CN108531141A - A kind of organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template - Google Patents
A kind of organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template Download PDFInfo
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Abstract
A kind of organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template, it is related to a kind of preparation method of composite phase-change energy storage material.Random orientation is presented the present invention is to solve the pore-size distribution of existing inorganic porous material and is easy to happen spalling phenomenon in dipping process, the composite phase-change material uniformity for adsorbing formation is poor, the low technical problem of thermal conductivity.The present invention：One, Al is prepared2O3Colloidal sol；Two, ceramic slurry is prepared；Three, orientation freezing；Four, composite phase-change material is prepared.The present invention is prepared for a kind of Al with orientation pore structure using freezing casting2O3Template, and use melt impregnating process completes the dipping of phase-change material.The results show, Al prepared by the present invention2O3There is template good encapsulation performance, the composite phase-change material of preparation to have higher energy storage density.
Description
Technical field
The present invention relates to a kind of preparation methods of composite phase-change energy storage material.
Background technology
The significant advantage that phase-change accumulation energy has storage density high, the utilization ratio for improving the energy are of great significance.
In practical applications, phase-changing energy storage material is easy to happen liquid leakage problems during solid-liquid phase change.For leakage problems,
There are three types of main solutions：First, phase-changing energy storage material is adsorbed in inorganic porous material and forms composite phase-change material
Material；Second, phase-changing energy storage material is wrapped in the microcapsules of organic polymer formation；Third, by phase-change material and high score
Sub- Material cladding is prepared into polymer-based composite setting phase-change material.For first method, common inorganic porous material has
Carbon foam (carbon foam), diatomite (diatomite), montmorillonite (montmorillonoid) etc..These are inorganic porous
Random orientation is often presented in the pore-size distribution of material, in dipping process, is easy to happen spalling phenomenon, adsorbs the compound phase of formation
It is poor to become material homogeneity, in heat transfer process, constantly to pass through the boundary that phase-change material is formed with inorganic porous material
Face reduces thermal conductivity.
Freezing injection molding and forming technology basic principle be：Slurry is placed on a plane low-temperature receiver, low-temperature receiver can be in slurry
Inside forms the temperature gradient of an orientation, and solvent can be oriented solidification along the direction of temperature gradient, be formed " ice crystal ", so
Afterwards by the way of vacuum freeze drying, make solvent directly from solid state sublimation to gaseous state, forms pore structure, and solute is then formed
Hole wall.
Invention content
The present invention is to solve the pore-size distributions of existing inorganic porous material, and random orientation is presented, in dipping process,
It is easy to happen spalling phenomenon, the composite phase-change material uniformity for adsorbing formation is poor, the low technical problem of thermal conductivity, and provides one
Kind organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template.
The preparation method of the organic matter composite phase-change energy storage material of filling orderly porous aluminum oxide template of the present invention be by with
What lower step carried out：
One, Al is prepared2O3Colloidal sol：Aluminium secondary butylate is dissolved in water, mixed solution is obtained, in 90 DEG C~95 DEG C water-baths and
Flow back 1h~1.5h under stirring condition, and dust technology is then added, and continues the 9h that flows back under 90 DEG C~95 DEG C water-baths and stirring condition,
Cooled to room temperature obtains Al2O3Colloidal sol；The molar ratio of the aluminium secondary butylate and water is 1:(60~100)；Described is dilute
The mass concentration of nitric acid is 65%~68%；The volume ratio of the dust technology and mixed solution is 1:(50~55)；
Two, ceramic slurry is prepared：Al prepared by step 12O3Colloidal sol flows back 10min~30min under the conditions of 50 DEG C, adds
Enter binder, be stirred at reflux 5min~10mim under the conditions of 50 DEG C, add dispersant, is stirred at reflux under the conditions of 50 DEG C
5min~10mim adds Al2O3Powder, then flow back under 50 DEG C of water-baths and stirring condition 2h~2.5h, naturally cools to
Room temperature obtains Al2O3Slurry；The Al2O3Al in slurry2O3Mass fraction be 10%~30%；The binder
The Al that quality is prepared with step 12O3The Al being added in colloidal sol and step 22O3The ratio of the gross mass of powder is 1:(65~70)；
The dispersant and Al2O3Al in slurry2O3Mass ratio be 1:(20~25)；
Three, orientation freezing：Al prepared by step 22O3Slurry is put into Teflon mould, is set with orientation freezing
It is standby to be oriented freezing at subzero 40~subzero 80 DEG C, it is then placed in freeze drier, is subzero 50 DEG C in vacuum and temperature
~it is 70 DEG C subzero under conditions of be dried processing 48h~75h, obtain with orientation pore structure Al2O3Template；
Four, composite phase-change material is prepared：The Al with orientation pore structure prepared with organic phase change material and step 32O3
Template prepares composite phase-change material using melt impregnation.
