CN108531141B - Preparation method of composite phase change energy storage material with organic matter filled with ordered pore alumina template - Google Patents
Preparation method of composite phase change energy storage material with organic matter filled with ordered pore alumina template Download PDFInfo
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Abstract
Organic matter filled ordered pore aluminaA preparation method of a composite phase-change energy storage material of a template relates to a preparation method of a composite phase-change energy storage material. The invention aims to solve the technical problems that the pore size distribution of the existing inorganic porous material is randomly oriented, the swelling crack phenomenon is easy to occur in the dipping process, and the composite phase change material formed by adsorption has poor uniformity and low thermal conductivity. The invention comprises the following steps: firstly, preparing Al2O3Sol; secondly, preparing ceramic slurry; thirdly, directional freezing; fourthly, preparing the composite phase change material. The invention adopts the freezing injection molding to prepare the Al with the directional hole structure2O3And (3) completing impregnation of the phase-change material by adopting a melting impregnation process. Experimental results prove that the Al prepared by the invention2O3The template has good packaging performance, and the prepared composite phase change material has high energy storage density.
Description
Technical Field
The invention relates to a preparation method of a composite phase change energy storage material.
Background
The phase change energy storage has the obvious advantage of high heat storage density and has important significance for improving the utilization efficiency of energy. In practical application, the phase change energy storage material is easy to have liquid leakage problem in the solid-liquid phase change process. The main solutions to the leakage problem are three: firstly, adsorbing a phase change energy storage material in an inorganic porous material to form a composite phase change material; secondly, wrapping the phase change energy storage material in microcapsules formed by organic polymers; thirdly, compounding the phase change material with a high polymer material to prepare the high polymer-based composite sizing phase change material. As the first method, commonly used inorganic porous materials are carbon foam (carbon foam), diatomaceous earth (diatomite), montmorillonite (montmorillonite), and the like. The pore size distribution of the inorganic porous materials is often in random orientation, the inorganic porous materials are easy to generate a spalling phenomenon in the dipping process, the uniformity of the composite phase change material formed by adsorption is poor, and the thermal conductivity is reduced by continuously passing through an interface formed by the phase change material and the inorganic porous materials in the heat transfer process.
The basic principle of the freeze injection molding process is as follows: the slurry is placed on a plane cold source, the cold source can form a directional temperature gradient in the slurry, the solvent can be directionally solidified along the direction of the temperature gradient to form 'ice crystals', then the solvent is directly sublimated to a gas state from a solid state by adopting a vacuum freeze drying mode to form a pore structure, and the solute forms a pore wall.
Disclosure of Invention
The invention provides a preparation method of a composite phase change energy storage material with an organic matter filled ordered pore alumina template, aiming at solving the technical problems that the pore size distribution of the existing inorganic porous material is randomly oriented, the pore size distribution is easy to generate a spalling phenomenon in the dipping process, the uniformity of the composite phase change material formed by adsorption is poor, and the thermal conductivity is low.
The preparation method of the composite phase change energy storage material with the ordered pore alumina template filled with the organic matter is carried out according to the following steps:
firstly, preparing Al2O3Sol: dissolving aluminum sec-butoxide in water to obtain a mixed solution, refluxing for 1-1.5 h under the conditions of 90-95 ℃ water bath and stirring, then adding dilute nitric acid, continuously refluxing for 9h under the conditions of 90-95 ℃ water bath and stirring, and naturally cooling to room temperature to obtain Al2O3Sol; the molar ratio of the aluminum sec-butoxide to the water is 1 (60-100); the mass concentration of the dilute nitric acid is 65-68 percent; the volume ratio of the dilute nitric acid to the mixed solution is 1 (50-55);
secondly, preparing ceramic slurry: al prepared in the first step2O3Refluxing the sol at 50 deg.C for 10-30 min, adding binder, stirring at 50 deg.C for 5-10 mm, adding disperser, and stirring at 50 deg.CStirring and refluxing for 5 min-10 mim under the condition of casting, then adding Al2O3Powder is refluxed for 2 to 2.5 hours in water bath at the temperature of 50 ℃ under the stirring condition, and naturally cooled to room temperature to obtain Al2O3Sizing agent; the Al is2O3Al in the slurry2O3The mass fraction of (A) is 10-30%; the quality of the binder and the Al prepared in the first step2O3Sol and Al added in step two2O3The ratio of the total mass of the powder is 1 (65-70); the dispersant and Al2O3Al in the slurry2O3The mass ratio of (1) to (20-25);
thirdly, directional freezing: al prepared in the second step2O3Placing the slurry into a polytetrafluoroethylene mold, performing directional freezing at minus 40-minus 80 ℃ by using directional freezing equipment, then placing the slurry into a freeze dryer, and performing drying treatment for 48-75 h under the conditions of vacuum and temperature of minus 50-minus 70 ℃ to obtain Al with a directional pore structure2O3A template;
fourthly, preparing the composite phase-change material: al with oriented pore structure prepared by organic phase change material and step three2O3The template adopts a melting dipping method to prepare the composite phase-change material.
