CN113265228A - Multi-energy-driven shape-stabilized phase change material and preparation method thereof - Google Patents
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Abstract
The invention discloses a multi-energy-driven shape-stabilized phase change material and a preparation method thereof, and belongs to the technical field of multifunctional phase change materials. The phase-change material is prepared by taking a blend of paraffin-like alkane and SEBS as a phase-change material, taking graphene aerogel as a shaping matrix and a photo-thermal and electro-thermal conversion medium, uniformly distributing the paraffin-like alkane/SEBS blended phase-change material in a three-dimensional pore structure of the graphene aerogel matrix, preparing the paraffin-like alkane/SEBS blended phase-change material by melt blending, preparing the graphene aerogel matrix by using an oxidation-reduction method, and introducing the paraffin-like alkane/SEBS blend into the three-dimensional pore structure of the graphene aerogel matrix. Under the combined action of the SEBS and the graphene aerogel, the shaped phase change material provided by the invention enables the composite material to have good shape stability and leakage prevention capability, can provide good optical/electric-thermal conversion performance, and can drive phase change under optical/electric stimulation to complete energy conversion and storage.
Description
Technical Field
The invention relates to the technical field of multifunctional phase-change materials, in particular to a multi-energy-driven shape-stabilized phase-change material and a preparation method thereof.
Background
With the rapid development of economy, the demand and consumption of energy have increased year by year. However, the widespread use of fossil fuels has severely affected the environment. The demand for developing clean and renewable energy and recycling energy is more and more urgent. However, renewable energy sources such as solar energy and wind energy have a problem that time and space are inconsistent. Therefore, it is important to develop energy storage technology. The heat energy storage technology is a research hotspot at present because the heat energy storage technology is beneficial to the peak load shifting of energy, the recycling of waste heat and the like. Latent heat storage is realized by phase change of a material, and compared with a sensible heat material, the phase change material has high storage density and can absorb and release a large amount of heat under the condition of approximate constant temperature. However, conventional phase change materials only react to temperature changes, which greatly limits their application to collecting thermal energy from changes other than temperature. The filler which can convert energy sources such as solar energy, electric energy, magnetic energy and the like into heat energy is introduced, the method for obtaining the heat energy is enriched, and the utilization efficiency of the heat energy is improved.
Graphene can form three-dimensional porous graphene aerogel for paraffin alkane shaping, but the micron-sized pore size of the aerogel has a limited shaping capacity on phase change materials. At present, the graphene aerogel shape-stabilized phase change material is improved mainly by optimizing the pore diameter of the aerogel, but the difficulty of aerogel preparation is increased.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a multi-energy-source driving shape-stabilized phase-change material, which takes a blend of paraffin alkane and hydrogenated styrene-butadiene block copolymer as a phase-change material, takes graphene aerogel as a shape-stabilized matrix and a photo-thermal and electro-thermal conversion medium, and the paraffin alkane/SEBS blended phase-change material is adsorbed in a three-dimensional pore structure of the graphene aerogel matrix.
Wherein the mass content of paraffin alkane in the paraffin alkane/SEBS blend is 85-95%.
Wherein the paraffin alkane is a paraffin alkane phase change material with the phase change temperature of 18-65 ℃.
Wherein the paraffin alkane is at least one of n-hexadecane, n-heptadecane, n-octadecane, n-nonadecane, n-eicosane, n-heneicosane and n-docosane.
Wherein the hydrogenated styrene-butadiene block copolymer is at least one of G1650, G1651, G1652, FG1901, 4033, 4044 and 4055.
The graphene aerogel is prepared by reducing and freeze-drying graphene oxide.
Wherein, the optimized graphene oxide powder is TNGO-10, the purity is more than 98 wt%, the number of layers is 1-2, and the diameter is 8-15 μm.
The invention further discloses a preparation method of the multi-energy-driven shape-stabilized phase change material, which comprises the following steps:
(1) preparing a paraffin/SEBS blending phase-change material by melt blending paraffin and SEBS;
(2) reacting graphene oxide with a reducing agent to prepare graphene hydrogel, and then freezing and drying to prepare a graphene aerogel matrix;
(3) and adsorbing the paraffin alkane/SEBS blended phase-change material in a three-dimensional pore structure of the graphene aerogel matrix to prepare the multi-energy-driven shape-stabilized phase-change material.