Al in step 2 of the present invention2O3Al in slurry2O3Consist of two parts, a part is added in step 2
Al2O3Powder, another part are the Al prepared in step 12O3Al in colloidal sol2O3；Wherein, the Al prepared in step 12O3It is molten
Al in glue2O3Al elements mole and step 1 in Al elements in the aluminium secondary butylate that is added mole it is identical.
Al prepared by the present invention2O3Pore size of template is smaller, can be very good to realize the physical package to phase-change material；This
The prepared Al of invention2O3The composite phase-change material uniformity of even aperture distribution in template, formation is fine；Al2O3Template along
There is the through-hole structure of orientation on ice-crystal growth direction, spalling phenomenon, and the composite phase-change formed will not occur in dipping process
Hole wall-phase-change material interface is not present in the diabatic process of the direction in material, has the preferable capacity of heat transmission；Al2O3Template
Contain hydroxyethyl cellulose in wall, there is certain elasticity, during solid-liquid phase change, the increase of volume can't cause to tie
The rupture of structure.
The present invention is prepared for a kind of Al with orientation pore structure using freezing casting2O3Template, and using melting leaching
Stain technique completes the dipping of phase-change material.The results show, Al prepared by the present invention2O3Template has good encapsulation
Can, the composite phase-change material of preparation has higher energy storage density.
The Al of the present invention2O3Template is along the through-hole structure in " ice crystal " direction of growth with orientation.
The Al with orientation pore structure prepared by step 3 of the present invention2O3Template density is 0.2043 ± 0.0059g/cm3；
Pass through Mercury-injection test Al2O3The porosity of template is 94.36%, specific surface area 0.388m2/ g, the most probable value peace in aperture
Mean value is respectively 45.36 μm and 46.83 μm.
By Adsorbent By Using Transient Plane Source Technique to Al2O3The thermal conductivity of template different directions is tested, the results showed that, along
The thermal conductivity in ice-crystal growth direction is 0.09517W/ (mK), is 0.07691W/ along the thermal conductivity perpendicular to ice-crystal growth direction
(mK), there is certain anisotropy.
Description of the drawings
Fig. 1 is the Al with orientation pore structure prepared by this test procedure three2O3Section SEM scanned photographs；
Fig. 2 is the Al with orientation pore structure prepared by this test procedure three2O3Section SEM scanned photographs；
Fig. 3 is the Al with orientation pore structure prepared by this test procedure three2O3Side SEM scanned photographs；
Fig. 4 is the Al with orientation pore structure prepared by this test procedure three2O3Side SEM scanned photographs；
Fig. 5 is the SEM scanned photographs in the section of composite phase-change material prepared by this experiment；
Fig. 6 is the SEM scanned photographs of the side of composite phase-change material prepared by this experiment；
Fig. 7 is infrared spectrogram；
Fig. 8 is that DSC-TG analyzes curve.
