CN109233751A - A kind of carbon-based composite phase-change energy storage material and preparation method thereof - Google Patents
A kind of carbon-based composite phase-change energy storage material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of carbon-based composite phase-change energy storage materials and preparation method thereof, and this method comprises the following steps: using lithium carbonate and potassium nitrate as raw material, heating after mixing, obtain lithium carbonate-potassium nitrate fused salt mixt;Potassium chloride is added into the fused salt mixt, heats, obtains low melting point eutectic fused salt;The eutectics fused salt is ground to powdery, adds graphene, is uniformly mixed, is obtained graphene/eutectics fused salt powder, the graphene/eutectics fused salt powder is uniformly mixed with expansible graphite matrix, obtains graphene/fused salt mixt powder;By the graphene/fused salt mixt powder cold moudling, the sample of regular shape is obtained;The sample is dried, is cooled to room temperature, repairing type obtains carbon-based composite phase-change energy storage material.Graphene is added in eutectic salt medium by the present invention, under the premise of retaining the higher latent heat of eutectics fused salt, improves the thermal coefficient of phase change medium, has excellent heat storage efficiency.
Description
Technical field
The invention belongs to the preparation technical fields of composite phase-change energy storage material, and in particular to a kind of carbon-based composite phase change energy-storing
Material and preparation method thereof.
Background technique
With the increase of world population, the mankind are also increasingly huge for the demand of Modern Industry Products, large-scale industrial
Production generates a large amount of Industry Waste flue gas.The discharge of industrial smoke not only causes energy waste, but also brings and be on the rise
Problem of environmental pollution.According to the height of waste heat supply temperature, flue gas can be divided into high-temperature flue gas (> 600 DEG C), medium temperature flue gas (230~
600 DEG C) and low-temperature flue gas (< 230 DEG C).It is high during being recycled using phase-change thermal storage technology to residual heat resources
Temperature, the UTILIZATION OF VESIDUAL HEAT IN situation of low-temperature flue gas are relatively preferable, and the utilization rate of waste heat of medium temperature flue gas is lower.
Currently, domestic and foreign scholars have done some researchs to the waste heat recycling of flue gas using phase change energy storage technology, study
Working media includes organic and inorganic.Wherein organic working media mainly has paraffin class, polyethylene glycol and acetamide
Equal fatty acids, the phase transition temperature of most of organic working media are lower than 150 DEG C, and melting latent heat is lower than 150Jg-1;It is inorganic
Class working media mainly has nitrate, chlorate, fluorination salt, and the phase transition temperature of the inorganic working media is higher, and melting is latent
Heat is larger.The corrosivity of most of nitrate is small and will not decompose at 500 DEG C or less, the disadvantage is that thermal coefficient is relatively low, because
This is easy to produce hot-spot in use.The compatibility of fluoride salt and canister material is preferable, has very high molten
Point and biggish melting latent heat belong to high temperature modification heat accumulating, but by liquid phase to have biggish volume contraction when solid phase,
If LiF is up to 23%, structural stability is reduced, influences the service performance of material.It works and is situated between as medium temperature phase-changing energy storage material
One of alternative of matter, carbonate and its fused salt mixt have application potential very much, but that there is also phase transition temperatures is relatively high,
The disadvantages of lower thermal coefficient causes heat storage efficiency not high, and stronger corrosivity is more demanding to packaging container.
Therefore, there is an urgent need to develop a kind of carbon-based composite phase-change energy storage material, to overcome disadvantage mentioned above, meet medium temperature flue gas
Waste heat recycles demand.
Summary of the invention
Medium temperature phase-changing energy storage material heat storage efficiency is not high, is not easy the defect encapsulated for existing in the prior art, this
Invention provides a kind of carbon-based composite phase-change energy storage material and preparation method thereof, which passes through to related process parameters
It is carbon-based without the advantages such as flowing, latent heat of phase change be higher can to obtain thermal coefficient with higher, solid-liquid phase change process for adjustment
Composite phase-change energy storage material.This kind of material has a lower phase transition temperature, higher heat storage efficiency, in use,
It will not occur to corrode packaging container phenomenon.It can preferably be recycled more than medium temperature flue gas using this kind of composite phase-change energy storage material
Thermal resource improves energy utilization rate, pushes the energy-saving and emission-reduction of high energy-consuming enterprises, thus is with a wide range of applications and imitates with economical
Benefit.
