CN109796937A - A kind of major diameter phase-transition heat-storage particle and preparation method thereof - Google Patents
A kind of major diameter phase-transition heat-storage particle and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of major diameter phase-transition heat-storage particles and preparation method thereof.Its technical solution is: alusil alloy powder acid alternately being washed with the washing of deionized water alternating or with alkali and deionized water, with drying under the conditions of 60~200 DEG C in protective atmosphere, the modified alusil alloy powder in surface is made；The modified alusil alloy powder in face is placed in high-temperature atmosphere furnace again, successively to be successively heated to 550~650 DEG C, 700~800 DEG C, 850~950 DEG C, 1050~1250 DEG C and 1350~1500 DEG C under the conditions of 5~10 DEG C/min, 10~20 DEG C/min, 5~8 DEG C/min, the rate and corresponding furnace atmosphere of 3~5 DEG C/min and 5~10 DEG C/min, major diameter phase-transition heat-storage particle is made in natural cooling.The diameter of major diameter phase-transition heat-storage particle is 214~310 μm.Preparation process of the present invention is simple, at low cost and easy to industrialized production, and made product can improve the utilization rate and utilization efficiency of heat, uses temperature height.
Description
Technical field
The invention belongs to phase-transition heat-storage granule technology fields.More particularly to a kind of major diameter phase-transition heat-storage particle and its preparation
Method.
Background technique
Phase-transition heat-storage particle by phase-change material is core, covering material is that shell is constituted.Since phase-transition heat-storage particle is with no corruption
Become the hot spot of Recent study when corrosion, anti-dielectric leakage, thermal storage density be larger and phase transformation the advantages that constant temperature.
Phase-change material is classified by phase transition temperature, and wherein phase transition temperature is known as high-temperature phase-change in 500 DEG C or more of phase-change material
Material.Aluminium and alusil alloy belong to one of high-temperature phase change heat accumulation material, good, better heat stability, phase transformation with thermal conductivity
The advantages that latent heat is big, thermal coefficient is big and thermal storage density is high.If right using aluminium or alusil alloy as the core of phase-transition heat-storage particle
Covering material has following requirement: good corrosion resistance, and stability of period is good, and temperature stress intensity is high, good in oxidation resistance.
In recent years, some scholars have carried out some research aluminium and alusil alloy as phase change heat storage material, disclose one
Composite phase change heat-accumulation material containing aluminium or alusil alloy a bit.Such as " a kind of High-temperature composite phase-change heat storage and preparation method thereof "
(201310175016.1) patented technology, the technology use white clay, alumine and aluminium powder for raw material, are directly pressed into after mixing
A kind of High-temperature composite phase-change heat storage is made in type, high-temperature roasting；" a kind of cermet with phase-transition heat-storage function and its
Preparation method " (201310293700.X) patented technology is that sintering helps with magnesia using alusil alloy powder and schmigel as raw material
A kind of cermet with phase-transition heat-storage function is made through dry ball milling, molding and roasting in agent.Above-mentioned technical method is all
It is directly used in phase-change material as raw material in the preparation of composite phase change heat-accumulation material, using phase-change material when undergoing phase transition
Heat absorption and heat release, which are realized, stores heat release purpose.But the method for this direct mixed-forming aluminium or alusil alloy powder in roasting process is molten
It easily reveals and overflows after change, and the aluminium of liquid phase or alusil alloy can also reduce the high-temperature physical property of material.
There are also scholars to study the production of aluminium or alusil alloy phase-transition heat-storage particle: a kind of " Al/Al2O3It stores
Hot material and preparation method thereof " (201010127955.5) patented technology, it is cooling with oxygen atmosphere after atomization using aluminium powder as raw material
Method is prepared for Al2O3Wrap up the core-shell type composite phase change heat-accumulation material of Al powder.The composite phase change heat-accumulation material pair of such core-shell structure
Equipment requirement is high, preparation process is complicated and is difficult to control, and the shell of preparation is relatively thin, it is difficult to meet intensity requirement, and the grain of raw material
Diameter is smaller to cause dust pollution.
" a kind of high-temperature phase change heat accumulation microcapsules and preparation method thereof " (201710502031.0) patented technology, with the conjunction of aluminium silicon
Bronze is raw material, forms phase-transition heat-storage microcapsules green body after carrying out directly processing with phosphate dihydrogen aluminum solution, or green body is roasted
The high-temperature phase change heat accumulation microcapsules with fine and close shell are formed afterwards.The preparation method of such microcapsules is simple, but the grain of raw material
Diameter is smaller to have bonding between the microcapsules of preparation, it is difficult to meet to the demanding industrial application of dispersibility.
