CN110157384A - A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity and preparation method thereof - Google Patents
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity and preparation method thereof Download PDFInfo
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Abstract
The invention discloses anti-oxidant composite phase-change heat-storage material of a kind of high thermal conductivity and preparation method thereof, raw material compositions are as follows: inorganic phase-changing material, adsorption carrier material and high thermal conductivity material;Inorganic phase-changing material is configured by 40% ~ 50% sodium chloride and 50% ~ 60% potassium chloride, and total amount 100%, the percentage is mass percent;Adsorption carrier material is fumed silica;High thermal conductivity materials are aluminium nitride.Inorganic phase-changing material: fumed silica: the mass ratio of aluminium nitride is 6:1:(1 ~ 3).Component is reasonable, and preparation process is simple, and thermal coefficient is high, convenient for encapsulation and uses, suitable for high temperature, air environment, and is not in the phenomenon of leakage in phase transition process.
Description
Technical field
The present invention relates to anti-oxidant composite phase-change heat-storage materials of a kind of high thermal conductivity and preparation method thereof, belong to composite material skill
Art field.
Background technique
Energy storage technology aims to solve the problem that the discontinuous problem of energy supply over time and space, is to improve energy utilization rate
Effective way.It is adopted in power supply industry " peak load shifting ", space flight and aviation, utilization of new energy resources, industrial afterheat recovery and civil buildings
It is warm etc. all to have broad application prospects.Compared to chemical electric power storage, heat-storage technology has energy storage (thermal energy) capacity big, stable
The advantages such as property environmental protection strong, at low cost.
Phase-change heat-storage material has many advantages, such as that storage density is big, the approximate isothermal of phase transition process, process are easy to control.It is wherein inorganic
Salt has great advantage because of the advantages that its price is low, highly-safe, phase transition temperature is easily deployed, in heat accumulation field.But it is simple
The generally existing thermal coefficient of inorganic salts it is low, phase transition process thermal resistance constantly changes, and has the problems such as certain corrosivity.Currently,
Studying compound phase-change heat-storage material is the main path for solving problem above.
Currently, compound phase-change heat-storage material multi-panel is to middle low temperature heat accumulation field, it is difficult to cope with aoxidized under the condition of high temperature, point
The problems such as solution, corrosion.And mostly added with water, ethyl alcohol, adhesive etc. in preparation process, material needs to dry, and preparation process is complicated,
And hole easy to form in sintering process, influence thermal coefficient.
Summary of the invention
Purpose: to solve the deficiencies in the prior art, the present invention provides a kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity
And preparation method thereof.
Technical solution: in order to solve the above technical problems, the technical solution adopted by the present invention are as follows:
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, raw material composition are as follows: inorganic phase-changing material, absorption carrier material
Material and high thermal conductivity material;
The inorganic phase-changing material is configured by 40%~50% sodium chloride and 50%~60% potassium chloride, total amount
It is 100%, the percentage is mass percent;
The adsorption carrier material is fumed silica;The high thermal conductivity materials are aluminium nitride.
Preferably, the inorganic phase-changing material: fumed silica: the mass ratio of aluminium nitride be 6:1:(1~
3)。
More preferably, the inorganic phase-changing material: fumed silica: the mass ratio of aluminium nitride is 6:1:3.
On the other hand, the present invention also provides a kind of preparation methods of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity, including
Following steps:
(1) inorganic phase-changing material is prepared;Respectively press mass fraction 40%~50% and 50%~60%, weigh sodium chloride and
Potassium chloride is stirred evenly using pulverizer to get inorganic phase-changing material;
(2) a certain amount of fumed silica is weighed, is mixed with inorganic phase-changing material made from step (1), uses pulverizer
It stirs evenly;
(3) sample by step (2) after mixing, is placed in electric furnace, and 750 DEG C are heated 2~3 hours;
(4) sample after step (3) heating is taken out, cools down at room temperature, then beats powder with pulverizer;
(5) a certain amount of aluminium nitride powder is weighed, mixes with sample made from step (4), is stirred evenly with pulverizer;
(6) sample made from a certain amount of step (5) is weighed, is put into mold, is pressed into bulk sample using press machine;
(7) bulk sample made from step (6) is taken, is placed in electric furnace, 800 DEG C are sintered, and obtain height after cooling
Thermally conductive anti-oxidant composite phase-change heat-storage material.