Al in step two of the present invention2O3Al in the slurry2O3Is composed of two parts, one part is Al added in the second step2O3Powder, another part of Al prepared in step one2O3Al in sol2O3(ii) a Wherein Al prepared in the first step2O3Al in sol2O3The molar amount of the Al element (B) is the same as the molar amount of the Al element in the aluminum sec-butoxide added in the first step.
Al prepared by the invention2O3The aperture of the template is small, so that physical packaging of the phase change material can be well realized; al prepared by the invention2O3The pore diameter distribution in the template is uniform, and the formed composite phase change material has good uniformity; al (Al)2O3Template growth along ice crystalsThe directional through hole structure is arranged in the direction, so that the phenomenon of spalling cannot occur in the dipping process, and the formed composite phase-change material does not have a hole wall-phase-change material interface in the heat transfer process in the direction, so that the composite phase-change material has better heat conductivity; al (Al)2O3The template wall contains hydroxyethyl cellulose, has certain elasticity, and the increase of the volume does not cause the fracture of the structure in the solid-liquid phase change process.
The invention adopts the freezing injection molding to prepare the Al with the directional hole structure2O3And (3) completing impregnation of the phase-change material by adopting a melting impregnation process. Experimental results prove that the Al prepared by the invention2O3The template has good packaging performance, and the prepared composite phase change material has high energy storage density.
Al of the invention2O3The template has a directional via structure along the "ice crystal" growth direction.
Al with directional pore structure prepared in step three of the invention2O3The density of the template is 0.2043 +/-0.0059 g/cm3(ii) a Testing of Al by mercury intrusion2O3The porosity of the template was 94.36%, and the specific surface area was 0.388m2In terms of a/g, the mode and mean values of the pore diameters were 45.36 μm and 46.83. mu.m, respectively.
For Al by transient planar heat source method2O3The thermal conductivity of the template in different directions is tested, and the result shows that the thermal conductivity along the growth direction of the ice crystal is 0.09517W/(m.K), the thermal conductivity perpendicular to the growth direction of the ice crystal is 0.07691W/(m.K), and the template has certain anisotropy.
Drawings
FIG. 1 shows Al with a directional pore structure prepared in the third step of this experiment2O3SEM scan of the cross section of (a);
FIG. 2 shows Al with a directional pore structure prepared in the third step of this experiment2O3SEM scan of the cross section of (a);
FIG. 3 shows Al with a directional pore structure prepared in the third step of this experiment2O3SEM scan of the side of (1);
FIG. 4 shows Al with a directional pore structure prepared in the third step of this experiment2O3SEM scan of the side of (1);
FIG. 5 is an SEM scan of a cross-section of a composite phase change material prepared in this experiment;
FIG. 6 is a SEM scan of the side of the composite phase change material prepared in this experiment;
FIG. 7 is an infrared spectrum;
FIG. 8 is a DSC-TG analysis curve.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a composite phase change energy storage material with an organic matter filled ordered pore alumina template, which is specifically carried out according to the following steps:
firstly, preparing Al2O3Sol: dissolving aluminum sec-butoxide in water to obtain a mixed solution, refluxing for 1-1.5 h under the conditions of 90-95 ℃ water bath and stirring, then adding dilute nitric acid, continuously refluxing for 9h under the conditions of 90-95 ℃ water bath and stirring, and naturally cooling to room temperature to obtain Al2O3Sol; the molar ratio of the aluminum sec-butoxide to the water is 1 (60-100); the mass concentration of the dilute nitric acid is 65-68 percent; the volume ratio of the dilute nitric acid to the mixed solution is 1 (50-55);
secondly, preparing ceramic slurry: al prepared in the first step2O3Refluxing the sol at 50 deg.C for 10 min-30 min, adding binder, stirring at 50 deg.C for 5 min-10 mm, adding disperser, stirring at 50 deg.C for 5 min-10 mm, adding Al2O3Powder is refluxed for 2 to 2.5 hours in water bath at the temperature of 50 ℃ under the stirring condition, and naturally cooled to room temperature to obtain Al2O3Sizing agent; the Al is2O3Al in the slurry2O3The mass fraction of (A) is 10-30%; the quality of the binder and the Al prepared in the first step2O3Sol and Al added in step two2O3The ratio of the total mass of the powder is 1 (65-70); the dispersant and Al2O3Al in the slurry2O3The mass ratio of (1) to (20-25);
thirdly, directional freezing: al prepared in the second step2O3Placing the slurry into a polytetrafluoroethylene mold, performing directional freezing at minus 40-minus 80 ℃ by using directional freezing equipment, then placing the slurry into a freeze dryer, and performing drying treatment for 48-75 h under the conditions of vacuum and temperature of minus 50-minus 70 ℃ to obtain Al with a directional pore structure2O3A template;
fourthly, preparing the composite phase-change material: al with oriented pore structure prepared by organic phase change material and step three2O3The template adopts a melting dipping method to prepare the composite phase-change material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the binder in the second step is hydroxyethyl cellulose. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the dispersant in the second step is cetyl trimethyl ammonium bromide. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the melting point of the organic phase change material in the fourth step is less than 120 ℃. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the organic phase change material in the fourth step is one or a mixture of more of acetic acid, lauric acid, n-tetradecanoic acid, stearic acid, tetradecane, heptadecane, eicosane, octacosane, n-tridecanol, n-tetradecanol, n-hexadecanol, xylitol, d-sorbitol, meso-erythritol and paraffin. The rest is the same as one of the first to fourth embodiments.