Summary of the invention
The present invention is directed to overcome prior art defect, it is therefore an objective to it is simple, at low cost and be easy to work to provide a kind of preparation process
The major diameter phase-transition heat-storage preparation method of granules that industry metaplasia produces；Prepared major diameter phase-transition heat-storage particle can improve the benefit of heat
With rate and utilization efficiency, temperature height is used.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that:
Step 1: alusil alloy powder acid and deionized water are alternately washed 1~10 time or use the alusil alloy powder
Alkali and deionized water alternately washing 1~10 time, then be placed in protective atmosphere, dry 3~12h, is made under the conditions of 60~200 DEG C
Surface is modified alusil alloy powder.
Step 2: the modified alusil alloy powder in the surface is first placed in high-temperature atmosphere furnace, according still further to following six stages
Heating cycle and corresponding furnace atmosphere are roasted, then cooled to room temperature, and major diameter phase-transition heat-storage particle is made.Greatly
The diameter of diameter phase-transition heat-storage particle is 214~310 μm.
The heating cycle of first stage is with the rate of 5~10 DEG C/min by room temperature to the first temperature；In the furnace
Atmosphere is steam atmosphere, and the entrance gauge pressure of the vapor is 0.01~0.9MPa, and temperature is before the entrance of the vapor
110~170 DEG C, the flow of the vapor is 3~5L/min.
The heating cycle of second stage is to be warming up to second temperature by the first temperature with the rate of 10~20 DEG C/min；It is described
Furnace atmosphere is air atmosphere.
The heating cycle of phase III is to be warming up to third temperature by second temperature with the rate of 5~8 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.01~0.05Mpa.
The heating cycle of fourth stage is to be warming up to the 4th temperature by third temperature with the rate of 3~5 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.05~0.1Mpa.
The heating cycle in the 5th stage is to be warming up to the 5th temperature by the 4th temperature with the rate of 5~10 DEG C/min；It is described
Furnace atmosphere is oxidizing atmosphere, 0.1~0.5Mpa of furnace pressure.
The heating cycle in the 6th stage is 30~180min of heat preservation under the conditions of five temperature, and the furnace atmosphere is air
Atmosphere.
First temperature be 550~650 DEG C, the second temperature be 700~800 DEG C, the third temperature be 850~
950 DEG C, the 4th temperature is 1050~1250 DEG C, and the 5th temperature is 1350~1500 DEG C.
The partial size of the alusil alloy powder is 50~300 μm, and the Si content in alusil alloy powder is 0.1~44wt%.
The pH value of the acid is 3~5.
The pH value of the alkali is 9~11.
The protective atmosphere is argon gas or is nitrogen atmosphere.
The oxidizing atmosphere is O2Content is greater than the oxygen-enriched air atmosphere of 21Vol%.
The present invention has following good effect compared with prior art:
The washing of alusil alloy powder is placed on drying in protective atmosphere by the present invention, then is placed in high-temperature atmosphere furnace, successively with 5
~10 DEG C/min, 10~20 DEG C/min, 5~8 DEG C/min, in the rate and corresponding furnace of 3~5 DEG C/min and 5~10 DEG C/min
Atmosphere is successively heated to corresponding temperature, cooled to room temperature；Major diameter phase-transition heat-storage particle is made；Therefore the present invention prepares work
Skill is simple, at low cost and be easy to industrial production.
The aluminium in alusil alloy that the present invention uses easily reacts with vapor for amphiprotic substance and generates aluminium hydroxide；
Again due to the dispersed distribution of aluminium and silicon in alusil alloy, so that the aluminium hydroxide that reaction generates not will form dense film and hinder
The further progress of reaction.Therefore, after alusil alloy places a period of time in vapor, surface will form aluminium hydroxide.?
Under hot conditions, aluminium hydroxide, which decomposes, generates aluminium oxide, forms aluminium oxide shell, and be wrapped in alusil alloy powder surface, obtains
Alusil alloy is core, aluminium oxide is shell with core-shell structure phase-transition heat-storage particle.Aluminium oxide has intensity big, high temperature resistant, resistance to
The advantages that molten aluminum corrodes, prepared major diameter phase-transition heat-storage particle long service life are corroded using the high and resistance to molten aluminum of temperature；Cause
This can effectively prevent the leakage after alusil alloy melts at high temperature, avoid the loss and corrosion resulting from of alusil alloy.