Preferably, the preparation method of the anti-oxidant composite phase-change heat-storage material of the high thermal conductivity, pulverizer revolving speed
For 34000r/min, smashing fineness is 70~300 mesh.
Preferably, the preparation method of the anti-oxidant composite phase-change heat-storage material of the high thermal conductivity, the gas phase two
The fineness of silica is 200~400 mesh.
Preferably, the preparation method of the anti-oxidant composite phase-change heat-storage material of the high thermal conductivity, addition it is inorganic
Phase-change material and fumed silica mass ratio are 6:1.This is without leakage optimum proportioning.
Preferably, the preparation method of the anti-oxidant composite phase-change heat-storage material of the high thermal conductivity, the nitridation of addition
Aluminium and fumed silica mass ratio are (1~3): 1, more preferably 3:1, heating conduction is the most superior at this time.
Preferably, in step (6), press pressure 20MPa, dwell time 60s.
The present invention also requires a kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, anti-oxidant compound by above-mentioned high thermal conductivity
The preparation method of phase-change heat-storage material is prepared.
The utility model has the advantages that anti-oxidant composite phase-change heat-storage material of high thermal conductivity provided by the invention and preparation method thereof, thermally conductive system
Number is high, convenient for encapsulation and uses, suitable for high temperature, air environment, and is not in the phenomenon of leakage in phase transition process, with
Lower advantage:
1) preparation process is simple, component is reasonable, and inorganic salts are completed to adsorb during high temperature melt with fumed silica,
Without adding lytic agent, uniform, no leakage is adsorbed.
2) present invention is using powdered aluminium nitride as heat conducting base material, and thermal conductivity is high, performance is stable, expansion rate is low, anti-
It aoxidizes, is anticorrosive, solving the problems, such as graphite-based material high-temperature oxydation, reducing equipment sealing cost.
3) the anti-oxidant composite phase-change heat-storage material of a kind of high thermal conductivity of the invention, can according to requiring, be processed into different size,
Brick body of different shapes, in phase transition process, brick body face shaping is remained unchanged, and is convenient for mass, modular applications.
Detailed description of the invention
Fig. 1 is the preparation flow figure of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity in embodiment;
Fig. 2 is the pictorial diagram of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity prepared in embodiment;
Fig. 3 is the DSC test curve figure of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity prepared in embodiment.
Specific embodiment
Illustrate below with reference to example to the present invention: percentage is mass percent in the present invention.
Embodiment 1
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, the preparation method comprises the following steps: weighing 58.5g sodium chloride, 74.5g chlorination
Potassium, pulverizer are stirring evenly and then adding into 22.2g fumed silica and are again stirring for uniformly;Obtained pulverized specimen is placed in electricity
It is heated 2 hours in heating furnace with 750 DEG C, takes out the cooling in room temperature, obtain fluffy aspect product;Fluffy aspect product are used and beat powder
Machine crushes, and 66.5g aluminium nitride powder is added, and is again stirring for uniformly;By gained pulverized specimen press machine briquet, molding pressure
Power 20MPa is placed in electric furnace at 800 DEG C after being sintered and cooled to obtain the final product.
Embodiment 2
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, the preparation method comprises the following steps: weighing 64.4g sodium chloride, 74.5g chlorination
Potassium, pulverizer are stirring evenly and then adding into 23.2g fumed silica and are again stirring for uniformly;Obtained pulverized specimen is placed in electricity
It is heated 2.1 hours in heating furnace with 750 DEG C, takes out the cooling in room temperature, obtain fluffy aspect product;Fluffy aspect product are used and are beaten
Powder machine crushes, and 69.5g aluminium nitride powder is added, and is again stirring for uniformly;By gained pulverized specimen press machine briquet, molding
Pressure 20MPa is placed in electric furnace at 800 DEG C after being sintered and cooled to obtain the final product.
Embodiment 3
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, the preparation method comprises the following steps: weighing 58.5g sodium chloride, 82g chlorination
Potassium, pulverizer are stirring evenly and then adding into 23.4g fumed silica and are again stirring for uniformly;Obtained pulverized specimen is placed in electricity
It is heated 2.2 hours in heating furnace with 750 DEG C, takes out the cooling in room temperature, obtain fluffy aspect product;Fluffy aspect product are used and are beaten
Powder machine crushes, and 70.2g aluminium nitride powder is added, and is again stirring for uniformly;By gained pulverized specimen press machine briquet, molding
Pressure 20MPa is placed in electric furnace at 800 DEG C after being sintered and cooled to obtain the final product.