In order to achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of carbon-based composite phase-change energy storage material, includes the following steps:
1) using lithium carbonate and potassium nitrate as raw material, 1-2h is heated under 750-900 DEG C (preferably 800 DEG C) after mixing
(preferably 1h) obtains lithium carbonate-potassium nitrate fused salt mixt;
2) potassium chloride is added into fused salt mixt obtained in step 1), is heated under 750-850 DEG C (preferably 800 DEG C)
1-2h (preferably 1h), obtains low melting point eutectic fused salt;
3) low melting point eutectic fused salt obtained in step 2) is ground to powdery, graphene is added, with 300-400r/min
Revolving speed grind, mix 2-3h, obtain uniformly mixed graphene/eutectics fused salt powder;
4) graphene obtained in step 3)/eutectics fused salt powder is uniformly mixed with expansible graphite matrix, is added
The alcohol of 95wt% obtains uniform graphene/fused salt mixt powder to the state of soaking (in order to cold moudling);
5) graphene/fused salt mixt powder cold moudling will be obtained in step 4), obtains the sample of sheet;
6) sample obtained in step 5) is dried 4-6h hours at 100-120 DEG C, is obtained after being cooled to room temperature, repairing type
Carbon-based composite phase-change energy storage material.
By conceiving above, chlorination is on the one hand used as phase-change material using the fused salt mixt of lithium carbonate and potassium nitrate
Potassium has obtained that fusing point is moderate, and the higher phase-change material of latent heat makes material have excellent thermal storage capability as fluxing agent;
On the other hand, by adding graphene, the advantage of its high thermal conductivity is made full use of, the heat of phase change composite material is improved
Storage efficiency.In addition, using expansible graphite for matrix, using uniaxial compression formula cold pressing forming process, medium temperature compound phase is prepared
Change energy-storage material efficiently solves the flow field problem of solid-liquid phase change process, ensure that the service performance of phase-changing energy storage material.
The preparation process more simplifies, and preparation cost is lower.
As further preferred, wherein the mass ratio of the lithium carbonate and potassium nitrate is 1:1.5~4 in step 1).
As further preferred, wherein the mass ratio of the lithium carbonate and potassium nitrate is 1:2 in step 1).
As further preferred, wherein the quality of the potassium chloride accounts for both fused salt mixt and potassium chloride in step 2)
The 10~15% of gross mass.
As further preferred, wherein the quality of the potassium chloride accounts for both fused salt mixt and potassium chloride in step 2)
The 12% of gross mass.
As further preferred, wherein the melting temperature of the low melting point eutectic fused salt is 400-450 in step 2)
℃。
As further preferred, wherein low melting point eutectic fused salt obtained in step 2) is ground to 50 in step 3)
Mesh~+200 mesh powdery is added the graphene of -800 mesh of 400 mesh, is ground with the revolving speed of 400r/min, mixes 2.5-3h, obtained
Uniformly mixed graphene/eutectics fused salt powder.
As further preferred, wherein the quality of the graphene accounts for low melting point eutectic fused salt and graphite in step 3)
The 5%~15% of both alkene gross mass.
As further preferred, wherein the quality of the graphene accounts for low melting point eutectic fused salt and graphite in step 3)
The 5~10% of both alkene gross mass.
As further preferred, wherein in step 3), graphene/eutectics fused salt powder size controlling 50 mesh~+
200 mesh.
As further preferred, wherein in step 4), the graphene/eutectics fused salt powder and expansible graphite matrix
Mass ratio be 3:1.
As further preferred, wherein the pressure of the cold moudling is 20~30MPa in step 5).
