CN106244118A - A kind of NaCl@Al of nucleocapsid structure2o3the preparation method of high-temperature phase change heat accumulation material - Google Patents
A kind of NaCl@Al of nucleocapsid structure2o3the preparation method of high-temperature phase change heat accumulation material Download PDFInfo
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- CN106244118A CN106244118A CN201610823261.2A CN201610823261A CN106244118A CN 106244118 A CN106244118 A CN 106244118A CN 201610823261 A CN201610823261 A CN 201610823261A CN 106244118 A CN106244118 A CN 106244118A
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- ethanol solution
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- nacl
- coona
- alcl
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 51
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000009825 accumulation Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- OVYTZAASVAZITK-UHFFFAOYSA-M sodium;ethanol;hydroxide Chemical compound [OH-].[Na+].CCO OVYTZAASVAZITK-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- -1 Metal aluminum salt Chemical class 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 23
- 229960004756 ethanol Drugs 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 13
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical group O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 3
- 229940009827 aluminum acetate Drugs 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- IZMPACFDPANMBU-UHFFFAOYSA-N C(C)O.[AlH3] Chemical compound C(C)O.[AlH3] IZMPACFDPANMBU-UHFFFAOYSA-N 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract description 3
- 230000007704 transition Effects 0.000 abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract 4
- 159000000000 sodium salts Chemical class 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000008187 granular material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 239000012782 phase change material Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- PWZUUYSISTUNDW-VAFBSOEGSA-N quinestrol Chemical compound C([C@@H]1[C@@H](C2=CC=3)CC[C@]4([C@H]1CC[C@@]4(O)C#C)C)CC2=CC=3OC1CCCC1 PWZUUYSISTUNDW-VAFBSOEGSA-N 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides the NaCl@Al of a kind of nucleocapsid 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.First depletion belongs to sodium salt and Metal aluminum salt is dissolved in ethanol respectively and makes solution, then in the ethanol solution of metal sodium salt, instill Metal aluminum salt solution, surfactant and the ethanol solution of another kind of Metal aluminum salt mix homogeneously is added again in mixed liquor, then in above solidliquid mixture, add NaOH ethanol solution be precipitated thing, drying precipitate after finally cleaning, roasting, i.e. obtain the NaCl@Al of nucleocapsid structure2O3High-temperature phase change heat accumulation material.Firm Al2O3NaCl in kernel is wrapped up by shell, can overcome the shortcoming that NaCl meets water decomposition, corrosivity is strong, enhance the stability of material；The phase transition temperature of NaCl is 801 DEG C so that this heat-storing material can use in higher temperatures environment.
Description
Technical field
The present invention provides the NaCl@Al of a kind of nucleocapsid structure2O3The preparation method of high-temperature phase change heat accumulation material, belongs to the energy
Efficiently utilize and heat-storing material preparation field.
Background technology
The use of regenerative resource is to solve energy crisis and the effective way of problem of environmental pollution in current global range.
In solar energy, wind energy, water energy, biomass energy, nuclear energy equal energy source, solar energy is abundant and can freely obtain, and has huge sending out
Exhibition prospect.At present, concentration solar generating (CSP) technology can convert solar energy into heat energy and further by steam turbine or
Person's heat engine generates electricity, and has great advantage in terms of substituting fossil energy or reducing carbon emission.But, solar energy itself
Unstability and the intermittent generated energy that can affect CSP system so that the popularization and application of CSP technology are affected.
Heat energy/cold can be stored by thermal energy storage system (TES), is possible not only to realize the efficient utilization of heat energy,
CSP power plant can also be made more freely to operate, thus solve energy resource supply and demand in time, temperature, electricity and place etc.
The mismatch problem of aspect.Research is pointed out, the running temperature of CSP system is the highest, and its thermal efficiency also increases.Therefore, only
Operating temperature could meet the demand of following CSP electricity generation system at the high-temperature phase change heat accumulation material of 500 ~ 1200 DEG C of scopes.
Summary of the invention
The present invention provides a kind of NaCl@Al preparing nucleocapsid structure2O3The method of high-temperature phase change heat accumulation material.The phase of NaCl
Temperature is 801 DEG C, can produce substantial amounts of heat content and heat accumulation low cost, in phase transition process in inorganic salt heat reservoir
Show absolute advantage.Al2O3As a kind of ceramic material, there is the highest fusing point (typically more than 2000 DEG C) and excellent
Good stability at elevated temperature, can be encapsulated NaCl phase-change material, makes the high-temperature heat accumulation material of a kind of nucleocapsid structure.
This structure can not only overcome the shortcoming that NaCl corrosivity is strong, and have and can increase heat transfer area, stops phase-change material
React with environment, control the advantages such as change in volume in phase transition process.