Specific implementation mode
Specific implementation mode one：Present embodiment is the composite phase-change storage that a kind of organic matter fills orderly porous aluminum oxide template
The preparation method of energy material, specifically carries out according to the following steps：
One, Al is prepared2O3Colloidal sol：Aluminium secondary butylate is dissolved in water, mixed solution is obtained, in 90 DEG C~95 DEG C water-baths and
Flow back 1h~1.5h under stirring condition, and dust technology is then added, and continues the 9h that flows back under 90 DEG C~95 DEG C water-baths and stirring condition,
Cooled to room temperature obtains Al2O3Colloidal sol；The molar ratio of the aluminium secondary butylate and water is 1:(60~100)；Described is dilute
The mass concentration of nitric acid is 65%~68%；The volume ratio of the dust technology and mixed solution is 1:(50~55)；
Two, ceramic slurry is prepared：Al prepared by step 12O3Colloidal sol flows back 10min~30min under the conditions of 50 DEG C, adds
Enter binder, be stirred at reflux 5min~10mim under the conditions of 50 DEG C, add dispersant, is stirred at reflux under the conditions of 50 DEG C
5min~10mim adds Al2O3Powder, then flow back under 50 DEG C of water-baths and stirring condition 2h~2.5h, naturally cools to
Room temperature obtains Al2O3Slurry；The Al2O3Al in slurry2O3Mass fraction be 10%~30%；The binder
The Al that quality is prepared with step 12O3The Al being added in colloidal sol and step 22O3The ratio of the gross mass of powder is 1:(65~70)；
The dispersant and Al2O3Al in slurry2O3Mass ratio be 1:(20~25)；
Three, orientation freezing：Al prepared by step 22O3Slurry is put into Teflon mould, is set with orientation freezing
It is standby to be oriented freezing at subzero 40~subzero 80 DEG C, it is then placed in freeze drier, is subzero 50 DEG C in vacuum and temperature
~it is 70 DEG C subzero under conditions of be dried processing 48h~75h, obtain with orientation pore structure Al2O3Template；
Four, composite phase-change material is prepared：The Al with orientation pore structure prepared with organic phase change material and step 32O3
Template prepares composite phase-change material using melt impregnation.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：Bonding described in step 2
Agent is hydroxyethyl cellulose.Other are same as the specific embodiment one.
Specific implementation mode three：The present embodiment is different from the first and the second embodiment in that：Described in step 2
Dispersant is cetyl trimethylammonium bromide.Other are the same as one or two specific embodiments.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：Institute in step 4
The fusing point for the organic phase change material stated is less than 120 DEG C.Other are identical as one of specific implementation mode one to three.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：Institute in step 4
The organic phase change material stated be acetic acid, lauric acid, positive tetradecylic acid, stearic acid, the tetradecane, heptadecane, eicosane, octacosane,
Positive tridecanol, tetradecanol, positive hexadecanol, xylitol, d- D-sorbites, one kind in meso-antierythrite and paraffin or
Several mixtures.Other are identical as one of specific implementation mode one to four.
