CN106854457A - A kind of polynary high-performance passes thermal storage and energy accumulation fused salt mixt and preparation method thereof - Google Patents
A kind of polynary high-performance passes thermal storage and energy accumulation fused salt mixt and preparation method thereof Download PDFInfo
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- CN106854457A CN106854457A CN201611198312.3A CN201611198312A CN106854457A CN 106854457 A CN106854457 A CN 106854457A CN 201611198312 A CN201611198312 A CN 201611198312A CN 106854457 A CN106854457 A CN 106854457A
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Abstract
The invention discloses one kind (LiNO3‑NaNO3‑KNO3‑Ca(NO3)2‑NaNO2) high-performance passes thermal storage and energy accumulation fused salt mixt and its compound method, the quality proportioning of five yuan of nitric acid components of molten salt is：LiNO3:1 20wt%；NaNO3:5 30wt%；KNO3:30 55wt%；Ca(NO3)2:1 10wt%；NaNO2:1 20wt%.Also disclose the preparation method of the fused salt mixt.Fused salt mixt of the present invention has that process for preparation is simple and easy to apply, fusing point is low, specific heat capacity is big, the features such as liquid warm area has good heat transfer property, and good thermal stability, the component stabilization under long-time high-temperature operation, it is a kind of excellent biography heat storage medium, it is adaptable to which solar energy power plant, chemical plant etc. use.
Description
Technical field
The present invention relates to physics heat transfer technical field of energy storage, more particularly to a kind of high-performance passes thermal storage and energy accumulation fused salt mixt material
Material and preparation method thereof.
Background technology
The world today faces energy shortage and problem of environmental pollution, and research and development new cleaning fuel technology is to the following mankind
Development it is extremely important.In numerous new energy, solar energy because its reserves " unlimitedness ", distribution generality, using spatter property,
Using advantages such as economy, the early research field for having been enter into people of heat generating is carried out using it.But solar energy is being developed, turned
During changing, transport and utilizing, there is quantity, form and temporal difference between the supply and demand of heat, it is necessary to take
Artificial process or technological means (heat-storing material) are stored and discharge heat, i.e. heat accumulation (energy) technology.Solar energy thermal-power-generating is profit
Scattered solar energy collecting is got up to any with condenser, by heat dump by solar absorption, then using heat transfer medium
Transfer heat to traditional TRT.It is that make use of the sun that solar energy thermal-power-generating is exactly with the difference of conventional Power Generation Mode
, first with heat sink by inside solar absorption to thermophore, then can be changed with water vapour again as the source of energy
Heat transfers heat away from being generated electricity.
Solar heat power generation system is broadly divided into slot type and tower two kinds, either slot type or tower-type electricity generation device, its
Heating-up temperature is all very high, is all up hundreds of to thousands of degree.And traditional heat transfer medium is difficult to bear such temperature, such as heat conduction
Oil mostly can only at most be heated to 380 DEG C or so, and temperature is crossed higher position and will be decomposed, this greatly limits the efficiency of Rankine cycle.
In addition, additional configuration accumulation of heat module is also needed to using the TRT of conduction oil, which increases the cost for generating electricity.
In order to further improve the operating temperature of steam turbine, the U.S., German some expert advices are in slot type of new generation warm
Using fuse salt as heat transfer medium in generating.They think that fuse salt has following excellent as the heat transfer medium of tank-type thermal power generation
Point：(1) operating temperature of steam turbine can be brought up to 450~500 DEG C by 393 DEG C of conduction oil, such that it is able to by Rankine
The efficiency of circulation improves 40% by the 37.6% of conduction oil；(2) it is constant in generating capacity due to improve the temperature of heat dump
In the case of, it is possible to reduce the volume and weight of energy-storage system；(3) fuse salt is compared with conduction oil, and price is low and will not be to ring
Border produces any harm.
The Molten Salt Heat Transfer heat storage owner for having been commercialized application will have：The Eurelios power stations and Hispanic of Italy
Hitec salt (the 7wt%NaNO that CESA-1 power stations use3- 53wt%KNO3- 40wt%NaNO2) as heat storage medium；Hitec bodies
It is 142 DEG C of fusing point, there is heat endurance below 454 DEG C, nitrogen can be needed with short-time duty to 538 DEG C, but during use
Protect to prevent the slow oxidation of nitrite component.The Solar two of California, USA use Solar salt
(60%NaNO3+ 40%KNO3) used as heat transfer heat storage medium, fusing point is 220 DEG C of 600 DEG C of maximum operation (service) temperatures, the power station runtime
Between do not occur big operational issue always；The molten salt system has good heat endurance and cheap cost, but due to it
Fusing point is too high, can exist during use and easily solidify and blocking pipeline causes equipment operating risk.