The invention was verified with the following tests:
test one: the test is a preparation method of the composite phase change energy storage material with the ordered pore alumina template filled with organic matters, and the preparation method is specifically carried out according to the following steps:
firstly, preparing Al2O3Sol: dissolving aluminum sec-butoxide in water to obtain a mixed solution, refluxing for 1h under the conditions of 90 ℃ water bath and stirring, adding dilute nitric acid, continuously refluxing for 9h under the conditions of 90 ℃ water bath and stirring, and naturally cooling to room temperature to obtain Al2O3Sol; the molar ratio of the aluminum sec-butoxide to the water is 1: 60; the mass concentration of the dilute nitric acid is 65-68 percent; the volume ratio of the dilute nitric acid to the mixed solution is 1: 50;
secondly, preparing ceramic slurry: al prepared in the first step2O3Refluxing the sol at 50 deg.C for 10min, adding binder, stirring and refluxing at 50 deg.C for 5min, adding dispersant, stirring and refluxing at 50 deg.C for 5min, and adding Al2O3Refluxing the powder for 2h in a water bath at 50 ℃ under stirring, and naturally cooling to room temperature to obtain Al2O3Sizing agent; the Al is2O3Al in the slurry2O3The mass fraction of (A) is 15%; the quality of the binder and the Al prepared in the first step2O3Sol and Al added in step two2O3The total mass ratio of the powder is 1: 66.7; the dispersant and Al2O3Al in the slurry2O3In a mass ratio of 1: 20; the binder in the second step is hydroxyethyl cellulose; the dispersant in the second step is hexadecyl trimethyl ammonium bromide;
thirdly, directional freezing: al prepared in the second step2O3Placing the slurry into a polytetrafluoroethylene mold, performing directional freezing at-70 deg.C with directional freezing equipment, placing into a freeze dryer, and drying at-60 deg.C under vacuum for 72h to obtain Al with directional pore structure2O3A template;
fourthly, preparing the composite phase-change material: heating xylitol to 120 ℃ to melt, maintaining the temperature at 120 ℃, and carrying out step three to prepare Al with an oriented pore structure2O3The template is immersed in molten xylitol, Al2O3Form panelCompletely immersing in molten xylitol to obtain the finished product, pouring out molten liquid, and retaining Al2O3And naturally cooling the template to room temperature to obtain the composite phase-change material.
Al with directional pore structure prepared in the third test step2O3The density of the template is 0.2043 +/-0.0059 g/cm3(ii) a Testing of Al by mercury intrusion2O3The porosity of the template was 94.36%, and the specific surface area was 0.388m2In terms of a/g, the mode and mean values of the pore diameters were 45.36 μm and 46.83. mu.m, respectively.
The Al prepared in the third step of the test is subjected to the transient plane heat source method2O3The thermal conductivity of the template in different directions is tested, and the result shows that the thermal conductivity along the growth direction of the ice crystal is 0.09517W/(m.K), the thermal conductivity perpendicular to the growth direction of the ice crystal is 0.07691W/(m.K), and the template has certain anisotropy.
FIGS. 1 and 2 show Al with a directional pore structure prepared in step three of this experiment2O3SEM scanning photograph of the cross section of (1), and FIGS. 3 and 4 are the Al with oriented pore structure prepared in the third experimental step2O3From the SEM scanning photograph of the side of the aluminum oxide template, the oriented porous structure of the aluminum oxide template can be observed, and the pore size of the template is preliminarily obtained to be about 50 μm.