The present invention is achieved through the following technical solutions:
A kind of NaCl@Al preparing nucleocapsid structure2O3The method of high-temperature phase change heat accumulation material, comprises the following steps:
(1) CH is weighed for 3:1 in molar ratio3COONa and AlCl3, it is dissolved in respectively in dehydrated alcohol, makes 0.05 ~ 0.6mol/L
CH3COONa ethanol solution and AlCl3Ethanol solution；
(2) under 0 ~ 40 DEG C of water bath condition, it is stirred vigorously CH3COONa ethanol solution, the speed with 3 ~ 5mL/min will simultaneously
AlCl3Ethanol solution instills CH3In COONa ethanol solution, continue stirring 0.5 ~ 1.5h after completion of dropwise addition, prepare Nano grade
The little granule of NaCl；
(3) in the mixture that step (2) obtains, Surfactant CTAB ethanol solution it is sequentially added into, and another kind of Metal aluminum salt
Ethanol solution, CTAB addition is 0.5 ~ 1g/L, Metal aluminum salt and CH3The mol ratio of COONa is 2 ~ 3:1, mix homogeneously；
(4) take NaOH to be dissolved in the dehydrated alcohol (less than 5 DEG C) of cold preservation, NaOH and (AlCl3+ Metal aluminum salt) mol ratio be
2~3:1；While being stirred vigorously under 0 ~ 40 DEG C of water bath condition, with the speed of 0.5 ~ 5 per second, NaOH ethanol solution is added
In the mixture of step (3), continuing stirring 1 ~ 2h after completion of dropwise addition, reaction is precipitated；
(5) precipitation that step (4) obtained filters, with absolute ethanol washing 3 times, after being dried 12 ~ 24h at 80 ~ 120 DEG C, with 1
DEG C/ramp of min to 500 ~ 700 DEG C of roasting 2 ~ 4h, obtain the NaCl@Al of nucleocapsid structure2O3High-temperature phase change heat accumulation material.
Metal aluminum salt described in step (3) is any one in aluminum acetate, eston, aluminum nitrate.
The invention has the beneficial effects as follows:
(1) use temperature≤300 DEG C of general middle low-temperature heat accumulating material, this heat-storing material uses temperature high, can 800 ~
The environment of 1400 DEG C uses, it is easier to meet the industrial requirement of solar plant；
(2) the NaCl@Al of the nucleocapsid structure of gained2O3Phase change heat storage material is Al due to outer layer covers2O3, thus there is resistance to height
Temperature (its fusing point is 2054 DEG C), thermal coefficient of expansion is low (between 4.9 ~ 9.3 × 10-6/ K), hardness advantages of higher；
(3) Al being coated with2O3Shell can be effectively protected the NaCl in kernel, it is to avoid the loss of NaCl and deep-etching；Al2O3
Being highly stable ceramic material, this structure can be effectively improved the heat stability of material.
Detailed description of the invention
Embodiment 1
(1) 0.03mol(2.46g is weighed) CH3COONa and 0.01mol(2.4143g) AlCl3·6H2O, is dissolved in 50mL anhydrous respectively
In ethanol, through ultrasonic, stirring after be configured to solution；
(2) under 0 DEG C of (in mixture of ice and water) water-bath, it is stirred vigorously CH3COONa ethanol solution, simultaneously with the speed of 3mL/min
By AlCl3·6H2O ethanol solution instills CH3In COONa ethanol solution, continue stirring 0.5h after completion of dropwise addition, prepare Nano grade
The little granule of NaCl；
(3) in the mixture that step (2) obtains, the Surfactant CTAB ethanol that 10mL mass concentration is 10g/L it is sequentially added into
Solution, and the Al (CH that 400mL concentration is 0.15mol/L3COO)3Ethanol solution, mix homogeneously；
(4) 0.21mol(8.4g is taken) NaOH granule is dissolved in the dehydrated alcohol (less than 5 DEG C) of 200mL cold preservation, after being stirred vigorously
Make solution, under 0 DEG C of (in mixture of ice and water) water-bath, with the speed of 0.5 per second, NaOH ethanol solution is added step (3)
Mixture in, after completion of dropwise addition continue stirring 1h, reaction is precipitated；
(5) precipitate that step (4) obtained filters, and with absolute ethanol washing 3 times, is dried 18h, by obtain at 100 DEG C
White powder to 500 DEG C of roasting 4h, obtains the NaCl@Al of nucleocapsid structure with the ramp of 1 DEG C/min2O3High-temperature phase change heat accumulation
Material.
Embodiment 2
(1) 0.03mol(2.46g is weighed) CH3COONa and 0.01mol(2.4143g) AlCl3·6H2O, be dissolved in respectively 100mL without
In water-ethanol, through ultrasonic, stirring after be configured to solution；
(2) under room temperature (25 DEG C) water-bath, it is stirred vigorously CH3COONa ethanol solution, simultaneously with the speed of 4mL/min by AlCl3·
6H2O ethanol solution instills CH3In COONa ethanol solution, continue stirring 1h after completion of dropwise addition, prepare little of the NaCl of Nano grade
Grain；
(3) in the mixture that step (2) obtains, the Surfactant CTAB ethanol that 20mL mass concentration is 10g/L it is sequentially added into
Solution, and Al (the OH) (CH that 400mL concentration is 0.15mol/L3COO)2Ethanol solution, mix homogeneously；
(4) 0.15mol(6g is taken) NaOH granule is dissolved in the dehydrated alcohol (less than 5 DEG C) of 200mL cold preservation, makes after being stirred vigorously
Become solution, under room temperature (25 DEG C) water-bath, with the speed of 1 per second by NaOH ethanol solution add step (3) mixture in,
Continuing stirring 1.5h after completion of dropwise addition, reaction is precipitated；
(5) precipitate step (4) obtained filters, and after absolute ethanol washing 3 times, is dried 24h, by obtain at 80 DEG C
White powder to 600 DEG C of roasting 3h, obtains the NaCl@Al of nucleocapsid structure with the ramp of 1 DEG C/min2O3High-temperature phase change heat accumulation
Material.