In sum, the commercialization fused salt that current solar generator enterprise uses has that fusing point is high, heat endurance is poor, long
Phase, these shortcomings constrained the development of solar photoelectric industry, urgently using the shortcomings of operating temperature range is narrow, cost is of a relatively high
Need technological break-through.
The content of the invention
Therefore, the technical problem to be solved in the present invention is to provide a kind of polynary high-performance and passes the hot material of thermal storage and energy accumulation fused salt mixt
Material.The invention solves the problems that another technical problem be to provide the polynary high-performance and pass thermal storage and energy accumulation fused salt mixt hot material
Preparation method.
The technical scheme is that, one kind (LiNO3-NaNO3-KNO3-Ca(NO3)2-NaNO2) polynary high-performance biography storage
Hot energy storage fused salt mixt, the fused salt particle be 50-100 mesh, including following mass percent component：
LiNO31-20%
NaNO35-30%
KNO330-55%
Ca(NO3)21-10%
NaNO21-20%.
Above-mentioned fused salt mixt system operating temperature is 86.8 DEG C~580 DEG C, under this temperature conditions, is operated 96 hours,
Loss is no more than 2%, much smaller than the fused salt formula that prior art is provided.
Anhydrous simple substance salt is complete in order to dry when preparing；Grinding sample preparation when fused salt Grain size controlling in 50-100 mesh, be for
Cause that mixture is sufficiently mixed while fineness is ensured, so as to ensure the accuracy of subsequent experimental.
Polynary high-performance of the invention passes thermal storage and energy accumulation fused salt mixt, it is preferred that including following mass percent
Component：
LiNO32-16%
NaNO315-30%
KNO330-55%
Ca(NO3)21-10%
NaNO21-20%.
Present invention also offers the preparation method that above-mentioned polynary high-performance passes thermal storage and energy accumulation fused salt mixt, mainly including following
Step：
A) simple substance dehydration of salt：
By Ca (NO3)2·4H2O is ground first, is then sieved so that the largest particles is less than 50 mesh, Ran Houfang
Enter in heater and dried 1-5 hour in 100-150 DEG C, be warming up to 250-350 DEG C of drying 8-12 hours, be transferred in drier
It is standby；
B) prepared by other anhydrous simple substance salt
By LiNO3、NaNO3、KNO3And NaNO2It is ground, then sieves, ensures all salt granularities 50~200
Mesh, above salt is put into heater, adjustment temperature be 100-150 DEG C prebake 8-12 hours, 150- is then warmed up to again
250 DEG C dry 8-12 hours, are put into standby in drying box；
C) preliminary mixing：
By LiNO3、NaNO3、KNO3、Ca(NO3)2And NaNO2Stainless steel is proportionally added into, macroscopic view is carried out to polybasic salt mixed
Close, polybasic salt is reached uniform mixing on a macroscopic scale；
D) microcosmic mixing is melted：
The uniform salt-mixture of micromixing is heated in heater, fused salt is heated first to be made inside heater
Temperature reaches 150-250 DEG C, after fused salt melts, fused salt mixt is kept this state 10-50 minutes, and then cooling down is to room
Temperature；
E) regrinding completes sample preparation：
The fused salt mixt solid that room temperature will be cooled to is regrind, and obtains the fused salt mixt particle of 50-100 mesh, so
Dry afterwards and seal this solid, that is, obtain high-performance and pass thermal storage and energy accumulation fused salt mixt.
In the preparation method of fused salt mixt of the invention, it is preferred that the step b) heaters are Electric heat oven.
In the preparation method of fused salt mixt of the invention, it is preferred that the step c) micromixings are using stirring, machine
One or two kinds of in tool rolling.