As further preferred, wherein the pressure of the cold moudling is 30MPa, and molding effect is best in step 5).
The present invention also provides a kind of composite phase-change energy storage material carbon-based as made from above-mentioned method, the phase transformation storage
Energy material has >=2Wm-1·K-1Thermal coefficient.
The invention has the following advantages:
1, graphene is added in eutectic salt medium by the present invention, under the premise of retaining the higher latent heat of eutectics fused salt,
The thermal coefficient of phase change medium is improved, there is excellent heat storage efficiency.
2, the present invention uses expansible graphite as encapsulating material, by control pressure through cold moudling, prepares certain
The sample of regular shape efficiently solves the flow field problem during eutectic salt medium solid-liquid phase change, ensure that phase-change accumulation energy material
The service performance of material.
3, preparation process of the invention more simplifies, and preparation cost is lower.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to carbon-based composite phase-change energy storage material proposed according to the present invention and preparation method thereof its specific embodiment,
Feature and its effect, detailed description is as follows.
Following material or reagent are commercially available if not illustrating.
Embodiment 1
The preparation method for present embodiments providing a kind of carbon-based composite phase-change energy storage material, includes the following steps:
1) 100g lithium carbonate is mixed with 150g potassium nitrate, is uniformly mixed and is placed in alumina crucible, in Muffle furnace
2h is heated at 900 DEG C, obtains lithium carbonate-potassium nitrate fused salt mixt;
2) 44.1g potassium chloride (KCl) is added into fused salt mixt obtained in step 1) and is used as fluxing agent, in Muffle furnace
2h is heated at 800 DEG C, obtains the eutectics fused salt that fusing point (being obtained by differential thermal analysis) is 450 DEG C;
3) low melting point eutectic fused salt obtained in step 2) is ground to -50 mesh~200 mesh to be placed in ball grinder, is added
The graphene for entering 15.6g is ground with the revolving speed of 400r/min by ball milling, mixes 2h, obtains uniformly mixed graphene/eutectic
Fused salt powder;Wherein graphene/eutectics fused salt powder partial size should be controlled in -50 mesh~+200 mesh;
4) graphene obtained in step 3)/eutectics fused salt powder is uniformly mixed with the expansible graphite of 97g, adds 20g
Alcohol is to slightly soaking state;Mixed powder is placed in mold, by control pressure through cold moudling, cold moudling pressure is
20MPa prepares phase-changing energy storage material sample.Sample after molding is put into 100 DEG C of drying boxes and is dried 4 hours, is cooled to
Carbon-based composite phase-change energy storage material is obtained after room temperature, repairing type.
Embodiment 2
The preparation method for present embodiments providing a kind of carbon-based composite phase-change energy storage material, includes the following steps:
1) 50g lithium carbonate is mixed with 200g potassium nitrate, is uniformly mixed and is placed in alumina crucible, in Muffle furnace
2h is heated at 900 DEG C, obtains lithium carbonate-potassium nitrate fused salt mixt;
2) 27.8g potassium chloride (KCl) is added into fused salt mixt obtained in step 1) and is used as fluxing agent, in Muffle furnace
2h is heated at 800 DEG C, obtains the eutectics fused salt that fusing point is 400 DEG C (being obtained by differential thermal analysis);
3) low melting point eutectic fused salt obtained in step 2) is ground to 50 mesh hereinafter, being placed in ball grinder, be added
The graphene of 24.5g is ground with the revolving speed of 400r/min by ball milling, mixes 2h, and it is molten to obtain uniformly mixed graphene/eutectic
Salt powder.Wherein graphene/fused salt mixt powder partial size should be controlled in -50 mesh~+200 mesh;
4) graphene obtained in step 3)/eutectics fused salt powder is uniformly mixed with the expansible graphite of 100.9g, it should
Step is only immixture, adds 20g alcohol to slightly soaking state.Mixed powder is placed in mold, by control pressure through cold
Molded, cold moudling pressure is 30MPa, prepares sample.It is small that sample after molding is put into drying 4 in 100 DEG C of drying boxes
When, carbon-based composite phase-change energy storage material is obtained after being cooled to room temperature, repairing type.
