CN101693823B - Method for preparing energy-storing materials through using phase-change materials to fill graphitized foam carbon - Google Patents

Method for preparing energy-storing materials through using phase-change materials to fill graphitized foam carbon Download PDF

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CN101693823B
CN101693823B CN2009103089092A CN200910308909A CN101693823B CN 101693823 B CN101693823 B CN 101693823B CN 2009103089092 A CN2009103089092 A CN 2009103089092A CN 200910308909 A CN200910308909 A CN 200910308909A CN 101693823 B CN101693823 B CN 101693823B
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phase change
change material
fill
energy storage
storage material
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CN101693823A (en
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史丽萍
钟业盛
赫晓东
李明伟
何飞
胡守亮
隋超
骆峰生
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Harbin Institute of Technology
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Abstract

A method for preparing energy-storing materials through using phase-change materials to fill graphitized foam carbon relates to the method for preparing energy-storing materials. The method solves the problems of existing heat-storing materials that the thermal coefficient is low, the heat-storing intensity is small and the performance is unstable. The method of the invention comprises: respectively feeding hydrochloric acid and ammonia into mixing solution of Al(NO3)3.9H2O, deionized water and absolute ethyl alcohol for obtaining Al2O3 colloidal sol, dipping LiF-CaF2 phase-change materials into the Al2O3 colloidal sol for obtaining alcogel through separation by ultrasonic, dipping the alcogel into aging solution for obtaining Al2O3 sol gel, dipping graphitized foam carbon into the Al2O3 sol gel, and drying the carbon until the weight loss is not more than 0.5%/hour-1%/hour, namely obtaining the energy-storing materials prepared through using the phase-change materials to fill graphitized foam carbon. The thermal coefficient of the energy-storing materials prepared through using the phase-change materials to fill graphitized foam carbon obtained in the invention is 15w/(m.K)-20 w/(m.K).

