CN106244118B - A kind of NaCl@Al of core-shell structure2O3The preparation method of high-temperature phase change heat accumulation material - Google Patents
A kind of NaCl@Al of core-shell structure2O3The preparation method of high-temperature phase change heat accumulation material Download PDFInfo
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- CN106244118B CN106244118B CN201610823261.2A CN201610823261A CN106244118B CN 106244118 B CN106244118 B CN 106244118B CN 201610823261 A CN201610823261 A CN 201610823261A CN 106244118 B CN106244118 B CN 106244118B
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Abstract
The present invention provides a kind of NaCl@Al of core-shell structure2O3The preparation method of high-temperature phase change heat accumulation material belongs to high efficiency of energy and utilizes and heat-storing material preparation field.It takes metal sodium salt and Metal aluminum salt to be dissolved in ethyl alcohol respectively first and solution is made, then Metal aluminum salt solution is instilled into the ethanol solution of metal sodium salt, the ethanol solution of surfactant and another Metal aluminum salt is added into mixed liquor again and is uniformly mixed, then NaOH ethanol solution is added into the above solidliquid mixture and obtains sediment, finally by the drying precipitate after cleaning, roasting to get the NaCl@Al for arriving core-shell structure2O3High-temperature phase change heat accumulation material.Firm Al2O3Shell wraps up the NaCl in kernel, and the disadvantage that the water decomposition of NaCl chance, corrosivity can be overcome strong enhances the stability of material；The phase transition temperature of NaCl is 801 DEG C, so that the heat-storing material can use in higher temperatures environment.
Description
Technical field
The present invention provides a kind of NaCl@Al of core-shell structure2O3The preparation method of high-temperature phase change heat accumulation material, belongs to the energy
Efficiently utilize and heat-storing material preparation field.
Background technique
The use of renewable energy is to solve the effective way of energy crisis and problem of environmental pollution in current global range.
In the energy such as solar energy, wind energy, water energy, biomass energy, nuclear energy, solar energy is abundant and can freely obtain, and has huge hair
Exhibition prospect.Currently, concentration solar generating (CSP) technology can convert solar energy into thermal energy and further by steam turbine or
Person's heat engine generates electricity, and has great advantage in substitution fossil energy or in terms of reducing carbon emission.However, solar energy itself
Unstability and the intermittent generated energy that will affect CSP system, so that the popularization and application of CSP technology are affected.
Thermal energy storage system (TES) can store thermal energy/cooling capacity, and the efficient utilization of thermal energy not only may be implemented,
CSP power plant can also be made more freely to operate, to solve energy resource supply and demand in time, temperature, electricity and place etc.
The mismatch problem of aspect.Research points out that the running temperature of CSP system is higher, and the thermal efficiency also increases.Therefore, only
Operating temperature is just able to satisfy the demand of the following CSP electricity generation system in the high-temperature phase change heat accumulation material of 500 ~ 1200 DEG C of ranges.
Summary of the invention
The present invention provides a kind of NaCl@Al for preparing core-shell structure2O3The method of high-temperature phase change heat accumulation material.The phase of NaCl
Temperature is 801 DEG C, can generate a large amount of heat content in phase transition process and heat accumulation is at low cost, in inorganic salts heat reservoir
Show absolute advantage.Al2O3As a kind of ceramic material, have very high fusing point (generally at 2000 DEG C or more) and excellent
NaCl phase-change material can be encapsulated by good stability at elevated temperature, and a kind of high-temperature heat accumulation material of core-shell structure is made.
The disadvantage that this structure can not only overcome NaCl corrosivity strong, and have and be capable of increasing heat transfer area, prevent phase-change material
The advantages that reacting with environment, controlling the volume change in phase transition process.