In the preparation method of fused salt mixt of the invention, it is preferred that step d) melts micro mixing according to such as
Lower step is carried out：
The uniform salt-mixture of micromixing is heated in Muffle furnace, during heating, is heated up with the speed of 10 DEG C/min,
Reach after 200 DEG C of thawings, fused salt mixt is kept for this state half an hour, room is then cooled to the speed of 10 DEG C/min
Temperature.
In the preparation method of fused salt mixt of the invention, it is preferred that the step d) heaters are Muffle furnace.
Other heaters can also, it is ensured that temperature, and Muffle furnace is therein a kind of preferred.
The present invention reduces fused salt mixt fusing point mechanism and is mainly：One-component fused salt fusing point is higher, and various fused salts are mixed
Get up to be formed to significantly reduce after eutectic fused salt mixt the fusing point of fused salt mixt, and in general, fused salt mixt component is more,
Fusing point is just relatively lower；Another one aspect, because Li, Na, K are homologue, belongs to alkali metal, and ionic condition has similar
Property, by five kinds of nitrate LiNO3-NaNO3-KNO3-Ca(NO3)2-NaNO2After mixing, increased alkaline-earth metal calcium ion energy
Enough and otheralkali metal nitrate forms new interionic active force, and the oxygen of nitrite and nitrate is suppressed to a certain extent
Change and decompose.Therefore, fused salt of the present invention has compared with low melting point, preferable heat endurance.
Fused salt mixt indices of the present invention are as follows：
Operating temperature range：87~590 DEG C；
Fusion temperature scope：About 87~140 DEG C；
Pyrolysis temperature range：590~650 DEG C
With LiNO disclosed in Chinese patent 00111406.93-KNO3-NaNO3-NaNO2System is compared, of the invention from mechanism
On have made intensive studies, it is proposed that new mechanism, while obtaining beneficial effect：
(1) fused salt mixt fusing point of the present invention is low, and its fusing point reduces nearly 110-160 DEG C, and heat decomposition temperature is also improved,
Expand operating temperature range；
(2) fused salt mixt heat endurance is high, and component volatilization is few in operating range.
(3) fused salt mixt thermal capacitance is larger, can pass heat storage medium as extensive；
(4) low cost, fused salt mixt each component is cheap；
(5) preparation method rationally, fused salt preparation process it is simple；
Brief description of the drawings
Fig. 1 is the DSC curve figure of the fused salt mixt of embodiment 1；
Fig. 2 is the TG curve maps of the fused salt mixt of embodiment 1；
Fig. 3 is the DSC curve figure of the fused salt mixt of embodiment 2；
Fig. 4 is the TG curve maps of the fused salt mixt of embodiment 2.
Specific embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Using STA449F3 types synchronous solving and SDT Q600 types synchronous solvings respectively to prepared by example
Five yuan of nitric acid congruent melting salt carry out DSC and TG tests under the rate of heat addition of 10K/min.
Embodiment 1
A kind of five yuan of nitric acid congruent melting salt, its component for including and constituent mass percentage are as follows：NaNO3, 30%；KNO3,
53%；LiNO3, 2%；Ca(NO3)2, 3%；NaNO2, 12%.
The embodiment fused salt mixt preparation method is：
1. weigh：
NaNO is weighed respectively according to above-listed proportioning3、Ca(NO3)2·4H2O、NaNO2、LiNO3、KNO3Required weight,
Place stand-by；
2. anhydrous simple substance salt is prepared：
By Ca (NO3)2·4H2O is ground first, is then sieved so that the largest particles is less than 50 mesh, Ran Houfang
Enter in Electric heat oven and dried 3 hours in 120 DEG C, baking oven is warming up into 300 DEG C dries 10 hours, is transferred to standby in drier；
By LiNO3、NaNO3、KNO3And NaNO2Grinding sieving in advance obtains the fine grained of 50~200 mesh, in Electric heat oven
In in 120 DEG C of prebake 12 hours, then be warmed up to 200 DEG C and dry 12 hours, NaNO is obtained3, KNO3, LiNO3And NaNO2It is anhydrous
Simple substance salt, is put into standby in drying box.