The present invention is verified with following tests：
Experiment one：This experiment is a kind of preparation for the composite phase-change energy storage material that organic matter fills orderly porous aluminum oxide template
Method specifically carries out according to the following steps：
One, Al is prepared2O3Colloidal sol：Aluminium secondary butylate is dissolved in water, mixed solution is obtained, in 90 DEG C of water-baths and stirring bar
Flow back 1h under part, and dust technology is then added, and continues the 9h that flows back under 90 DEG C of water-baths and stirring condition, and cooled to room temperature obtains
To Al2O3Colloidal sol；The molar ratio of the aluminium secondary butylate and water is 1:60；The mass concentration of the dust technology be 65%~
68%；The volume ratio of the dust technology and mixed solution is 1:50；
Two, ceramic slurry is prepared：Al prepared by step 12O3Colloidal sol flows back 10min under the conditions of 50 DEG C, is added and bonds
Agent is stirred at reflux 5min under the conditions of 50 DEG C, adds dispersant, is stirred at reflux 5min under the conditions of 50 DEG C, adds Al2O3
Powder, then flow back under 50 DEG C of water-baths and stirring condition 2h, and cooled to room temperature obtains Al2O3Slurry；The Al2O3
Al in slurry2O3Mass fraction be 15%；The Al that the quality of the binder is prepared with step 12O3Colloidal sol and step 2
The Al of middle addition2O3The ratio of the gross mass of powder is 1:66.7；The dispersant and Al2O3Al in slurry2O3Mass ratio be
1:20；Binder described in step 2 is hydroxyethyl cellulose；Dispersant described in step 2 is cetyl trimethyl
Ammonium bromide；
Three, orientation freezing：Al prepared by step 22O3Slurry is put into Teflon mould, is set with orientation freezing
It is standby to be oriented freezing at subzero 70 DEG C, it is then placed in freeze drier, under conditions of vacuum and temperature are subzero 60 DEG C
Processing 72h is dried, obtains the Al with orientation pore structure2O3Template；
Four, composite phase-change material is prepared：Xylitol is heated to 120 DEG C to melt, temperature maintains 120 DEG C, will walk
Rapid three Al with orientation pore structure prepared2O3Template immerses in the xylitol of melting, Al2O3Template is completely immersed in melting
It is that dipping is completed in xylitol, molten liquid is poured out, Al is retained2O3Composite phase-change is made after cooled to room temperature in template
Material.
The Al with orientation pore structure prepared by this test procedure three2O3Template density is 0.2043 ± 0.0059g/cm3；
Pass through Mercury-injection test Al2O3The porosity of template is 94.36%, specific surface area 0.388m2/ g, the most probable value peace in aperture
Mean value is respectively 45.36 μm and 46.83 μm.
The Al by Adsorbent By Using Transient Plane Source Technique prepared by this test procedure three2O3The thermal conductivity of template different directions carries out
Test, the results showed that, the thermal conductivity along ice-crystal growth direction is 0.09517W/ (mK), along perpendicular to ice-crystal growth direction
Thermal conductivity be 0.07691W/ (mK), have certain anisotropy.
Fig. 1 and Fig. 2 is the Al with orientation pore structure prepared by this test procedure three2O3Section SEM scanned photographs,
Fig. 3 and Fig. 4 is the Al with orientation pore structure prepared by this test procedure three2O3Side SEM scanned photographs, the energy from figure
Observe the orienting stephanoporate structure of alumina formwork, and the aperture for tentatively obtaining template is about 50 μm.
The density of composite phase-change material prepared by this experiment is 1.4446 ± 0.0551g/cm3, the wherein quality of xylitol
Score is 86.36% ± 0.28%.
Fig. 5 is the SEM scanned photographs in the section of composite phase-change material prepared by this experiment, and Fig. 6 is answering for this experiment preparation
The SEM scanned photographs for closing the side of phase-change material do not observe pore structure from figure, and it can be seen that oxygen from side view
The hole wall trace for changing aluminum alloy pattern plate, illustrates that alumina formwork is filled by xylitol completely.
Fig. 7 is infrared spectrogram, and curve 1 is composite phase-change material prepared by this experiment, and curve 2 is xylitol, and curve 3 is
The Al with orientation pore structure prepared by this test procedure three2O3, test result shows：Xylitol successfully soaks in this experiment
Al is entered2O3In template.
Fig. 8 is that DSC-TG analyzes curve, and curve 1 is the DSC curve of xylitol, and the molten of xylitol is obtained after data processing
Point is 91.08 DEG C, latent heat of phase change 180kJ/kg.Curve 3 is mass-change curve of the xylitol between 30 DEG C~120 DEG C,
Curve shows that in this temperature range, xylitol has good stability；Curve 2 is composite phase-change material prepared by this experiment
DSC curve, it is 91.50 DEG C, latent heat of phase change 151kJ/kg that its fusing point is obtained after data processing, has very high heat accumulation close
Degree；Curve 4 is mass-change curve of the composite phase-change material of this experiment preparation between 30 DEG C~120 DEG C, and curve shows
In this temperature range, composite phase-change material has good stability.Curve 1 and curve 2 are endothermic peak.