The invention is realized by the following technical scheme:
A kind of NaCl@Al preparing core-shell structure2O3The method of high-temperature phase change heat accumulation material, comprising the following steps:
(1) CH is weighed for 3:1 in molar ratio3COONa and AlCl3, it is dissolved in dehydrated alcohol respectively, it is made 0.05 ~
The CH of 0.6mol/L3COONa ethanol solution and AlCl3Ethanol solution；
(2) CH is vigorously stirred under 0 ~ 40 DEG C of water bath condition3COONa ethanol solution, while will with the speed of 3 ~ 5mL/min
AlCl3Ethanol solution instills CH3Continue 0.5 ~ 1.5h of stirring in COONa ethanol solution, after completion of dropwise addition, Nano grade is made
NaCl little particle；
(3) Surfactant CTAB ethanol solution, and another metal are sequentially added in the mixture obtained to step (2)
Aluminium salt ethanol solution, CTAB additive amount are 0.5 ~ 1g/L, Metal aluminum salt and CH3The molar ratio of COONa is 2 ~ 3:1, is uniformly mixed；
(4) NaOH is taken to be dissolved in the dehydrated alcohol (lower than 5 DEG C) refrigerated, NaOH and (AlCl3+ Metal aluminum salt) mole
Than for 2 ~ 3:1；While being vigorously stirred under 0 ~ 40 DEG C of water bath condition, with the speed of 0.5 ~ 5 drop per second by NaOH ethanol solution
It is added in the mixture of step (3), continues 1 ~ 2h of stirring after completion of dropwise addition, reaction is precipitated；
(5) precipitating for obtaining step (4) filters, and is washed 3 times with dehydrated alcohol, dry 12 at 80 ~ 120 DEG C ~ for 24 hours
Afterwards, 500 ~ 700 DEG C of 2 ~ 4h of roasting are warming up to the rate of 1 DEG C/min, obtain the NaCl@Al of core-shell structure2O3High-temperature phase change heat accumulation
Material.
Metal aluminum salt described in step (3) is aluminum acetate, eston, any one in aluminum nitrate.
The beneficial effects of the present invention are:
(1) use temperature≤300 DEG C of general middle low-temperature heat accumulating material, the heat-storing material is high using temperature, Ke Yi
It is used in 800 ~ 1400 DEG C of environment, it is easier to meet the industrial requirement of solar plant；
(2) the NaCl@Al of resulting core-shell structure2O3Phase change heat storage material is due to outer layer covers Al2O3, thus have
High temperature resistant (its fusing point is 2054 DEG C), thermal expansion coefficient is low (between 4.9 ~ 9.3 × 10-6/ K), the advantages that hardness is high；
(3) Al coated2O3The NaCl in kernel can be effectively protected in shell, avoid the loss and deep-etching of NaCl；
Al2O3It is highly stable ceramic material, which can effectively improve the thermal stability of material.
Specific embodiment
Embodiment 1
(1) 0.03mol(2.46g is weighed) CH3COONa and 0.01mol(2.4143g) AlCl3·6H2O is dissolved in 50mL respectively
In dehydrated alcohol, solution is configured to after ultrasound, stirring；
(2) CH is vigorously stirred under 0 DEG C of (in mixture of ice and water) water-bath3COONa ethanol solution, while with 3mL/min's
Speed is by AlCl3·6H2O ethanol solution instills CH3Continue to stir 0.5h in COONa ethanol solution, after completion of dropwise addition, nanometer is made
The NaCl little particle of rank；
(3) Surfactant CTAB that 10mL mass concentration is 10g/L is sequentially added in the mixture obtained to step (2)
Al (the CH that ethanol solution and 400mL concentration are 0.15mol/L3COO)3Ethanol solution is uniformly mixed；
(4) 0.21mol(8.4g is taken) NaOH particle is dissolved in the dehydrated alcohol (lower than 5 DEG C) that 200mL refrigerated, acutely stirs
Solution is made after mixing, under 0 DEG C of (in mixture of ice and water) water-bath, NaOH ethanol solution is added with the speed of 0.5 drop per second and is walked
Suddenly in the mixture of (3), continue to stir 1h after completion of dropwise addition, reaction is precipitated；
(5) sediment for obtaining step (4) filters, and is washed 3 times with dehydrated alcohol, the dry 18h at 100 DEG C, will
To white powder 500 DEG C of roasting 4h are warming up to the rate of 1 DEG C/min, obtain the NaCl@Al of core-shell structure2O3High-temperature phase-change
Heat-storing material.