The step 1 melt blending is preferably carried out at 180 ℃, and a heating environment provided by common oil bath heating equipment can be adopted.
In order to better realize the invention, the melt blending in the step 1 needs to reach a certain stirring speed and maintain the stirring for a certain time, and preferably, a speed-reducing and force-increasing stirrer can be adopted, the stirring speed is not lower than 70rpm, and the time is not less than 30 min.
And 2, specifically, preparing a graphene oxide dispersion solution, adding ascorbic acid as a reducing agent, and carrying out reduction reaction in an oven at 95 ℃ for 6 hours to obtain the graphene hydrogel.
Wherein, the temperature of the reduction reaction in the step 2 is controlled at 95 ℃.
And 2, performing a freeze-drying method, namely dialyzing the graphene hydrogel, and performing freeze-drying in a vacuum and low-temperature environment to obtain the graphene aerogel.
Wherein, the step 3 adopts a vacuum impregnation method, the vacuum degree is lower than-0.08 MPa at 180 ℃, and the impregnation time is not less than 3 h.
The beneficial effects produced by the invention are as follows:
according to the invention, a thermoplastic elastomer hydrogenated styrene-butadiene block copolymer (SEBS) and paraffin alkane blend is used as a phase change material, a graphene aerogel is used as a shaping matrix, the strong compatibility of the SEBS and the paraffin alkane is utilized, the fluidity of the paraffin alkane is firstly changed, the paraffin alkane/SEBS blend phase change material is further shaped by utilizing the capillary action of the graphene aerogel, the micron-sized light graphene aerogel used as a supporting matrix can be encapsulated without changing the phase change behavior of the material, the enthalpy value of the composite material is retained to the greatest extent, and the composite material has good shape stability and leakage prevention capability under the combined action of the SEBS and the graphene aerogel;
the multi-energy-source driven shape-stabilized phase change material prepared by the invention simultaneously has the following characteristics: the material achieves the purpose of phase change temperature control by utilizing the phase change latent heat of the phase change material, and the light three-dimensional porous matrix accounts for extremely low proportion in the composite material, so that the load rate of the phase change material can reach nearly 94%, the leakage is avoided, the heat storage capacity is extremely high, and the good electric conduction and photo-thermal conversion capacity of graphene introduces the photo/electric-thermal conversion performance to the composite material;
due to the fact that the graphene has excellent heat conduction and electric conduction performance and can absorb light energy in the full-wave band range (ultraviolet-visible-infrared) and convert the light energy into heat energy, the multi-energy driving shape-stabilized phase change material provides good light/electricity-heat conversion performance, and can drive phase change under light/electricity stimulation to complete energy conversion and storage.
Drawings
FIG. 1 is a graph showing the setting effects at 80 ℃ in examples 1 to 3 and comparative examples 1 to 3;
FIG. 2 is a DSC curve before and after 200 consecutive thermal cycles of example 1 and comparative example 1;
FIG. 3 is a schematic view of photothermal conversion and a performance curve of example 1, comparative example 2 and comparative example 4;
FIG. 4 is a schematic diagram of electrothermal conversion and performance curves at 5V and 8V voltages in example 1.
Detailed Description
The paraffin alkane material is an important organic phase change material, has low cost, wide source and adjustable phase change temperature, has wide application prospect in an energy storage system, and the hydrogenated styrene-butadiene block copolymer (SEBS) is a linear triblock copolymer which takes polystyrene as a terminal segment and takes an ethylene-butylene copolymer obtained by hydrogenation of polybutadiene as a middle elastic block, the SEBS does not contain unsaturated double bonds, has good stability and aging resistance, and has better compatibility with paraffin alkane.
The graphene is used as an excellent heat conduction, electric conduction and photo-thermal conversion medium, the phase-change material is introduced into the phase-change material, the defect that the traditional phase-change material is driven to store energy only by temperature can be effectively overcome, the phase-change material is used for developing a multi-energy-driven composite phase-change material, and solar energy and electric energy can be effectively converted into heat energy and stored.
According to the invention, the fluidity of paraffin alkane is improved by using SEBS, the fluidity of the phase change material is changed to a certain extent, and then the graphene aerogel is used for shaping, so that the latent heat of phase change can be retained to a large extent and can be effectively shaped. Meanwhile, the introduction of the graphene enables the composite material to have light-heat conversion, electricity-heat conversion and heat energy storage performance, so that multi-energy-driven phase change becomes possible.