Embodiment 3
The preparation method for present embodiments providing a kind of carbon-based composite phase-change energy storage material, includes the following steps:
1) 62.5g lithium carbonate is mixed with 187.5g potassium nitrate, is uniformly mixed and is placed in alumina crucible, in Muffle furnace
In heat 2h at 900 DEG C, obtain lithium carbonate-potassium nitrate fused salt mixt;
2) 30g potassium chloride (KCl) is added into fused salt mixt obtained in step 1) and is used as fluxing agent, in Muffle furnace
2h is heated at 800 DEG C, obtains the eutectics fused salt that fusing point is 430 DEG C (being obtained by differential thermal analysis);
3) low melting point eutectic fused salt obtained in step 2) is ground to 50 mesh hereinafter, being placed in ball grinder, be added
The graphene of 27.8g is ground with the revolving speed of 400r/min by ball milling, mixes 2h, and it is molten to obtain uniformly mixed graphene/eutectic
Salt powder.Wherein the partial size after graphene/fused salt mixt powder ball milling should be controlled in -50 mesh~+200 mesh;
4) graphene obtained in step 3)/eutectics fused salt powder is uniformly mixed with the expansible graphite of 102.6g, it should
Step is only immixture, adds 30g alcohol to slightly soaking state.Mixed powder is placed in mold, by control pressure through cold
Molded, cold moudling pressure is 30MPa, prepares sample.It is small that sample after molding is put into drying 4 in 100 DEG C of drying boxes
When, carbon-based composite phase-change energy storage material is obtained after being cooled to room temperature, repairing type.
The carbon-based composite phase-change energy storage material being prepared is tested as follows, after tested, three above embodiment obtains
The thermal coefficient of the carbon-based composite phase-change energy storage material arrived >=2Wm-1·K-1, show to significantly improve by graphene
The thermal coefficient of phase-changing energy storage material, and then improve heat storage efficiency.
Testing procedure is as follows,
(1) differential thermal analysis:
Using total obtained in step 2) of the STA409PC synchronous solving (German NETZSH company) to embodiment 1-3
The powder sample of brilliant fused salt carries out TG-DSC analysis, and powder sample quality is 11.504mg, which is placed to oxidation
In aluminium crucible, 600 DEG C are risen to by room temperature under an argon atmosphere, heating rate is 10 DEG C/min, after 7-8 hours, passes through the differential thermal
Analysis show that the fusing point of the eutectics fused salt of embodiment 1-3 is respectively 450 DEG C, 400 DEG C and 430 DEG C respectively;
(2) thermal coefficient:
It is measured respectively using 5000 type Conduction Coefficient Detector Basing of FLASHLINE (Anter corporation company of the U.S.) real
It applies the thermal diffusivity λ of the carbon-based composite phase-change energy storage material of a 1-3, uses Ar gas shielded in measurement process, temperature range 200~
600 DEG C, so be calculated its thermal coefficient >=2Wm-1·K-1。
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form.Base
It is obtained by those of ordinary skill in the art without making creative efforts every other in the embodiment of the present invention
Embodiment shall fall within the protection scope of the present invention.
Claims (15)
1. a kind of preparation method of carbon-based composite phase-change energy storage material, which comprises the steps of:
1) using lithium carbonate and potassium nitrate as raw material, 1-2h is heated at 750-900 DEG C after mixing, obtains lithium carbonate-nitric acid
The fused salt mixt of potassium;
2) potassium chloride is added into fused salt mixt obtained in step 1), heats 1-2h at 750-850 DEG C, it is total to obtain low melting point
Brilliant fused salt;
3) low melting point eutectic fused salt obtained in step 2) is ground to powdery, graphene is added, with turning for 300-400r/min
Speed grinds, mixes 2-3h, obtains uniformly mixed graphene/eutectics fused salt powder;
4) graphene obtained in step 3)/eutectics fused salt powder is uniformly mixed with expansible graphite matrix, 95wt% is added
Alcohol to the state of soaking, obtain uniform graphene/fused salt mixt powder;
5) graphene/fused salt mixt powder cold moudling will be obtained in step 4), obtains the sample of sheet;
6) sample obtained in step 5) is dried 4-6h hours at 100-120 DEG C, be cooled to after room temperature, repairing type obtain it is carbon-based
Composite phase-change energy storage material.