Embodiment 2
(1) 0.03mol(2.46g is weighed) CH3COONa and 0.01mol(2.4143g) AlCl3·6H2O is dissolved in respectively
In 100mL dehydrated alcohol, solution is configured to after ultrasound, stirring；
(2) CH is vigorously stirred under room temperature (25 DEG C) water-bath3COONa ethanol solution, while will with the speed of 4mL/min
AlCl3·6H2O ethanol solution instills CH3Continue to stir 1h in COONa ethanol solution, after completion of dropwise addition, Nano grade is made
NaCl little particle；
(3) Surfactant CTAB that 20mL mass concentration is 10g/L is sequentially added in the mixture obtained to step (2)
Al (OH) (CH that ethanol solution and 400mL concentration are 0.15mol/L3COO)2Ethanol solution is uniformly mixed；
(4) 0.15mol(6g is taken) NaOH particle is dissolved in the dehydrated alcohol (lower than 5 DEG C) that 200mL refrigerated, is vigorously stirred
After solution is made, under room temperature (25 DEG C) water-bath, with it is per second 1 drop speed by NaOH ethanol solution be added step (3) mixing
Continue to stir 1.5h in object, after completion of dropwise addition, reaction is precipitated；
(5) sediment for obtaining step (4) filters, and after washing 3 times with dehydrated alcohol, dries at 80 DEG C for 24 hours, will
To white powder 600 DEG C of roasting 3h are warming up to the rate of 1 DEG C/min, obtain the NaCl@Al of core-shell structure2O3High-temperature phase-change
Heat-storing material.
Embodiment 3
(1) 0.03mol(2.46g is weighed) CH3COONa and 0.01mol(2.4143g) AlCl3·6H2O is dissolved in respectively
In 200mL dehydrated alcohol, solution is configured to after ultrasound, stirring；
(2) CH is vigorously stirred under 40 DEG C of water-baths3COONa ethanol solution, while with the speed of 5mL/min by AlCl3·
6H2O ethanol solution instills CH3Continue to stir 1.5h in COONa ethanol solution, after completion of dropwise addition, the NaCl that Nano grade is made is small
Particle；
(3) Surfactant CTAB that 20mL mass concentration is 15g/L is sequentially added in the mixture obtained to step (2)
Al (the NO that ethanol solution and 300mL concentration are 0.3mol/L3)3Ethanol solution is uniformly mixed；
(4) 0.3mol(12g is taken) NaOH particle is dissolved in the dehydrated alcohol (lower than 5 DEG C) that 300mL refrigerated, is vigorously stirred
After solution is made, under 40 DEG C of water-baths, with it is per second 5 drop speed by NaOH ethanol solution be added step (3) mixture in, drop
Continue to stir 2h after adding, reaction is precipitated；
(5) sediment for obtaining step (4) filters, and is washed 3 times with dehydrated alcohol, the dry 12h at 120 DEG C, will
To white powder 700 DEG C of roasting 2h are warming up to the rate of 1 DEG C/min, obtain the NaCl@Al of core-shell structure2O3High-temperature phase-change
Heat-storing material.