Examples of preparation of materials
The preparation examples of the multi-energy-source-driven shape-stabilized phase-change material are carried out as follows, and the mixture ratio of the phase-change wax OP44E and the SEBS and the blending and stirring time in different examples are shown in Table 1.
Mechanically stirring, melting and blending OP44E phase-change wax and SEBS for a certain time at 180 ℃, wherein the stirring speed is 70rpm, and the mixture is uniformly mixed to present a transparent color, so as to obtain the paraffin/SEBS blended phase-change material;
preparing 20ml of graphene oxide dispersion liquid (2mg/ml), adding 80mg of ascorbic acid as a reducing agent, carrying out reduction reaction in a 95 ℃ drying oven for 6 hours to obtain graphene hydrogel, dialyzing the hydrogel for 2 days by using an ethanol solution, and carrying out vacuum drying for 48 hours at-40 ℃ by using a freeze dryer to obtain a graphene aerogel matrix;
and (3) placing the paraffin/SEBS blended phase-change material and the graphene aerogel in a vacuum drying oven at 180 ℃ and under-0.08 MPa for 3h to enable the paraffin/SEBS blended phase-change material to be adsorbed in the three-dimensional pore structure of the graphene aerogel matrix, so as to obtain the multi-energy driving shape-stabilized phase-change material.
TABLE 1 Material proportioning Table for different examples
Comparative example 1
A preparation method of a composite phase-change material comprises the following steps: preparing 20ml of graphene oxide dispersion liquid (2mg/ml), adding 80mg of ascorbic acid as a reducing agent, carrying out reduction reaction in a 95 ℃ drying oven for 6 hours to obtain graphene hydrogel, dialyzing the hydrogel for 2 days by using an ethanol solution, and carrying out vacuum drying for 48 hours at-40 ℃ by using a freeze dryer to obtain a graphene aerogel matrix;
and (3) placing the paraffin and the graphene aerogel in a vacuum drying oven at 180 ℃ and under-0.08 MPa for 3h to make the paraffin adsorbed in the three-dimensional pore structure of the graphene aerogel matrix to obtain the composite phase-change material.
Comparative example 2
A preparation method of a composite phase-change material comprises the following steps: and mechanically stirring, melting and blending 30gOP44E phase-change wax and 1.5g of SEBS (FG1901) at 180 ℃ for 30min, wherein the stirring speed is 70rpm until the system is uniformly mixed and presents a transparent color, and naturally cooling to obtain the composite phase-change material.
Comparative example 3
The dosage of OP44E phase-change wax is 30g, the dosage of SEBS is 0.6g, the blending and stirring time is 15min, and the rest is the same as the preparation method of the embodiment.
Comparative example 4
Pure OP44E phase change wax was used.
Examples of Performance test
The results of the phase change temperature and the phase change latent heat parameters measured by the phase change materials of the 3 embodiments are shown in table 1, and the heat storage performance is tested by a DSC-Q20 heat flow type differential scanning calorimeter produced by the American TA instruments company, the temperature is 10-80 ℃, the temperature rising (lowering) rate is 5 ℃/min, and the nitrogen protection is performed. As can be seen from Table 1, the enthalpy values of the phase change latent heat of the multi-energy-source driven shape-stabilized phase change materials obtained in examples 1 to 3 are all above 190J/g and are matched with the load factor of the phase change materials. The paraffin and alkane phase change material with higher enthalpy can be used for obtaining the multi-energy-driven shape-stabilized phase change material with higher latent heat value.
TABLE 1 statistical table of phase transition temperature and latent heat of phase transition parameters
The shaping effects of the multi-energy-source-driven shape-stabilized phase change materials obtained in examples 1 to 3 and the shape-stabilized phase change materials obtained in comparative examples 1 to 3 were respectively detected, and the results are shown in fig. 1, and it can be seen from fig. 1 that the multi-energy-source-driven shape-stabilized phase change materials obtained in examples 1 to 3 did not leak significantly at 80 ℃.