The alusil alloy powder diameter that the present invention uses for 50~300 μm, the diameter of major diameter phase-transition heat-storage particle obtained is 214~
310 μm, in identical shell thickness, the heat storage performance of major diameter phase-transition heat-storage particle is higher, improves heat utilization ratio and benefit
Use efficiency.
Therefore, preparation process of the present invention is simple, at low cost and easy to industrialized production, prepared with composite shell
Phase-transition heat-storage particle can improve the utilization rate and utilization efficiency of heat, use temperature height；It is able to satisfy solar plant, industrial furnace
With the heat utilization of hot industry exhaust gas.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limitation of its protection scope.
In present embodiment:
The pH value of the acid is 3~5；The pH value of the alkali is 9~11；O in the oxidizing atmosphere2Content is greater than
21Vol%；The diameter of the major diameter phase-transition heat-storage particle is 214~310 μm.
It is repeated no more in embodiment.
Embodiment 1
A kind of major diameter phase-transition heat-storage particle and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1: by alternately washing 1~5 time of alusil alloy powder acid and deionized water, then be placed in protective atmosphere, 60
The modified alusil alloy powder in surface is made in dry 3~7h under the conditions of~120 DEG C.
Step 2: the modified alusil alloy powder in the surface is first placed in high-temperature atmosphere furnace, according still further to following six stages
Heating cycle and corresponding furnace atmosphere are roasted, then cooled to room temperature, and major diameter phase-transition heat-storage particle is made.
The heating cycle of first stage is with the rate of 5~7 DEG C/min by room temperature to the first temperature；Gas in the furnace
Atmosphere is steam atmosphere, and the entrance gauge pressure of the vapor is 0.01~0.3MPa, and temperature is 110 before the entrance of the vapor
~170 DEG C, the flow of the vapor is 3~5L/min.
The heating cycle of second stage is to be warming up to second temperature by the first temperature with the rate of 10~14 DEG C/min；It is described
Furnace atmosphere is air atmosphere.
The heating cycle of phase III is to be warming up to third temperature by second temperature with the rate of 5~8 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.01~0.05Mpa.
The heating cycle of fourth stage is to be warming up to the 4th temperature by third temperature with the rate of 3~5 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.05~0.1Mpa.
The heating cycle in the 5th stage is to be warming up to the 5th temperature by the 4th temperature with the rate of 5~10 DEG C/min；It is described
Furnace atmosphere is oxidizing atmosphere, 0.1~0.5Mpa of furnace pressure.
The heating cycle in the 6th stage is 30~180min of heat preservation under the conditions of five temperature, and the furnace atmosphere is air
Atmosphere.
First temperature is 550~590 DEG C；The second temperature is 700~740 DEG C；The third temperature be 850~
890℃；4th temperature is 1050~1160 DEG C；5th temperature is 1350~1410 DEG C.
The partial size of the alusil alloy powder is 50~140 μm, and the Si content in alusil alloy powder is 0.1~15wt%.
The protective atmosphere is argon gas.
Embodiment 2
A kind of major diameter phase-transition heat-storage particle and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1: by alternately washing 3~8 times of alusil alloy powder alkali and deionized water, then be placed in protective atmosphere,
The modified alusil alloy powder in surface is made in dry 6~10h under the conditions of 100~160 DEG C.
Step 2: the modified alusil alloy powder in the surface is first placed in high-temperature atmosphere furnace, according still further to following six stages
Heating cycle and corresponding furnace atmosphere are roasted, then cooled to room temperature, and major diameter phase-transition heat-storage particle is made.
The heating cycle of first stage is with the rate of 6.5~8.5 DEG C/min by room temperature to the first temperature；The furnace
Interior atmosphere is steam atmosphere, and the entrance gauge pressure of the vapor is 0.3~0.6MPa, and temperature is before the entrance of the vapor
110~170 DEG C, the flow of the vapor is 3~5L/min.
The heating cycle of second stage is to be warming up to second temperature by the first temperature with the rate of 13~17 DEG C/min；It is described
Furnace atmosphere is air atmosphere.
The heating cycle of phase III is to be warming up to third temperature by second temperature with the rate of 5~8 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.01~0.05Mpa.
The heating cycle of fourth stage is to be warming up to the 4th temperature by third temperature with the rate of 3~5 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.05~0.1Mpa.
The heating cycle in the 5th stage is to be warming up to the 5th temperature by the 4th temperature with the rate of 5~10 DEG C/min；It is described
Furnace atmosphere is oxidizing atmosphere, 0.1~0.5Mpa of furnace pressure.