Embodiment 3
(1) 0.03mol(2.46g is weighed) CH3COONa and 0.01mol(2.4143g) AlCl3·6H2O, be dissolved in respectively 200mL without
In water-ethanol, through ultrasonic, stirring after be configured to solution；
(2) under 40 DEG C of water-baths, it is stirred vigorously CH3COONa ethanol solution, simultaneously with the speed of 5mL/min by AlCl3·6H2O second
Alcoholic solution instills CH3In COONa ethanol solution, continue stirring 1.5h after completion of dropwise addition, prepare the little granule of NaCl of Nano grade；
(3) in the mixture that step (2) obtains, the Surfactant CTAB ethanol that 20mL mass concentration is 15g/L it is sequentially added into
Solution, and the Al (NO that 300mL concentration is 0.3mol/L3)3Ethanol solution, mix homogeneously；
(4) 0.3mol(12g is taken) NaOH granule is dissolved in the dehydrated alcohol (less than 5 DEG C) of 300mL cold preservation, makes after being stirred vigorously
Becoming solution, under 40 DEG C of water-baths, with the speed of 5 per second by the mixture of NaOH ethanol solution addition step (3), dropping is tied
Continuing stirring 2h after bundle, reaction is precipitated；
(5) precipitate that step (4) obtained filters, and with absolute ethanol washing 3 times, is dried 12h, by obtain at 120 DEG C
White powder to 700 DEG C of roasting 2h, obtains the NaCl@Al of nucleocapsid structure with the ramp of 1 DEG C/min2O3High-temperature phase change heat accumulation
Material.
Claims (10)
1. the NaCl Al of a nucleocapsid structure2O3The preparation method of high-temperature phase change heat accumulation material, comprises the following steps:
(1) by CH3COONa and AlCl3Sample for 3:1 in molar ratio, be dissolved in respectively in dehydrated alcohol, make CH3COONa ethanol
Solution and AlCl3Ethanol solution；
(2) under 0 ~ 40 DEG C of water bath condition, it is stirred vigorously CH3COONa ethanol solution, simultaneously by AlCl3Ethanol solution instills
CH3In COONa ethanol solution, after completion of dropwise addition, continue stirring 0.5 ~ 1.5h；
(3) in the mixture that step (2) obtains, it is sequentially added into Surfactant CTAB ethanol solution and another kind of Metal aluminum salt
Ethanol solution, mix homogeneously；
(4) take NaOH to be dissolved in the dehydrated alcohol of cold preservation, while being stirred vigorously under 0 ~ 40 DEG C of water bath condition, by NaOH second
Alcoholic solution adds in the mixture of step (3), continues stirring 1 ~ 2h after completion of dropwise addition, and reaction is precipitated；
(5) precipitation that step (4) obtained filters, and with absolute ethanol washing 3 times, after being dried 12 ~ 24h, rises at 80 ~ 120 DEG C
Temperature, to 500 ~ 700 DEG C of roasting 2 ~ 4 h, obtains the NaCl@Al of nucleocapsid structure2O3High-temperature phase change heat accumulation material.
Preparation method the most according to claim 1, it is characterised in that CH in step (1)3COONa ethanol solution and AlCl3
Ethanol solution concentration is 0.05 ~ 0.6mol/L.
Preparation method the most according to claim 1, it is characterised in that dropping AlCl in step (2)3The speed of ethanol solution
It is 3 ~ 5mL/min.
Preparation method the most according to claim 1, it is characterised in that in step (3), CTAB addition is 0.5 ~ 1g/L.
Preparation method the most according to claim 1, it is characterised in that Metal aluminum salt and CH in step (3)3COONa mole
Ratio is 2 ~ 3:1.
6. according to the preparation method described in claim 1 or 6, it is characterised in that in step (3), Metal aluminum salt is aluminum acetate, alkali
Any one in formula aluminum acetate, aluminum nitrate.
Preparation method the most according to claim 1, it is characterised in that in step (4), the dehydrated alcohol temperature of cold preservation is low
In 5 DEG C.
Preparation method the most according to claim 1, it is characterised in that NaOH and (AlCl in step (4)3+ Metal aluminum salt)
Mol ratio is 2 ~ 3:1.
Preparation method the most according to claim 1, it is characterised in that: the speed of dropping NaOH ethanol solution in step (4)
For 0.5 ~ 5 per second.
Preparation method the most according to claim 1, it is characterised in that: in step (5), heating rate is 1 DEG C/min.
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| CN106244118B CN106244118B (en) | 2019-02-19 |
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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 |
-
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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