Claims (10)
1. a kind of NaCl@Al of core-shell structure2O3The preparation method of high-temperature phase change heat accumulation material, comprising the following steps:
(1) by CH3COONa and AlCl3It is sampled in molar ratio for 3:1, is dissolved in dehydrated alcohol respectively, CH is made3COONa ethyl alcohol
Solution and AlCl3Ethanol solution；
(2) under 0 ~ 40 DEG C of water bath condition, it is vigorously stirred CH3COONa ethanol solution, while by AlCl3Ethanol solution instills
CH3Continue 0.5 ~ 1.5h of stirring in COONa ethanol solution, after completion of dropwise addition；
(3) Surfactant CTAB ethanol solution and another Metal aluminum salt are sequentially added in the mixture obtained to step (2)
Ethanol solution is uniformly mixed；
(4) NaOH is taken to be dissolved in the dehydrated alcohol refrigerated, while being vigorously stirred under 0 ~ 40 DEG C of water bath condition, by NaOH second
Alcoholic solution is added in the mixture of step (3), continues 1 ~ 2h of stirring after completion of dropwise addition, and reaction is precipitated；
(5) precipitating obtained step (4) filters, and wash 3 times with dehydrated alcohol, dry 12 at 80 ~ 120 DEG C ~ for 24 hours after, liter
Temperature obtains the NaCl@Al of core-shell structure to 500 ~ 700 DEG C of 2 ~ 4 h of roasting2O3High-temperature phase change heat accumulation material.
2. preparation method according to claim 1, which is characterized in that CH in step (1)3COONa ethanol solution and AlCl3
Ethanol solution concentration is 0.05 ~ 0.6mol/L.
3. preparation method according to claim 1, which is characterized in that AlCl is added dropwise in step (2)3The speed of ethanol solution
For 3 ~ 5mL/min.
4. preparation method according to claim 1, which is characterized in that CTAB additive amount is 0.5 ~ 1g/L in step (3).
5. preparation method according to claim 1, which is characterized in that another Metal aluminum salt and CH in step (3)3COONa
Molar ratio be 2 ~ 3:1.
6. preparation method according to claim 1, which is characterized in that in step (3) another Metal aluminum salt be aluminum acetate,
Any one in eston, aluminum nitrate.
7. preparation method according to claim 1, which is characterized in that the dehydrated alcohol temperature refrigerated in step (4) is low
In 5 DEG C.
8. preparation method according to claim 1, which is characterized in that NaOH and (AlCl in step (4)3+ another kind metal
Aluminium salt) molar ratio be 2 ~ 3:1.
9. preparation method according to claim 1, it is characterised in that: the speed of NaOH ethanol solution is added dropwise in step (4)
For 0.5 ~ 5 drop per second.
10. preparation method according to claim 1, it is characterised in that: heating rate is 1 DEG C/min in step (5).
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Citations (5)
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| CN101112687A (en) * | 2007-06-08 | 2008-01-30 | 北京化工大学 | Core-shell structure magnetic microsphere aluminum oxide and method for preparing the same |
| CN102166532A (en) * | 2010-05-04 | 2011-08-31 | 昆明理工大学 | Heat-storing catalytic composite functional material and preparation method thereof |
| CN102407150A (en) * | 2011-10-11 | 2012-04-11 | 华东理工大学 | Titanium dioxide/silver/silver chloride core-shell photochemical catalyst and preparation method thereof |
| CN102631876A (en) * | 2012-04-06 | 2012-08-15 | 上海蓝怡科技有限公司 | Method for preparing core-shell-structured magnetic nano particles |
| CN105214090A (en) * | 2015-09-11 | 2016-01-06 | 吴晓红 | A kind of Fe 3o 4the synthetic method of ZnO core-shell nanospheres |
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2016
- 2016-09-14 CN CN201610823261.2A patent/CN106244118B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101112687A (en) * | 2007-06-08 | 2008-01-30 | 北京化工大学 | Core-shell structure magnetic microsphere aluminum oxide and method for preparing the same |
| CN102166532A (en) * | 2010-05-04 | 2011-08-31 | 昆明理工大学 | Heat-storing catalytic composite functional material and preparation method thereof |
| CN102407150A (en) * | 2011-10-11 | 2012-04-11 | 华东理工大学 | Titanium dioxide/silver/silver chloride core-shell photochemical catalyst and preparation method thereof |
| CN102631876A (en) * | 2012-04-06 | 2012-08-15 | 上海蓝怡科技有限公司 | Method for preparing core-shell-structured magnetic nano particles |
| CN105214090A (en) * | 2015-09-11 | 2016-01-06 | 吴晓红 | A kind of Fe 3o 4the synthetic method of ZnO core-shell nanospheres |
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