The heating cycle in the 6th stage is 30~180min of heat preservation under the conditions of five temperature, and the furnace atmosphere is air
Atmosphere.
First temperature is 580~620 DEG C；The second temperature is 730~770 DEG C；The third temperature be 880~
910℃；4th temperature is 1150~1210 DEG C；5th temperature is 1400~1460 DEG C.
The partial size of the alusil alloy powder is 130~220 μm, and the Si content in alusil alloy powder is 15~30wt%.
The protective atmosphere is nitrogen atmosphere.
Embodiment 3
A kind of major diameter phase-transition heat-storage particle and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1: by alternately washing 6~10 times of alusil alloy powder alkali and deionized water, then be placed in protective atmosphere,
The modified alusil alloy powder in surface is made in dry 9~12h under the conditions of 140~200 DEG C.
Step 2: the modified alusil alloy powder in the surface is first placed in high-temperature atmosphere furnace, according still further to following six stages
Heating cycle and corresponding furnace atmosphere are roasted, then cooled to room temperature, and major diameter phase-transition heat-storage particle is made.
The heating cycle of first stage is with the rate of 8~10 DEG C/min by room temperature to the first temperature；In the furnace
Atmosphere is steam atmosphere, and the entrance gauge pressure of the vapor is 0.6~0.9MPa, and temperature is before the entrance of the vapor
110~170 DEG C, the flow of the vapor is 3~5L/min.
The heating cycle of second stage is to be warming up to second temperature by the first temperature with the rate of 16~20 DEG C/min；It is described
Furnace atmosphere is air atmosphere.
The heating cycle of phase III is to be warming up to third temperature by second temperature with the rate of 5~8 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.01~0.05Mpa.
The heating cycle of fourth stage is to be warming up to the 4th temperature by third temperature with the rate of 3~5 DEG C/min；The furnace
Interior atmosphere is oxidizing atmosphere, and furnace pressure is 0.05~0.1Mpa.
The heating cycle in the 5th stage is to be warming up to the 5th temperature by the 4th temperature with the rate of 5~10 DEG C/min；It is described
Furnace atmosphere is oxidizing atmosphere, 0.1~0.5Mpa of furnace pressure.
The heating cycle in the 6th stage is 30~180min of heat preservation under the conditions of five temperature, and the furnace atmosphere is air
Atmosphere.
First temperature is 610~650 DEG C；The second temperature is 760~800 DEG C；The third temperature be 920~
950℃；4th temperature is 1200~1250 DEG C；5th temperature is 1450~1500 DEG C.
The partial size of the alusil alloy powder is 210~300 μm, and the Si content in alusil alloy powder is 30~44wt%.
The protective atmosphere is argon atmosphere.
Present embodiment has following good effect compared with prior art:
The washing of alusil alloy powder is placed on drying in protective atmosphere by present embodiment, then is placed in high-temperature atmosphere furnace
It is interior, successively with 5~10 DEG C/min, 10~20 DEG C/min, 5~8 DEG C/min, the rate of 3~5 DEG C/min and 5~10 DEG C/min and
Corresponding furnace atmosphere is successively heated to corresponding temperature, cooled to room temperature；Major diameter phase-transition heat-storage particle is made；Therefore this
Specific embodiment preparation process is simple, at low cost and be easy to industrial production.
The aluminium in alusil alloy that present embodiment uses easily reacts with vapor for amphiprotic substance and generates hydrogen
Aluminium oxide；Again due to the dispersed distribution of aluminium and silicon in alusil alloy, so that the aluminium hydroxide that reaction generates not will form dense thin
Film and hinder reaction further progress.Therefore, after alusil alloy places a period of time in vapor, surface will form hydrogen-oxygen
Change aluminium.Under the high temperature conditions, aluminium hydroxide, which decomposes, generates aluminium oxide, forms aluminium oxide shell, and be wrapped in alusil alloy powder table
Face, obtain alusil alloy be core, aluminium oxide be shell have core-shell structure phase-transition heat-storage particle.Aluminium oxide has intensity big, resistance to
The advantages that high temperature, resistance to molten aluminum corrode, prepared major diameter phase-transition heat-storage particle long service life use the high and resistance to molten aluminum of temperature
It corrodes；Therefore it can effectively prevent the leakage after alusil alloy melts at high temperature, avoid the loss of alusil alloy and thereby result in
Corrosion；The alusil alloy powder diameter that present embodiment uses is 50~300 μm, major diameter phase-transition heat-storage particle obtained
Diameter be 214~310 μm, in identical shell thickness, the heat storage performance of major diameter phase-transition heat-storage particle is higher, improves heat
Measure utilization rate and utilization efficiency.
