, the graphene can effectively improve the thermal conductivity without salt deposition, improve the uniformity of inorganic hydrated salt and reduce the phase separation problem, and the electrical conductivity and the thermal conductivity of a columnar body in the direction perpendicular to the bottom surface and the direction parallel to the bottom surface have certain anisotropy, and the Na adopted by the invention2SO4·10H2Borax is added into O as a nucleating agent, so that Na can be effectively solved2SO4·10H2The supercooling degree of O is low.
A preparation method of the composite phase-change material comprises the following steps:
(1) preparing a graphite oxide solution by using a modified Hummers method such as Chen J, Yao B, Li C, et al, an improved Hummers method for eco-friendly synthesis [ J ] Carbon,2013,64(11):225-229. the modified Hummers method is described, drying the graphite oxide solution under an ultrasonic and high-pressure environment, and then cooling the graphite oxide solution to obtain the three-dimensional graphene hydrogel;
(2) precooling the three-dimensional graphene hydrogel obtained in the step (1), and then freeze-drying in a vacuum environment to obtain a three-dimensional sleeve-shaped graphene aerogel;
(3) mixing Borax and Na2SO4·10H2Mixing O uniformly to obtain mixed salt, mixing the mixed salt with the three-dimensional sleeve-shaped graphene aerogel obtained in the step (2), and then sealing and heating to fully melt the mixed salt and completely immerse the three-dimensional sleeve-shaped graphene aerogel;
(4) and (4) placing the three-dimensional sleeve-shaped graphene aerogel immersed by the mixed salt obtained in the step (3) under a vacuum condition, keeping the temperature at a constant temperature, and then cooling to obtain the composite phase-change material.
The concentration of the graphite oxide solution in the step (1) is 5-8 mg/mL.
The time of the ultrasound in the step (1) is 1-2 h.
The drying temperature in the step (1) is 160-180 ℃, the drying time is 12-24 hours, and graphite can be converted into three-dimensional graphene under the temperature and pressure.
The pre-cooling temperature in the step (2) is-15 to-30 ℃, and the pre-cooling time is 2 to 4 hours.
And (3) during the freeze drying in the step (2), keeping the environmental vacuum degree to be less than or equal to 100Pa, wherein the freeze drying temperature is-10 to-30 ℃, and the freeze drying time is 24 to 36 hours.
And (4) sealing and heating at 50-70 ℃ for 2-4 h in the step (3).
In the step (4), the vacuum condition is 0.075-0.085 MPa, the constant temperature is kept at 50-70 ℃, and the constant temperature is kept for 0.5-2 hours.
The reaction in the step (1) is as follows: in the improved hummers method, graphite is oxidized under the action of a strong oxidant to obtain graphite oxide; stripping graphite oxide into few-layer graphene oxide through ultrasonic stripping; under the high temperature and high pressure provided by the hydrothermal reaction kettle, the graphene oxide is reduced, and the graphene aerogel with a three-dimensional structure is formed.
In the step (2): and (3) after freeze drying, maintaining the three-dimensional structure of the hydrogel in the step (1) to obtain the three-dimensional graphene aerogel with mechanical strength.
In the step (3): the three-dimensional graphene aerogel is used as a filling framework and provides a multilayer gap structure, and the effect of slowing down the phase separation of inorganic salts is achieved to a certain extent.
In the step (4): and (3) fully filling and compounding inorganic salt and the three-dimensional graphene by adopting a vacuum impregnation method, and cooling to obtain the composite phase-change material.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
(1) the three-dimensional sleeve-shaped graphene structure is applied to compounding with inorganic hydrated salt, a new thought is provided for solving the problems of phase separation, supercooling and the like, the application field of the inorganic hydrated salt is greatly expanded, and the application prospect is wide;
(2) the three-dimensional graphene in the three-dimensional graphene/inorganic hydrated salt composite material prepared by the invention provides excellent mechanical property and structural stability, meanwhile, the graphene can effectively improve the thermal conductivity without salt deposition, improve the uniformity of inorganic hydrated salt and reduce the phase separation problem, and the electrical conductivity and the thermal conductivity of a columnar body in the direction vertical to the bottom surface and in the direction parallel to the bottom surface have certain anisotropy, so that the three-dimensional graphene/inorganic hydrated salt composite phase-change material obtained by the invention can be used as a phase-enlarging capsule to be applied to the fields of building ecological energy conservation and the like.