The density of the composite phase-change material prepared by the test is 1.4446 +/-0.0551 g/cm3Wherein the mass fraction of the xylitol is 86.36% +/-0.28%.
Fig. 5 is an SEM scanning photograph of a cross section of the composite phase change material prepared in the present experiment, and fig. 6 is an SEM scanning photograph of a side surface of the composite phase change material prepared in the present experiment, in which a pore structure is not observed, and a pore wall trace of the alumina template can be seen from the side surface view, indicating that the alumina template is completely filled with xylitol.
FIG. 7 is an infrared spectrum, in which curve 1 is the composite phase change material prepared in this test, curve 2 is xylitol, and curve 3 is Al with directional pore structure prepared in step three of this test2O3And the test result shows that: in this test xylitol was successfully impregnated with Al2O3Among the templates.
FIG. 8 is a DSC-TG analysis curve, curve 1 is a DSC curve of xylitol, and the melting point of the xylitol obtained after data processing is 91.08 ℃, and the latent heat of phase change is 180 kJ/kg. The curve 3 is the mass change curve of the xylitol between 30 ℃ and 120 ℃, and the curve shows that the xylitol has good stability in the temperature range; the curve 2 is a DSC curve of the composite phase change material prepared in the test, and the composite phase change material obtained after data processing has a melting point of 91.50 ℃, latent heat of phase change of 151kJ/kg and very high heat storage density; the curve 4 is the mass change curve of the composite phase change material prepared by the test at 30-120 ℃, and the curve shows that the composite phase change material has good stability in the temperature range. Curves 1 and 2 are endothermic peaks.
Claims (5)
1. A preparation method of a composite phase change energy storage material with an ordered pore alumina template filled with organic matter is characterized in that the preparation method of the composite phase change energy storage material with the ordered pore alumina template filled with organic matter is carried out according to the following steps:
firstly, preparing Al2O3Sol: dissolving aluminum sec-butoxide in water to obtain a mixed solution, refluxing for 1-1.5 h under the conditions of 90-95 ℃ water bath and stirring, then adding dilute nitric acid, continuously refluxing for 9h under the conditions of 90-95 ℃ water bath and stirring, and naturally cooling to room temperature to obtain Al2O3Sol; the molar ratio of the aluminum sec-butoxide to the water is 1 (60-100); the mass concentration of the dilute nitric acid is 65-68 percent; the volume ratio of the dilute nitric acid to the mixed solution is 1 (50-55);
secondly, preparing ceramic slurry: al prepared in the first step2O3Refluxing the sol at 50 deg.C for 10 min-30 min, adding binder, stirring at 50 deg.C for 5 min-10 mm, adding disperser, stirring at 50 deg.C for 5 min-10 mm, adding Al2O3Powder is refluxed for 2 to 2.5 hours in water bath at the temperature of 50 ℃ under the stirring condition, and naturally cooled to room temperature to obtain Al2O3Sizing agent; the Al is2O3Al in the slurry2O3The mass fraction of (A) is 10-30%; the quality of the binder and the Al prepared in the first step2O3Sol and Al added in step two2O3The ratio of the total mass of the powder is 1 (65-70); the dispersant and Al2O3Al in the slurry2O3The mass ratio of (1) to (20-25);
thirdly, directional freezing: al prepared in the second step2O3Placing the slurry into a polytetrafluoroethylene mold, performing directional freezing at minus 40-minus 80 ℃ by using directional freezing equipment, then placing the slurry into a freeze dryer, and performing drying treatment for 48-75 h under the conditions of vacuum and temperature of minus 50-minus 70 ℃ to obtain Al with a directional pore structure2O3A template;
fourthly, preparing the composite phase-change material: al with oriented pore structure prepared by organic phase change material and step three2O3The template adopts a melting dipping method to prepare the composite phase-change material.
2. The method for preparing the composite phase change energy storage material of the organic matter filled ordered pore alumina template according to claim 1, wherein the binder in the second step is hydroxyethyl cellulose.
3. The method for preparing the composite phase change energy storage material with the organic matter filled ordered pore alumina template according to claim 1, wherein the dispersant in the second step is cetyl trimethyl ammonium bromide.
4. The method for preparing the composite phase change energy storage material of the organic matter filled ordered pore alumina template according to claim 1, wherein the melting point of the organic phase change material in the fourth step is less than 120 ℃.
5. The method for preparing the composite phase change energy storage material filled with the ordered pore alumina template by the organic matters according to claim 1, wherein the organic phase change material in the fourth step is one or a mixture of more of acetic acid, lauric acid, n-tetradecanoic acid, stearic acid, tetradecane, heptadecane, eicosane, octacosane, n-tridecanol, n-tetradecanol, n-hexadecanol, xylitol, d-sorbitol, meso-erythritol and paraffin.
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