Therefore, present embodiment preparation process is simple, at low cost and easy to industrialized production, and prepared having is multiple
The phase-transition heat-storage particle for closing shell can improve the utilization rate and utilization efficiency of heat, use temperature height；Be able to satisfy solar plant,
The heat recovery of industrial furnace high-temperature heat exchange and hot industry exhaust gas.
Claims (7)
1. a kind of preparation method of major diameter phase-transition heat-storage particle, it is characterised in that the step of preparation method is:
Step 1: by alusil alloy powder acid and deionized water alternately washing 1~10 time or by the alusil alloy powder alkali and
Deionized water alternately washing 1~10 time, then be placed in protective atmosphere, dry 3~12h, is made surface under the conditions of 60~200 DEG C
Modified alusil alloy powder；
Step 2: the modified alusil alloy powder in the surface is first placed in high-temperature atmosphere furnace, according still further to the heating in following six stages
System and corresponding furnace atmosphere are roasted, then cooled to room temperature, and major diameter phase-transition heat-storage particle is made；
The heating cycle of first stage is with the rate of 5~10 DEG C/min by room temperature to the first temperature；The furnace atmosphere
For steam atmosphere, the entrance gauge pressure of the vapor is 0.01~0.9MPa, before the entrance of the vapor temperature be 110~
170 DEG C, the flow of the vapor is 3~5L/min；
The heating cycle of second stage is to be warming up to second temperature by the first temperature with the rate of 10~20 DEG C/min；In the furnace
Atmosphere is air atmosphere；
The heating cycle of phase III is to be warming up to third temperature by second temperature with the rate of 5~8 DEG C/min；Gas in the furnace
Atmosphere is oxidizing atmosphere, and furnace pressure is 0.01~0.05Mpa；
The heating cycle of fourth stage is to be warming up to the 4th temperature by third temperature with the rate of 3~5 DEG C/min；Gas in the furnace
Atmosphere is oxidizing atmosphere, and furnace pressure is 0.05~0.1Mpa；
The heating cycle in the 5th stage is to be warming up to the 5th temperature by the 4th temperature with the rate of 5~10 DEG C/min；In the furnace
Atmosphere is oxidizing atmosphere, 0.1~0.5Mpa of furnace pressure；
The heating cycle in the 6th stage is 30~180min of heat preservation under the conditions of five temperature, and the furnace atmosphere is air gas
Atmosphere；
First temperature is 550~650 DEG C, and the second temperature is 700~800 DEG C, and the third temperature is 850~950
DEG C, the 4th temperature is 1050~1250 DEG C, and the 5th temperature is 1350~1500 DEG C.
2. the preparation method of major diameter phase-transition heat-storage particle according to claim 1, it is characterised in that the alusil alloy
The partial size of powder is 50~300 μm, and the Si content in alusil alloy powder is 0.1~44wt%.
3. the preparation method of major diameter phase-transition heat-storage particle according to claim 1, it is characterised in that the pH value of the acid
It is 3~5.
4. the preparation method of major diameter phase-transition heat-storage particle according to claim 1, it is characterised in that the pH value of the alkali
It is 9~11.
5. the preparation method of major diameter phase-transition heat-storage particle according to claim 1, it is characterised in that the protective atmosphere
It for argon gas or is nitrogen atmosphere.
6. the preparation method of major diameter phase-transition heat-storage particle according to claim 1, it is characterised in that the oxidizing atmosphere
For O2Content is greater than the oxygen-enriched air atmosphere of 21Vol%.
7. a kind of major diameter phase-transition heat-storage particle, it is characterised in that the major diameter phase-transition heat-storage particle is according to claim 1
Major diameter phase-transition heat-storage particle prepared by the preparation method of major diameter phase-transition heat-storage particle described in any one of~6；
The diameter of the major diameter phase-transition heat-storage particle is 214~310 μm.
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| CN112371064A (en) * | 2020-10-20 | 2021-02-19 | 武汉科技大学 | Phase change heat storage microcapsule with frame shear wall shell structure and preparation method thereof |
| CN112589092A (en) * | 2020-12-08 | 2021-04-02 | 武汉科技大学 | High-temperature phase change heat storage composite material and preparation method thereof |
| CN114717437A (en) * | 2021-10-11 | 2022-07-08 | 中国矿业大学 | Preparation method and application of aluminum-based metal high-temperature phase change heat storage composite material |
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