3. preliminary mixing：
Anhydrous simple substance salt 1.50g NaNO obtained in above-mentioned steps are taken respectively3, 2.65g KNO3, 0.10g LiNO3,
0.15g Ca(NO3)2With 0.60g NaNO2, material purity is equal>99%.Above-mentioned five kinds anhydrous simple substance salt are poured into a container,
With the method for machinery rolling, make up to uniform in macro-scale；
4. microcosmic mixing is melted：
Melt it heating in said mixture Muffle furnace, in heating process, heating-up temperature is since room temperature with 10
DEG C/speed of min carries out intensification and is heated to 300 DEG C or so, it is kept for this state half an hour, then with the speed of 10 DEG C/min
Rate slowly cools to normal temperature；
5. grind：
Gained solid abrasive will be cooled down to powdered, the fused salt mixt particle of 50~100 mesh will be obtained, be subsequently dried and sealed this
Solid, you can obtain described high-performance and pass thermal storage and energy accumulation fused salt mixt.
The DSC curve that obtains of test as shown in figure 1, test result shows, five yuan of nitric acid congruent melting salt exothermic peak starting points
Near 126.4 DEG C (i.e. fused salt fusing points), peak value is 137.9 DEG C；The TG curves that test is obtained are as shown in Fig. 2 in order to more accurate
Determination heat decomposition temperature, take the intersection point of extrapolated baseline and TG curves greatest gradient point tangent line for fused salt heat decomposition temperature (i.e.
Thermal stable temperature), Fig. 2 shows the thermogravimetric starting point of the fused salt near 590 DEG C, therefore the operation interval of the fused salt be 126.4~
590℃。
Embodiment 2
A kind of five yuan of nitric acid congruent melting salt, its component for including and constituent mass percentage are as follows：NaNO3, 15%；KNO3,
39%；LiNO3, 16%；Ca(NO3)2, 10%；NaNO2, 20%.
The embodiment fused salt mixt preparation method is：
1. weigh：
NaNO is weighed respectively according to above-listed proportioning3、Ca(NO3)2·4H2O、NaNO2、LiNO3、KNO3Required weight,
Place stand-by；
2. anhydrous simple substance salt is prepared：
By Ca (NO3)2·4H2O is ground first, is then sieved so that the largest particles is less than 50 mesh, Ran Houfang
Enter in Electric heat oven and dried 3 hours in 120 DEG C, baking oven is warming up into 300 DEG C dries 10 hours, is transferred to standby in drier；
By LiNO3、NaNO3、KNO3And NaNO2Grinding sieving in advance obtains the fine grained of 50~200 mesh, in Electric heat oven
In in 120 DEG C of prebake 12 hours, then be warmed up to 200 DEG C and dry 12 hours, NaNO is obtained3, KNO3, LiNO3And NaNO2It is anhydrous
Simple substance salt, is put into standby in drying box.
3. preliminary mixing：
Anhydrous simple substance salt 0.75g NaNO obtained in above-mentioned steps are taken respectively3, 1.95g KNO3, 0.80g LiNO3,
0.50g Ca(NO3)2With 1.00g NaNO2, material purity is equal>99%.Above-mentioned five kinds anhydrous simple substance salt are poured into a container,
With the method for machinery rolling, make up to uniform in macro-scale；
4. microcosmic mixing is melted：
Melt it heating in said mixture Muffle furnace, in heating process, heating-up temperature is since room temperature with 10
DEG C/speed of min carries out intensification and is heated to 300 DEG C or so, it is kept for this state half an hour, then with the speed of 10 DEG C/min
Rate slowly cools to normal temperature；
5. grind：
Gained solid abrasive will be cooled down to powdered, the fused salt mixt particle of 50~100 mesh will be obtained, be subsequently dried and sealed this
Solid, you can obtain described high-performance and pass thermal storage and energy accumulation fused salt mixt.