Drawings
FIG. 1 is a cross-sectional profile of a composite phase change material of the present invention;
FIG. 2 is a graph of the heat release process for a phase change material in accordance with the present invention;
FIG. 3 is a T-T cooling curve for different composite phase change materials;
FIG. 4 is 3D-rGO/Na2SO4·10H2O/2％Na2B4O7·10H2DSC curve diagram of O composite phase change material.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Preparing a graphite oxide solution by adopting an improved Hummers method laboratory, diluting the graphite oxide solution to 5mg/mL, performing ultrasonic treatment for 1h, putting 60mL of the graphite oxide solution into a hydrothermal kettle, preserving heat for 16h in a vacuum drying oven at 180 ℃, and cooling to room temperature to obtain the three-dimensional graphene hydrogel. Pre-freezing the hydrogel for 2 hours, and freeze-drying for 24 hours in a vacuum freeze dryer under the condition that the vacuum degree is less than or equal to 100Pa to obtain the three-dimensional sleeve-shaped graphene aerogel.
Adding excessive Na2SO4·10H2Placing O and three-dimensional graphene in a beaker, and adding Na2SO4·10H2The amount of O is satisfied at Na2SO4·10H2And completely immersing the three-dimensional graphene after melting the O. Sealing the beaker with preservative film, placing in a vacuum drying oven at 70 deg.C, heating at constant temperature for 2 hr to allow Na2SO4·10H2The O is melted sufficiently. And taking out the beaker, and pricking about 30-60 holes of the safety film by using a syringe needle, wherein the air holes are uniformly distributed.
Will burnThe cup is still placed in a vacuum drying oven, and the temperature is kept at 70 ℃ for 0.5h under the vacuum condition to ensure that Na is contained2SO4·10H2And fully compounding the O solution and the three-dimensional graphene, and cooling to room temperature to obtain the uniform composite phase-change material. In FIG. 1, (a) and (b) are SEM photographs of three-dimensional sleeve-shaped graphene, (c) and (D) are 3D-rGO/Na2SO4·10H2And (4) SEM (scanning electron microscope) picture of the O composite phase change material. Novel three-dimensional sleeve column structure graphite alkene provides good storage space for phase change material, and wherein three-dimensional graphite alkene volume porosity is about 94%, and phase change material can evenly stably be saved in sleeve column structure at the phase transition in-process, effectively alleviates inorganic hydrated salt phase separation problem.
Example 2
The graphite oxide solution is prepared by adopting an improved Hummers method laboratory. Diluting the prepared graphite oxide solution to 8mg/ml, performing ultrasonic treatment for 2h, placing 60ml in a hydrothermal kettle, preserving the heat for 24h at 180 ℃ in a vacuum drying oven, and cooling to room temperature to obtain the three-dimensional graphene hydrogel. Pre-freezing the hydrogel for 3h, and freeze-drying for 36h in a vacuum freeze dryer under the condition that the vacuum degree is less than or equal to 100Pa to obtain the three-dimensional sleeve-shaped graphene aerogel.
Mixing Na2SO4·10H2Placing O and three-dimensional graphene in a beaker, and adding Na2SO4·10H2The amount of O is satisfied at Na2SO4·10H2And completely immersing the three-dimensional graphene after melting the O. Sealing the beaker with preservative film, placing in a vacuum drying oven at 60 deg.C, heating at constant temperature for 3 hr to allow Na2SO4·10H2The O is melted sufficiently. The beaker is taken out, about 50 holes are punctured in the safety film by a syringe needle, and the air holes are uniformly distributed.