Description

Fill the method that graphite bubble foam charcoal prepares energy storage material with phase change material
Technical field
The present invention relates to a kind of preparation method of energy storage material.
Background technology
Mainly there is two large problems in existing heat accumulating, and the one, thermal conductivity is low, is 0.20-0.24W/ (mK) as the thermal conductivity of paraffin; The 2nd, there is liquid flow phenomenon in the solid-liquid phase change process.In general, the method that improves the phase-change heat-storage material thermal conductivity mainly comprises two kinds: the one, and in interchanger, adopt metal fin structure or honeycomb structure to expand heat interchanging area; The 2nd, in phase-change heat-storage material, add highly heat-conductive material, as thin metal strip, little metal ring, porous metal material, copper sheet and porous metal foam filler etc.Though these methods can both improve the heat conductivility of phase change material, but also increased the weight and volume of heat reservoir significantly, the storage density of heat reservoir also significantly reduces, and also there is corrodibility in the partial phase change material to metallic substance, has therefore limited its practical application.The method that solves liquid fluidity in the solid-liquid phase change process also comprises two kinds, the one, and preparation microcapsule phase-change heat accumulating is wrapped in phase change material in the microcapsule body that macromolecular material is a shell; The 2nd, phase change material and macromolecular material are carried out blended melting, phase change material is wrapped in the network structure of macromolecular material.Because the melt temperature of macromolecular material is higher than the transformation temperature of phase change material, so when solid-liquid phase change took place, macromolecular material still was in solid state, this phenomenon is also referred to as " typing phase change material ".Though these two kinds of methods can solve the liquid fluidity problem of phase change material, the thermal conductivity of macromolecular material is about 0.115-0.345W/ (mK), has further worsened the heat transfer property of phase change material again.Therefore how to prepare the thermal conductivity height, storage density is big and the New-type phase change heat accumulating of stable performance, has become the key of heat-storage technology practical application.
Summary of the invention
Technical problem to be solved by this invention is that existing heat accumulating thermal conductivity is low, storage density is little and the problem of unstable properties in order to solve, and provides a kind of and has filled the method that graphite bubble foam charcoal prepares energy storage material with phase change material.
The present invention is as follows with the method that phase change material filling graphite bubble foam charcoal prepares energy storage material: one, with Al (NO 3) 39H 2O, deionized water and absolute ethyl alcohol and stirring are mixed 10min～15min, obtain mixture, then mixture is adopted heating in water bath to 50 ℃～55 ℃, the hydrochloric acid that adds concentration again and be 0.2mol/L～0.3mol/L continues to react 10min～15min under 50 ℃～55 ℃ condition, drop to room temperature, add volumetric concentration again and be 98% ammoniacal liquor, reaction 10min～15min obtains Al 2O 3Colloidal sol; Two, with LiF-CaF 2Phase change material immerses Al 2O 3In the colloidal sol, be ultrasonic dispersing 20min～30min under the condition of 40KHz～50KHz at dispersion frequency then, obtain alcogel; Three, alcogel is soaked in the aged solution 24 hours under temperature is 50 ℃～55 ℃ condition, can obtains being wrapped in LiF CaF 2The Al of phase change material 2O 3Collosol and gel; Four, the greying Carbon foam is immersed in the described Al of step 3 2O 3In the collosol and gel 4 hours～6 hours, Al 2O 3The collosol and gel liquid level did not have greying Carbon foam 1mm～5mm, it is under 150 ℃～180 ℃ the condition dry 96 hours～100 hours in normal pressure, temperature then, until the weight loss amount be no more than 0.5%/hour～1%/hour, stop drying, promptly handy phase change material is filled the energy storage material of graphite bubble foam charcoal preparation; Al (NO in the step 1 3) 39H 2The mol ratio of O, deionized water, dehydrated alcohol, hydrochloric acid and strong aqua is 1: 3.85: 10: 8.5 * 10 -4: 0.0325; The described LiF-CaF of step 2 2Phase change material LiF and CaF 2By 3～8: 12 mass ratio mixes; Aged solution described in the step 3 is that the tetraethyl orthosilicate volumetric concentration is 65%～70% tetraethyl orthosilicate ethanolic soln; LiF CaF described in the step 1 2The phase change material particle diameter is 30 μ m～50 μ m; The mean pore size of the Carbon foam of greying described in the step 4 is 500 μ m～600 μ m, and porosity is 70～90%.
According to the fourier heat conduction differential equation, any continuous solid body is had:
ρ R c R ∂ T R ∂ t = ▿ . ( K R ▿ T R ) + q · - - - ( 1 )
For the phase change material that solid-liquid phase change takes place, its energy equation can be written as
ϵ ( ρc ) PCM ∂ T PCM ∂ t + ρ PCM Lϵ df dt = ▿ . ( K eff ▿ T PCM ) + h sf a sf ( T s - T PCM ) - - - ( 2 )
First of the left end of equation (2)
Figure G200910308909220091028D000023
For the interior of phase change material can increase item, second of the left end of equation (2)
Figure G200910308909220091028D000024
Be phase-change accumulation energy, these two energy increments that characterized phase change material from macroscopic view.First of the right-hand member of equation (2)
Figure G200910308909220091028D000025
Be net heat conduction heat, second is h Sfa Sf(T 1-T PCM) heat that contacts of Carbon foam framework material and phase change material.
Because the high heat conductance of greying Carbon foam, so the handy phase change material of the present invention institute is filled the net heat conductance K of the energy storage material that graphite bubble foam charcoal prepares EffBigger, thus the clean conduction heat that imports phase change material into will increase greatly, and the three-dimensional net structure that the greying Carbon foam is exclusive has enlarged a of thermal source and phase change material SfThe ability that (the interface contact area of unit volume), so the contacting heat and also will obtain increasing of Carbon foam framework material and phase change material, this hot merit can material shift heat fast also is improved.