The DSC curve that obtains of test as shown in figure 3, test result shows, five yuan of nitric acid congruent melting salt exothermic peak starting points
Near 86.8 DEG C (i.e. fused salt fusing points), peak value is 93.6 DEG C；The TG curves that test is obtained are as shown in figure 4, in order to accurate
Determine heat decomposition temperature, take the intersection point of extrapolated baseline and TG curves greatest gradient point tangent line for the heat decomposition temperature of fused salt is (i.e. warm
Equilibrium temperature), Fig. 4 shows the thermogravimetric starting point of the fused salt near 580 DEG C, therefore the operation interval of the fused salt is 86.8~580
℃。
Embodiment 3
A kind of five yuan of nitric acid congruent melting salt, its component for including and constituent mass percentage are as follows：NaNO3, 25%；KNO3,
55%；LiNO3, 10%；Ca(NO3)2, 7%；NaNO2, 3%, it is 121.6 DEG C that fusing point is analyzed after tested, and heat decomposition temperature is 592
℃。
Embodiment 4
A kind of five yuan of nitric acid congruent melting salt, its component for including and constituent mass percentage are as follows：NaNO3, 20%；KNO3,
48%；LiNO3, 8%；Ca(NO3)2, 4%；NaNO2, 20%, it is 118.9 DEG C that fusing point is analyzed after tested, and heat decomposition temperature is 587
℃。
Fused salt mixt heat endurance of the invention is high, and component volatilization is few in operating range, and thermal capacitance is larger, can be as big rule
Mould passes heat storage medium；Low cost, fused salt mixt each component is cheap；Preparation method is reasonable, fused salt preparation process is simple, is beneficial to
Large-scale promotion.
Claims (7)
1. one kind (LiNO3-NaNO3-KNO3-Ca(NO3)2-NaNO2) polynary high-performance biography thermal storage and energy accumulation fused salt mixt, its feature
It is：The fused salt particle be 50-100 mesh, including following mass percent component：
LiNO31-20%
NaNO35-30%
KNO330-55%
Ca(NO3)21-10%
NaNO21-20%.
2. polynary high-performance as claimed in claim 1 passes thermal storage and energy accumulation fused salt mixt, it is characterised in that：Including following quality hundred
Divide the component of ratio：
LiNO32-16%
NaNO315-30%
KNO330-55%
Ca(NO3)21-10%
NaNO21-20%.
3. polynary high-performance passes the preparation method of thermal storage and energy accumulation fused salt mixt described in claim 1, it is characterised in that：Mainly include
Following steps：
A) simple substance dehydration of salt：
By Ca (NO3)2·4H2O is ground first, is then sieved so that the largest particles is less than 50 mesh, is then placed in adding
Dried 1-5 hours in 100-150 DEG C in thermal, be warming up to 250-350 DEG C and dry 8-12 hours, be transferred to standby in drier
With；
B) prepared by other anhydrous simple substance salt
By LiNO3、NaNO3、KNO3And NaNO2It is ground, then sieves, to ensure all salt granularities in 50~200 mesh, will be with
Upper salt is put into heater, adjustment temperature be 100-150 DEG C prebake 8-12 hours, 150-250 DEG C of baking is then warmed up to again
It is dry 8-12 hours, it is put into standby in drying box；
C) preliminary mixing：
By LiNO3、NaNO3、KNO3、Ca(NO3)2And NaNO2Stainless steel is proportionally added into, micromixing is carried out to polybasic salt,
Polybasic salt is set to reach uniform mixing on a macroscopic scale；
D) microcosmic mixing is melted：
The uniform salt-mixture of micromixing is heated in heater, fused salt is heated first makes heater internal temperature
Reach 150-250 DEG C, after fused salt melts, fused salt mixt is kept this state 10-50 minutes, then cooling down is to room temperature；
E) regrinding completes sample preparation：
The fused salt mixt solid that room temperature will be cooled to is regrind, and obtains the fused salt mixt particle of 50-100 mesh, Ran Hougan
Dry this solid of sealing, that is, obtain high-performance and pass thermal storage and energy accumulation fused salt mixt.
4. the preparation method of fused salt mixt as claimed in claim 3, it is characterised in that the step b) heaters are electric heating
Baking oven.
5. the preparation method of fused salt mixt as claimed in claim 3, it is characterised in that the step c) micromixings are using stirring
Mix, machinery rolling in one or two kinds of.
6. the preparation method of fused salt mixt as claimed in claim 3, it is characterised in that step d) fusings micro mixing is pressed
Carried out according to following steps：
The uniform salt-mixture of micromixing is heated in Muffle furnace, during heating, is heated up with the speed of 10 DEG C/min, reached
After 200 DEG C melt, fused salt mixt is kept for this state half an hour, room temperature is then cooled to the speed of 10 DEG C/min.
7. the preparation method of fused salt mixt as claimed in claim 3, it is characterised in that the step d) heaters are Muffle
Stove.
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Cited By (1)
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| CN108800276A (en) * | 2018-05-08 | 2018-11-13 | 李渊 | A kind of electric heat-storage device |
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Application publication date: 20170616 |