Placing the beaker in a vacuum drying oven, keeping the temperature of 60 deg.C under vacuum for 1.5h to allow Na2SO4·10H2And fully compounding the O solution and the three-dimensional graphene, and cooling to room temperature to obtain the uniform composite phase-change material. For Na2SO4·10H2O raw material and 3D-rGO/Na2SO4·10H2DSC thermal performance analysis is carried out on the O composite phase change material, and the DSC thermal performance analysis is shown in figure 2. 3D-rGO/Na2SO4·10H2The phase transition temperature of the O composite phase change material is lower than Na2SO4·10H2The phase transition temperature of O, so that the obtained 3D-rGO can effectively improve the heat conductivity of the phase transition material.
Example 3
The graphite oxide solution is prepared by adopting an improved Hummers method laboratory. Diluting the prepared graphite oxide solution to 7mg/ml, performing ultrasonic treatment for 2h, putting 45ml in a hydrothermal kettle, preserving the heat for 12h at 160 ℃ in a vacuum drying oven, and cooling to room temperature to obtain the three-dimensional graphene hydrogel. Pre-freezing the hydrogel for 4h at-30 ℃, keeping the vacuum degree of less than or equal to 100Pa in a vacuum freeze dryer, and freeze-drying for 24h at-30 ℃ to obtain the three-dimensional sleeve-shaped graphene aerogel.
Mixing Borax and Na2SO4·10H2And O is uniformly mixed according to the mass ratio of 1:100, 1:50, 1:33 and 1:25 respectively, the mixture and the three-dimensional graphene are placed in a beaker, and the amount of the mixture is enough to completely immerse the three-dimensional graphene after melting. Sealing the beaker with preservative film, placing in a vacuum drying oven at 70 deg.C, heating at constant temperature for 4 hr to allow Na2SO4·10H2The O is melted sufficiently. The beaker is taken out, and about 40 holes are punctured in the safety film by using the syringe needle, and the air holes are uniformly distributed.
And (3) still placing the beaker in a vacuum drying oven, keeping the temperature of 50 ℃ for 2 hours under the vacuum condition to fully compound the mixture solution and the three-dimensional graphene, and cooling to room temperature to obtain the uniform composite phase-change material. FIG. 3 is a T-T cooling curve of different composite phase change materials, from which 3D-rGO and Na can be known2B4O7·10H2O can effectively reduce the supercooling degree of the phase change material, wherein 3D-rGO and Na2B4O7·10H2The combined effect of the borax and the Na is more obvious2SO4·10H2When the mass ratio of O is 1:50, the supercooling degree is reduced to 2.5 ℃.
Example 4
The graphite oxide solution is prepared by adopting an improved Hummers method laboratory. Diluting the prepared graphite oxide solution with a certain concentration of 6mg/ml, performing ultrasonic treatment for 1.5h, placing 60ml in a hydrothermal kettle, preserving heat for 14h at 160 ℃ in a vacuum drying oven, and cooling to room temperature to obtain the three-dimensional graphene hydrogel. Pre-freezing the hydrogel at-15 ℃ for 2h, and freeze-drying the hydrogel in a vacuum freeze dryer at-10 ℃ for 24h under the condition that the vacuum degree is less than or equal to 100Pa to obtain the three-dimensional sleeve-shaped graphene aerogel.
Mixing Borax and Na2SO4·10H2Mixing O uniformly according to the mass ratio of 1:50, placing the mixture and the three-dimensional graphene in a beaker, adding Na2SO4·10H2The amount of O is satisfied at Na2SO4·10H2And completely immersing the three-dimensional graphene after melting the O. Sealing the beaker with preservative film, placing in a vacuum drying oven at 50 deg.C, heating at constant temperature for 4 hr to allow Na2SO4·10H2The O is melted sufficiently. The beaker is taken out, about 30 holes are punctured on the safety film by a syringe needle, and the air holes are uniformly distributed.