Embodiment 4
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, the preparation method comprises the following steps: weighing 58.5g sodium chloride, 74.5g chlorination
Potassium, pulverizer are stirring evenly and then adding into 22.2g fumed silica and are again stirring for uniformly;Obtained pulverized specimen is placed in electricity
It is heated 2 hours in heating furnace with 750 DEG C, takes out the cooling in room temperature, obtain fluffy aspect product;Fluffy aspect product are used and beat powder
Machine crushes, and 44.4g aluminium nitride powder is added, and is again stirring for uniformly;By gained pulverized specimen press machine briquet, molding pressure
Power 20MPa is placed in electric furnace at 800 DEG C after being sintered and cooled to obtain the final product.
Embodiment 5
A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, the preparation method comprises the following steps: weighing 58.5g sodium chloride, 74.5g chlorination
Potassium, pulverizer are stirring evenly and then adding into 22.2g fumed silica and are again stirring for uniformly;Obtained pulverized specimen is placed in electricity
It is heated 2 hours in heating furnace with 750 DEG C, takes out the cooling in room temperature, obtain fluffy aspect product;Fluffy aspect product are used and beat powder
Machine crushes, and 66.6g aluminium nitride powder is added, and is again stirring for uniformly;By gained pulverized specimen press machine briquet, molding pressure
Power 20MPa is placed in electric furnace at 800 DEG C after being sintered and cooled to obtain the final product.
Comparative example 1
Referring to Chinese Patent Application No. 201610823261.2, a kind of NaCl@Al of core-shell structure2O3High-temperature phase change heat accumulation
The preparation method of material, the preparation method comprises the following steps:
(1) by CH3COONa and AlCl3It is sampled in molar ratio for 3:1, is dissolved in dehydrated alcohol respectively, CH3COONa is made
Ethanol 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 drop
Enter CH3Continue 0.5~1.5h of stirring in COONa ethanol solution, after completion of dropwise addition;
(3) Surfactant CTAB ethanol solution and another metal are sequentially added in the mixture obtained to step (2)
Aluminium salt ethanol solution is uniformly mixed;
(4) NaOH is taken to be dissolved in the dehydrated alcohol refrigerated, it, will while being vigorously stirred under 0~40 DEG C of water bath condition
NaOH ethanol 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 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 NaCl@Al of core-shell structure is obtained2O3High-temperature phase change heat accumulation material.
Comparative example 2
Referring to Chinese Patent Application No. 201610100879.6, a kind of preparation side for high temperature composite heat storage material of being formed
Method, the preparation method comprises the following steps:
(1) by vermiculite 1300 DEG C at a temperature of handle 20min, it is mixed for 1:10 according to mass ratio with phase-change material after cooling
Close, the phase-change material by 40.0%~60.0wt% MgCl2, the KCl and 19.6~29.6wt% of 20.4~30.4wt%
NaCl composition, the sum of phase-change material be 100%;
(2) by said mixture at 400 DEG C, negative pressure keeps the temperature 6h under conditions of being -15kPa, prepares composite phase-change material,
Then by composite phase-change material Mechanical Crushing to 40 mesh, for 24 hours, the modified carbon fiber accounts for mechanical mixture after adding modified carbon fiber
The 2%~8% of composite phase-change material gross mass;
(3) high-temperature agglomerant and the compression moulding under the pressure of 10~20MPa is added dropwise, finally 300 DEG C at a temperature of protect
Warm 30min solidify up to the sizing high temperature composite heat storage material.