The multi-energy-driven shape-stabilized phase change material obtained in example 1 and the phase change material obtained in comparative example 1 were subjected to continuous 200 cycles of heat cycle, and DSC curves before and after the cycle were measured and plotted, and the results are shown in fig. 2, in example 1, the enthalpy value of heat absorption was 226.30J/g, the enthalpy value of heat release was 226.10J/g, the enthalpy value of heat absorption was 219.50J/g, the enthalpy value of heat release was 221.00J/g, the specific gravity of enthalpy value decrease was 3.005% and 2.256%, in comparative example 1, the enthalpy value of heat absorption was 236.80J/g, the enthalpy value of heat release was 235.90, the enthalpy value of heat absorption was 202.50J/g, the enthalpy value of heat release was 202.80J/g, and the enthalpy value decrease was 14.485% and 14.031%, respectively. From the calculation results, it is understood that example 1 has more excellent cycle reliability than comparative example 1.
The results of the multi-energy-driven shape-stabilized phase change material obtained in example 1 and the photothermal conversion effects of comparative examples 2 and 4 were respectively examined, and as can be seen in fig. 3, the obtained multi-energy-driven shape-stabilized phase change material has photothermal conversion and storage capabilities.
The electric-thermal conversion effect of the multi-energy-source-driven shape-stabilized phase-change material obtained in example 1 is detected, and the result is shown in fig. 4, and it can be seen from fig. 4 that the obtained multi-energy-source-driven shape-stabilized phase-change material has electric-thermal conversion and storage capabilities.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. Several alternatives or modifications to the described embodiments may be made without departing from the inventive concept and such alternatives or modifications should be considered as falling within the scope of the present invention.
Claims (10)
1. A multi-energy-source driven shape-stabilized phase change material is characterized in that: the multi-energy-source-driven shaping phase-change material comprises a paraffin alkane/SEBS (styrene-ethylene-butadiene-styrene) blend and graphene aerogel, the paraffin alkane and hydrogenated styrene-butadiene block copolymer blend is used as the phase-change material, the graphene aerogel is used as a shaping matrix and a photothermal and electrothermal conversion medium, and the paraffin alkane/SEBS blend phase-change material is adsorbed in a three-dimensional pore structure of the graphene aerogel matrix.
2. The multi-energy-source driven shape-stabilized phase-change material as claimed in claim 1, wherein: the mass content of paraffin alkane in the paraffin alkane/SEBS blend is 85-95%.
3. A multiple energy source driven shape-stabilized phase change material as claimed in claim 1 or 2, wherein: the paraffin alkane is a paraffin alkane phase change material with the phase change temperature of 18-65 ℃.
4. The multi-energy-source driven shape-stabilized phase-change material as claimed in any one of claims 1 to 3, wherein: the paraffin alkane is at least one of n-hexadecane, n-heptadecane, n-octadecane, n-nonadecane, n-eicosane, n-heneicosane and n-docosane.
5. The multi-energy-source driven shape-stabilized phase-change material as claimed in any one of claims 1 to 4, wherein: the hydrogenated styrene-butadiene block copolymer is at least one of G1650, G1651, G1652, FG1901, 4033, 4044 and 4055.
6. The method for preparing the multi-energy-source driven shape-stabilized phase-change material according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) preparing a paraffin/SEBS blending phase-change material by melt blending paraffin and SEBS;
(2) reacting graphene oxide with a reducing agent to prepare graphene hydrogel, and then freezing and drying to prepare a graphene aerogel matrix;
(3) and adsorbing the paraffin alkane/SEBS blended phase-change material in a three-dimensional pore structure of the graphene aerogel matrix to prepare the multi-energy-driven shape-stabilized phase-change material.
7. The method for preparing a multi-energy-source driven shape-stabilized phase-change material as claimed in claim 6, wherein: step 1 the blending temperature is controlled at 170-190 ℃.
8. The method for preparing a multi-energy-source driven shape-stabilized phase-change material according to claim 6 or 7, wherein: the freeze-drying method is to prepare the graphene aerogel by dialyzing the graphene hydrogel and then freeze-drying the graphene hydrogel in a vacuum and low-temperature environment.
9. The method for preparing the multi-energy-source driven shape-stabilized phase change material according to any one of claims 6 to 8, wherein: step 3 adopts a vacuum impregnation method, the vacuum degree is lower than-0.08 MPa at 180 ℃, and the impregnation time is not less than 3 h.
10. The use of the multi-energy-driven shape-stabilized phase change material according to any one of claims 1 to 5 in the fields of thermal energy storage, light-to-heat conversion and storage, or electricity-to-heat conversion and storage.
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| CN114636188A (en) * | 2022-03-18 | 2022-06-17 | 华南师大(清远)科技创新研究院有限公司 | Phase change material-based heating warm patch |
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