And (3) still placing the beaker in a vacuum drying oven, keeping the temperature of 70 ℃ for 1h under the vacuum condition to fully compound the mixture solution and the three-dimensional graphene, and cooling to room temperature to obtain the uniform composite phase-change material. FIG. 4 is 3D-rGO/Na2SO4·10H2O/2％Na2B4O7·10H2The DSC curve chart of the O composite phase change material shows that the supercooling degree of the phase change material is about 8 ℃, and the supercooling degree of the composite phase change material can be obtained by the DSC curve chart and 3D-rGO/Na due to certain hysteresis of DSC test2B4O7·10H2The O recombination is effectively improved.
Claims (7)
1. The composite phase change material is characterized by comprising three-dimensional graphene and mixed salt filled between the three-dimensional graphene, wherein the mixed salt comprises borax and Na2SO4·10H2O, borax and Na in the mixed salt2SO4·10H2The mass ratio of O is (0-1): 25, the mass ratio of the three-dimensional graphene to the mixed salt is 1: (7-10);
the composite phase-change material is prepared by the following steps:
(1) preparing a graphite oxide solution by adopting an improved Hummers method, carrying out ultrasonic treatment, drying, and then cooling to obtain a three-dimensional graphene hydrogel;
(2) precooling the three-dimensional graphene hydrogel obtained in the step (1), and then freeze-drying in a vacuum environment to obtain a three-dimensional sleeve-shaped graphene aerogel;
(3) mixing Borax and Na2SO4·10H2Mixing O uniformly to obtain mixed salt, mixing the mixed salt with the three-dimensional sleeve-shaped graphene aerogel obtained in the step (2), and then sealing and heating to fully melt the mixed salt and completely immerse the three-dimensional sleeve-shaped graphene aerogel;
(4) placing the three-dimensional sleeve-shaped graphene aerogel immersed by the mixed salt obtained in the step (3) under a vacuum condition, keeping the temperature at a constant temperature, and then cooling to obtain the composite phase-change material;
the environmental vacuum degree is kept to be less than or equal to 100Pa, the freeze drying temperature is-10 to-30 ℃, and the freeze drying time is 24 to 36 hours;
in the step (2): after freeze drying, the three-dimensional structure of the hydrogel in the step (1) is maintained, and the three-dimensional graphene aerogel with mechanical strength which can be utilized is obtained; and (4) taking the three-dimensional graphene aerogel in the step (3) as a filling framework, providing a multilayer gap structure, and playing a role in slowing down the phase separation of inorganic salts to a certain extent.
2. The composite phase-change material as claimed in claim 1, wherein the concentration of the graphite oxide solution in step (1) is 5-8 mg/mL.
3. The composite phase-change material as claimed in claim 1, wherein the ultrasonic treatment time in step (1) is 1-2 h.
4. The composite phase-change material as claimed in claim 1, wherein the drying temperature in step (1) is 160-180 ℃ and the drying time is 12-24 h.
5. The composite phase-change material according to claim 1, wherein the pre-cooling temperature in the step (2) is-15 to 30 ℃, and the pre-cooling time is 2 to 4 hours.
6. The composite phase-change material as claimed in claim 1, wherein the sealing heating temperature in step (3) is 50-70 ℃ and the sealing heating time is 2-4 h.
7. The composite phase-change material according to claim 1, wherein the vacuum condition in the step (4) is 0.075-0.085 MPa, the constant temperature is 50-70 ℃, and the constant temperature is kept for 0.5-2 h.
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| CN110499145A (en) * | 2019-08-26 | 2019-11-26 | 张立强 | Aeroge adsorbs phase-change accumulation energy powder, preparation method and applications |
| CN110564374B (en) * | 2019-09-18 | 2021-08-03 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
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| CN104531077A (en) * | 2015-01-27 | 2015-04-22 | 云南师范大学 | Preparation method of expanded-graphite-base hydrated salt composite solid-solid phase-change energy storage material |
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