Comparative example 3
Referring to Chinese Patent Application No. 201310175016.1, a kind of High-temperature composite phase-change heat storage and its preparation side
Method, the preparation method comprises the following steps:
(1) raw material is subjected to ingredient, mixing that then raw mixture is dry grinded in the ball mill according to formula rate
30min is poured out, and weight is added and is the polyvinyl alcohol adhesive of formula material total weight 5%, and is fully ground in mortar, directly
To being uniformly mixed, the half-dry type powder blank for being suitable for compression molding is obtained, in which: by weight percentage, the recipe ratio
Example are as follows: white clay 5%, alumine 25%~45%, aluminium powder 50%~70%, raw material weight summation are 100%;
(2) it suppresses each green body and weighs uniformly mixed 10g blank, the side unidirectionally pressurizeed is taken in powder compressing machine
Formula, first add-on type pressure 3MPa, then unloads, then green body is made in add-on type pressure 6MPa, dwell time 20min;
(3) green body is placed in drying box, is warming up to 150 DEG C and keeps the temperature 2 hours;
(4) green body after drying is placed in chamber type electric resistance furnace, is heated up with the speed of 5 DEG C/min, when temperature reaches 660 DEG C
Shi Baowen 10min;
(5) it is then heated up with the speed of 10 DEG C/min, keeps the temperature 10min when temperature reaches 870 DEG C;
(6) 950 DEG C of maximum sintering temperature and heat preservation 120min, rear furnace cooling are finally warming up to the speed of 10 DEG C/min
To room temperature, High-temperature composite phase-change heat storage is obtained.
Comparative example 4
Referring to Chinese Patent Application No. 201711322736.0, a kind of compound heat accumulation ceramic based material of high-temperature phase-change and its system
Preparation Method, the preparation method comprises the following steps:
(1) 20~30 parts of lithium carbonate, 20~30 parts of potassium carbonate, 30~40 parts of sodium carbonate and 10~15 parts of ceramic substrate are mixed
It closes, be ground to 400~500 mesh and be uniformly mixed, obtain inorganic salts ceramic matrix systems;
(2) 1~2 part of highly-conductive hot carbon fiber, 1~2 part of doped graphite are heated in 500~600 DEG C of inert gases
15min is then added in above-mentioned inorganic salts ceramic matrix systems, is uniformly mixed by being ground to 400~500 mesh, is formed multiple
Zoarium system;
(3) after the pressurized molding of above-mentioned compound system, 2.4~2.8MPa of moulding pressure, 2~2.5min of pressing time, in
700~760 DEG C of 20~30min of sintering are cooled to room temperature after the completion of sintering, obtain the compound heat accumulation ceramic based material of high-temperature phase-change.
Comparative example 1: preparation process is complicated;It needs to add ethanol solution, is also easy to produce gap during heat-agglomerating, influences to lead
Hot property;For core-shell structure, can not compression moulding, bulk density is low.
Comparative example 2: easy to oxidize under high temperature air environment using modified carbon fiber material.
Comparative example 3: preparation process is complicated;Polyvinyl alcohol need to be added, gap is also easy to produce during heat-agglomerating, influences thermally conductive
Performance;Aluminium powder is easy to oxidize under high temperature air environment, and there are security risks for chance water.
Comparative example 4: preparation process is complicated, heats in inert gas;Using carbon fiber and graphite, hold under high temperature air environment
It is oxidizable.
Phase-change heat-storage material performance test obtained by above-described embodiment
One, Determination of conductive coefficients is as follows:
Embodiment 1-3 test equipment: Hot Disk (TPS 2500), comparative example 1-4 are to indicate data in patent.
Table 1
As it can be seen from table 1 the anti-oxidant composite phase-change heat-storage material thermal coefficient energy of high thermal conductivity described in the embodiment of the present invention
Enough reach 5.13-11.98W/ (m*K);Higher than similar-type products several times on the market, it is known that existing similar-type products on the market are led
Hot coefficient can only achieve 1.55-2.86W/ (m*K), and currently used high-temp solid accumulation of heat magnesia brick thermal coefficient is 1-2W/ (m*
K)。
Two, Thermal cycle oxidation and leakage experiment test
High temperature circulation experiment:
(1) it by sample made from embodiment 1 to embodiment 4, is placed in alumina crucible, is added in Muffle furnace with 900 DEG C
Heat 2 hours, taking-up are placed in air cooling;
(2) step (1) is pressed iterative cycles 100 times;
(3) sample surfaces, no significant change, no precipitation salt are observed;
(4) it weighs, circulation front and back mass change only 0.3%.
According to sample material analysis and circulation experiment result is combined it is found that a kind of anti-oxidant compound heat accumulation of high thermal conductivity of the present invention
Material can be stablized in air environment and use at 900 DEG C.Under theory, it can be applied to 1000 DEG C.Therefore, this material can be in air
Use is to 900 DEG C without oxidation and the phenomenon of leakage in environment.