The greying Carbon foam is a kind of by the interconnected network structure of graphite tape crystal, has light weight, high heat conduction, high conduction, thermal expansivity is low and three-dimensional isotropic characteristic.Filled high-temperature phase change material in the hole of this material has realized adopting the rigidity encapsulation of graphite foam to phase change material, makes it have the double characteristic of quick transmission heat and increase self thermal capacitance concurrently.The energy storage material with the preparation of phase change material filling graphite bubble foam charcoal of gained of the present invention can be worked under 1300 ℃～2200 ℃ hot environment, by adjusting LiF and CaF 2Proportion of composing, its phase transition temperature interval is 680 ℃～720 ℃; Gained energy storage material thermal conductivity of the present invention is 15w/ (mK)～20w/ (mK), has bigger macroscopical thermal conductivity, has realized the quick response to heat energy, has avoided protected object surface superheated phenomenon.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: filling graphite bubble foam charcoal with phase change material in the present embodiment, to prepare the method for energy storage material as follows: one, with Al (NO 3) 39H 2O, deionized water and absolute ethyl alcohol and stirring are mixed 10min～15min, obtain mixture, then mixture is adopted heating in water bath to 50 ℃～55 ℃, the hydrochloric acid that adds concentration again and be 0.2mol/L～0.3mol/L continues to react 10min～15min under 50 ℃～55 ℃ condition, drop to room temperature, add volumetric concentration again and be 98% ammoniacal liquor, reaction 10min～15min obtains Al 2O 3Colloidal sol; Two, with LiF CaF 2Phase change material immerses Al 2O 3In the colloidal sol, be ultrasonic dispersing 20min～30min under the condition of 40KHz～50KHz at dispersion frequency then, obtain alcogel; Three, alcogel is soaked in the aged solution 24 hours under temperature is 50 ℃～55 ℃ condition, can obtains being wrapped in LiF-CaF 2The Al of phase change material 2O 3Collosol and gel; Four, the greying Carbon foam is immersed in the described Al of step 3 2O 3In the collosol and gel 4 hours～6 hours, Al 2O 3The collosol and gel liquid level did not have greying Carbon foam 1mm～5mm, it is under 150 ℃～180 ℃ the condition dry 96 hours～100 hours in normal pressure, temperature then, until the weight loss amount be no more than 0.5%/hour～1%/hour, stop drying, promptly handy phase change material is filled the energy storage material of graphite bubble foam charcoal preparation; Al (NO in the step 1 3) 39H 2The mol ratio of O, deionized water, dehydrated alcohol, hydrochloric acid and strong aqua is 1: 3.85: 10: 8.5 * 10 -4: 0.0325; The described LiF-CaF of step 2 2Phase change material LiF and CaF 2By 3～8: 12 mass ratio mixes; Aged solution described in the step 3 is that the tetraethyl orthosilicate volumetric concentration is 65%～70% tetraethyl orthosilicate ethanolic soln.
The energy storage material with the preparation of phase change material filling graphite bubble foam charcoal of present embodiment gained can be worked under 1300 ℃～2200 ℃ hot environment, by adjusting LiF and CaF 2Proportion of composing, its phase transition temperature interval is 680 ℃～720 ℃; Gained energy storage material thermal conductivity of the present invention is 15w/ (mK)～20w/ (mK), has bigger macroscopical thermal conductivity, has realized the quick response to heat energy, has avoided protected object surface superheated phenomenon.Present embodiment the handy phase change material energy storage material main component of filling the preparation of graphite bubble foam charcoal be C (skeleton), Al 2O 3(ceramic case) and LiF-CaF 2Mixture.
Embodiment two: present embodiment and embodiment one are different is that the mean pore size of the Carbon foam of greying described in the step 4 is 500 μ m～600 μ m, and porosity is 70%～90%.Other is identical with embodiment one.
The energy storage material with the preparation of phase change material filling graphite bubble foam charcoal of present embodiment gained can be worked under 1300 ℃～2200 ℃ hot environment, by adjusting LiF and CaF 2Proportion of composing, its phase transition temperature interval is 680 ℃～720 ℃; Gained energy storage material thermal conductivity of the present invention is 16w/ (mK)～19w/ (mK), has bigger macroscopical thermal conductivity, has realized the quick response to heat energy, has avoided protected object surface superheated phenomenon.Present embodiment the handy phase change material energy storage material main component of filling the preparation of graphite bubble foam charcoal be C (skeleton), Al 2O 3(ceramic case) and LiF-CaF 2Mixture.Embodiment three: present embodiment is different with embodiment one or two is in the step 1 mixture to be adopted heating in water bath to 51 ℃～54 ℃.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different with embodiment one or two is in the step 1 mixture to be adopted heating in water bath to 53 ℃.Other is identical with embodiment one or two.
Embodiment five: present embodiment and embodiment three are different is that the concentration of hydrochloric acid in the step 1 is 0.25mol/L.Other is identical with embodiment three.
Embodiment six: what present embodiment and embodiment one, two or five were different is that the step 3 aged solution is that the tetraethyl orthosilicate volumetric concentration is 66%～69% tetraethyl orthosilicate ethanolic soln.Other is identical with embodiment one, two or five.
Embodiment seven: what present embodiment and embodiment one, two or five were different is that the step 3 aged solution is that the tetraethyl orthosilicate volumetric concentration is 68% tetraethyl orthosilicate ethanolic soln.Other is identical with embodiment one, two or five.
Embodiment eight: present embodiment and embodiment six are different is in the step 3 alcogel to be soaked under temperature is 51 ℃～54 ℃ condition in the aged solution 24 hours.Other is identical with embodiment six.
Embodiment nine: present embodiment and embodiment six are different is in the step 3 alcogel to be soaked under temperature is 53 ℃ condition in the aged solution 24 hours.Other is identical with embodiment six.
Embodiment ten: present embodiment and embodiment one, two, five or eight are different is that drying temperature in the step 4 is 160 ℃.Other is identical with embodiment one, two, five or eight.
Embodiment 11: that present embodiment and embodiment one to ten are different is the LiF-CaF described in the step 1 2The phase change material particle diameter is 30 μ m～50 μ m.Other is identical with embodiment one to ten.