Claims (5)
1. a kind of organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template, it is characterised in that have
The preparation method that machine object fills the composite phase-change energy storage material of orderly porous aluminum oxide template carries out according to the following steps：
One, Al is prepared2O3Colloidal sol：Aluminium secondary butylate is dissolved in water, mixed solution is obtained, in 90 DEG C~95 DEG C water-baths and stirring
Under the conditions of flow back 1h~1.5h, be then added dust technology, continuation flows back 9h under 90 DEG C~95 DEG C water-baths and stirring condition, natural
It is cooled to room temperature, obtains Al2O3Colloidal sol；The molar ratio of the aluminium secondary butylate and water is 1:(60~100)；The dust technology
Mass concentration be 65%~68%；The volume ratio of the dust technology and mixed solution is 1:(50~55)；
Two, ceramic slurry is prepared：Al prepared by step 12O3Colloidal sol flows back 10min~30min under the conditions of 50 DEG C, is added viscous
Tie agent, be stirred at reflux 5min~10mim under the conditions of 50 DEG C, add dispersant, be stirred at reflux under the conditions of 50 DEG C 5min~
10mim adds Al2O3Powder, then flow back under 50 DEG C of water-baths and stirring condition 2h~2.5h, and cooled to room temperature obtains
To Al2O3Slurry；The Al2O3Al in slurry2O3Mass fraction be 10%~30%；The quality and step of the binder
Rapid one Al prepared2O3The Al being added in colloidal sol and step 22O3The ratio of the gross mass of powder is 1:(65~70)；Point
Powder and Al2O3Al in slurry2O3Mass ratio be 1:(20~25)；
Three, orientation freezing：Al prepared by step 22O3Slurry is put into Teflon mould, is existed with orientation freezing equipment
Subzero 40~subzero 80 DEG C are oriented freezing, are then placed in freeze drier, are subzero 50 DEG C~zero in vacuum and temperature
Processing 48h~75h is dried under conditions of lower 70 DEG C, obtains the Al with orientation pore structure2O3Template；
Four, composite phase-change material is prepared：The Al with orientation pore structure prepared with organic phase change material and step 32O3Template
Composite phase-change material is prepared using melt impregnation.
2. a kind of organic matter according to claim 1 fills the system of the composite phase-change energy storage material of orderly porous aluminum oxide template
Preparation Method, it is characterised in that the binder described in step 2 is hydroxyethyl cellulose.
3. a kind of organic matter according to claim 1 fills the system of the composite phase-change energy storage material of orderly porous aluminum oxide template
Preparation Method, it is characterised in that the dispersant described in step 2 is cetyl trimethylammonium bromide.
4. a kind of organic matter according to claim 1 fills the system of the composite phase-change energy storage material of orderly porous aluminum oxide template
Preparation Method, it is characterised in that the fusing point of the organic phase change material described in step 4 is less than 120 DEG C.
5. a kind of organic matter according to claim 1 fills the system of the composite phase-change energy storage material of orderly porous aluminum oxide template
Preparation Method, it is characterised in that the organic phase change material described in step 4 is acetic acid, lauric acid, positive tetradecylic acid, stearic acid, 14
Alkane, eicosane, octacosane, positive tridecanol, tetradecanol, positive hexadecanol, xylitol, d- D-sorbites, interior disappears at heptadecane
The mixture of one or more of rotation-antierythrite and paraffin.
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Cited By (2)
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| CN110256103A (en) * | 2019-07-18 | 2019-09-20 | 覃向阳 | One method of porous alumina ceramics base phase becomes heat-insulation composite material |
| CN110372346A (en) * | 2019-07-18 | 2019-10-25 | 马桂明 | A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material |
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