2. the preparation method of carbon-based composite phase-change energy storage material as described in claim 1, which is characterized in that wherein in step 1)
In, the mass ratio of the lithium carbonate and potassium nitrate is 1:1.5~4.
3. the preparation method of carbon-based composite phase-change energy storage material as claimed in claim 2, which is characterized in that wherein in step 1)
In, the mass ratio of the lithium carbonate and potassium nitrate is 1:2.
4. the preparation method of carbon-based composite phase-change energy storage material as described in claim 1, which is characterized in that wherein in step 2)
In, the quality of the potassium chloride accounts for the 10~15% of both fused salt mixt and potassium chloride gross mass.
5. the preparation method of carbon-based composite phase-change energy storage material as claimed in claim 4, which is characterized in that wherein in step 2)
In, the quality of the potassium chloride accounts for the 12% of both fused salt mixt and potassium chloride gross mass.
6. the preparation method of carbon-based composite phase-change energy storage material as described in claim 1, which is characterized in that wherein in step 2)
In, the melting temperature of the low melting point eutectic fused salt is 400-450 DEG C.
7. the preparation method of carbon-based composite phase-change energy storage material as described in claim 1, which is characterized in that wherein in step 3)
In, low melting point eutectic fused salt obtained in step 2) is ground to 50 mesh~+200 mesh powdery, the stone of -800 mesh of 400 mesh is added
Black alkene is ground with the revolving speed of 400r/min, mixes 2.5-3h, obtains uniformly mixed graphene/eutectics fused salt powder.
8. the preparation method of carbon-based composite phase-change energy storage material as claimed in claim 7, which is characterized in that wherein in step 3)
In, the quality of the graphene accounts for the 5%~15% of both low melting point eutectic fused salt and graphenes gross mass.
9. the preparation method of carbon-based composite phase-change energy storage material as claimed in claim 8, which is characterized in that wherein in step 3)
In, the quality of the graphene accounts for the 5~10% of both low melting point eutectic fused salt and graphenes gross mass.
10. the preparation method of carbon-based composite phase-change energy storage material as claimed in claim 9, which is characterized in that wherein in step
3) in, the graphene/eutectics fused salt powder size controlling is in 50 mesh~+200 mesh.
11. the preparation method of carbon-based composite phase-change energy storage material as described in claim 1, which is characterized in that wherein in step
4) in, the mass ratio of the graphene/eutectics fused salt powder and expansible graphite matrix is 3:1.
12. the preparation method of carbon-based composite phase-change energy storage material as described in claim 1, which is characterized in that wherein in step
5) in, the pressure of the cold moudling is 20~30MPa.
13. the preparation method of carbon-based composite phase-change energy storage material as claimed in claim 12, which is characterized in that wherein in step
5) in, the pressure of the cold moudling is 30MPa.
14. a kind of carbon-based composite phase-change energy storage material, which is characterized in that the carbon-based composite phase-change energy storage material is to pass through right
It is required that made from the described in any item methods of 1-13.
15. carbon-based composite phase-change energy storage material as claimed in claim 14, which is characterized in that the phase-changing energy storage material has
≥2W·m-1·K-1Thermal coefficient.
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CN114060781A (en) * | 2021-09-30 | 2022-02-18 | 深圳市联域光电股份有限公司 | Aluminum alloy heat dissipation cavity structure containing heat storage body for LED lamp and preparation method thereof |
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CN114060781A (en) * | 2021-09-30 | 2022-02-18 | 深圳市联域光电股份有限公司 | Aluminum alloy heat dissipation cavity structure containing heat storage body for LED lamp and preparation method thereof |
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