Theory analysis is as follows: the present invention it is used 801 DEG C of sodium chloride fusing point, 1413 DEG C of boiling point, do not aoxidized under high temperature, regardless of
Solution;It 770 DEG C of potassium chloride, 1420 DEG C of boiling point, do not aoxidize, decompose under high temperature;Silica, 1723 DEG C of fusing point, 2230 DEG C of boiling point,
Property is stablized;Aluminium nitride, 2400 DEG C of fusing point, 1000 DEG C or more, oxidation reaction occurs for Cai Huiyu air, and forms sull
Still can Protective substances, until 1370 DEG C.
Several composite phase change heat-accumulation material hot propertys of table 2
Material | Phase-change material content % | Phase transition temperature (DEG C) | Latent heat of phase change (KJ/Kg) |
Na2SO4/SiO2 | 50 | 879 | 84.94 |
NaNO3/MgO | 40 | 308 | 59.1 |
KCl-KF/ spinelle | 23+17 | 646 | 70.98 |
NaCl/SiC | 30 | 801 | 157.9 |
Na2CO3-Ba2CO3/MgO | 24+26 | 686 | 72.6 |
Fig. 1 is the preparation flow figure of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity in embodiment;
Fig. 2 is the pictorial diagram of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity prepared in embodiment;
Fig. 3 is the DSC test curve figure of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity prepared in embodiment, phase transformation
Temperature is 667.3 DEG C, latent heat of phase change 214.1J/g, and comprehensive performance is superior.
The present invention is disclosed with preferred embodiment above, so it is not intended to limiting the invention, all to use equivalent replacement
Or equivalent transformation mode technical solution obtained, it is within the scope of the present invention.
Claims (10)
1. a kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, which is characterized in that its raw material composition are as follows: inorganic phase-changing material,
Adsorption carrier material and high thermal conductivity material;
The inorganic phase-changing material is configured by 40% ~ 50% sodium chloride and 50% ~ 60% potassium chloride, total amount 100%, institute
Stating percentage is mass percent;
The adsorption carrier material is fumed silica;The high thermal conductivity materials are aluminium nitride.
2. the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 1, which is characterized in that the inorganic-phase variable
Material: fumed silica: the mass ratio of aluminium nitride is 6:1:(1 ~ 3).
3. the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 1 or 2, which is characterized in that described inorganic
Phase-change material: fumed silica: the mass ratio of aluminium nitride is 6:1:3.
4. a kind of preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity, which comprises the following steps:
(1) inorganic phase-changing material is prepared;Mass fraction 40% ~ 50% and 50% ~ 60% is pressed respectively, is weighed sodium chloride and potassium chloride, is made
It is stirred evenly with pulverizer to get inorganic phase-changing material;
(2) a certain amount of fumed silica is weighed, mixes with inorganic phase-changing material made from step (1), is stirred with pulverizer
Uniformly;
(3) sample by step (2) after mixing, is placed in electric furnace, and 750 DEG C are heated 2 ~ 3 hours;
(4) sample after step (3) heating is taken out, cools down at room temperature, then beats powder with pulverizer;
(5) a certain amount of aluminium nitride powder is weighed, mixes with sample made from step (4), is stirred evenly with pulverizer;
(6) sample made from a certain amount of step (5) is weighed, is put into mold, is pressed into bulk sample using press machine;
(7) bulk sample made from step (6) is taken, is placed in electric furnace, 800 DEG C are sintered, and obtain high thermal conductivity after cooling
Anti-oxidant composite phase-change heat-storage material.
5. the preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 4, which is characterized in that beat
Powder machine revolving speed is 34000r/min, and smashing fineness is 70 ~ 300 mesh.
6. the preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 4, which is characterized in that institute
The fineness for stating fumed silica is 200 ~ 400 mesh.
7. the preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 4, which is characterized in that add
The inorganic phase-changing material and fumed silica mass ratio entered is 6:1.
8. the preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 4, which is characterized in that add
The aluminium nitride and fumed silica mass ratio entered is (1 ~ 3): 1.
9. the preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity according to claim 1, which is characterized in that step
Suddenly in (6), press pressure 20MPa, dwell time 60s.
10. a kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity, which is characterized in that described in any item by claim 4-9
The preparation method of the anti-oxidant composite phase-change heat-storage material of high thermal conductivity is prepared.
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