Claims (10)

1. fill the method that graphite bubble foam charcoal prepares energy storage material with phase change material, it is characterized in that filling graphite bubble foam charcoal with phase change material, to prepare the method for energy storage material as follows: one, with Al (NO 3) 39H 2O, deionized water and absolute ethyl alcohol and stirring are mixed 10min～15min, obtain mixture, then mixture is adopted heating in water bath to 50 ℃～55 ℃, the hydrochloric acid that adds concentration again and be 0.2mol/L～0.3mol/L continues to react 10min～15min under 50 ℃～55 ℃ condition, drop to room temperature, add volumetric concentration again and be 98% strong aqua, reaction 10min～15min obtains Al 2O 3Colloidal sol; Two, with LiF-CaF 2Phase change material immerses Al 2O 3In the colloidal sol, be ultrasonic dispersing 20min～30min under the condition of 40KHZ～50KHZ at dispersion frequency then, obtain alcogel; Three, alcogel is soaked in the aged solution 24 hours under temperature is 50 ℃～55 ℃ condition, can obtains being wrapped in LiF-CaF 2The Al of phase change material 2O 3Collosol and gel; Four, the greying Carbon foam is immersed in the described Al of step 3 2O 3In the collosol and gel 4 hours～6 hours, Al 2O 3The collosol and gel liquid level did not have greying Carbon foam 1mm～5mm, it is under 150 ℃～180 ℃ the condition dry 96 hours～100 hours in normal pressure, temperature then, until the weight loss amount be no more than 0.5%/hour～1%/hour, stop drying, promptly handy phase change material is filled the energy storage material of graphite bubble foam charcoal preparation; Al (NO in the step 1 3) 39H 2The mol ratio of O, deionized water, dehydrated alcohol, hydrochloric acid and strong aqua is 1: 3.85: 10: 8.5 * 10 -4: 0.0325; The described LiF-CaF of step 2 2Phase change material LiF and CaF 2By 3～8: 12 mass ratio mixes; Aged solution described in the step 3 is that the tetraethoxy volumetric concentration is 65%～70% tetraethoxy ethanolic soln.
2. according to claim 1ly fill the method that graphite bubble foam charcoal prepares energy storage material with phase change material, the mean pore size that it is characterized in that the Carbon foam of greying described in the step 4 is 500 μ m～600 μ m, and porosity is 70%～90%.
3. according to claim 1 and 2ly fill the method that graphite bubble foam charcoal prepares energy storage material, it is characterized in that in the step 1 mixture adopted heating in water bath to 51 ℃～54 ℃ with phase change material.
4. according to claim 1 and 2ly fill the method that graphite bubble foam charcoal prepares energy storage material, it is characterized in that in the step 1 mixture adopted heating in water bath to 53 ℃ with phase change material.
5. according to claim 3ly fill the method that graphite bubble foam charcoal prepares energy storage material with phase change material, the concentration that it is characterized in that hydrochloric acid in the step 1 is 0.25mol/L.
6. describedly fill the method that graphite bubble foam charcoal prepares energy storage material according to claim 1,2 or 5, it is characterized in that the step 3 aged solution is that the tetraethoxy volumetric concentration is 66%～69% tetraethoxy ethanolic soln with phase change material.
7. describedly fill the method that graphite bubble foam charcoal prepares energy storage material according to claim 1,2 or 5, it is characterized in that the step 3 aged solution is that the tetraethoxy volumetric concentration is 68% tetraethoxy ethanolic soln with phase change material.
8. according to claim 6ly fill the method that graphite bubble foam charcoal prepares energy storage material, it is characterized in that in the step 3 alcogel was soaked under temperature is 51 ℃～54 ℃ condition in the aged solution 24 hours with phase change material.
9. according to claim 6ly fill the method that graphite bubble foam charcoal prepares energy storage material, it is characterized in that in the step 3 alcogel was soaked under temperature is 53 ℃ condition in the aged solution 24 hours with phase change material.
10. describedly fill the method that graphite bubble foam charcoal prepares energy storage material according to claim 1,2,5 or 8, it is characterized in that the LiF-CaF described in the step 2 with phase change material 2The phase change material particle diameter is 30 μ m～50 μ m.
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CN108587576B (en) * 2018-07-23 2020-10-30 淄博职业学院 Heat-conducting silicone grease for computer heat dissipation and preparation method thereof
CN109321211B (en) * 2018-10-19 2021-04-27 福州大学 Graphitized hierarchical porous carbon composite phase-change energy storage material and preparation method thereof
CN109855163A (en) * 2019-03-04 2019-06-07 孙铮 Passively with active convolution building energy conservation sub-controlling unit
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