CN104109508B - Nitrate-system molten salt heat storage material and preparation method thereof - Google Patents
Nitrate-system molten salt heat storage material and preparation method thereof Download PDFInfo
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- CN104109508B CN104109508B CN201410306984.6A CN201410306984A CN104109508B CN 104109508 B CN104109508 B CN 104109508B CN 201410306984 A CN201410306984 A CN 201410306984A CN 104109508 B CN104109508 B CN 104109508B
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Abstract
The invention provides a nitrate-system molten salt heat storage material and a preparation method thereof. The nitrate-system molten salt heat storage material comprises potassium nitrate and sodium nitrate, wherein a mass ratio of sodium nitrate to potassium nitrate is 30-70: 30-70, and the contents of impurity ions consisting of Ca＜2+＞, Mg＜2+＞, Cl＜-＞ and SO4＜2-＞ in potassium nitrate and sodium nitrate are respectively less than 100 ppm, 100 ppm, 200 ppm and 300 ppm. Compared with the prior art, no other component or additive is needed, the preparation method is simple and easily practicable, an obvious cost advantage is obtained, and the nitrate-system molten salt heat storage material and the preparation method thereof are of important significance to promotion of rapid development of the photo-thermal power generation field and reduction of cost for photo-thermal power generation.
Description
Technical field
The present invention relates to energy field, and in particular to a kind of nitric acid salt system fused salt heat accumulating and preparation method thereof.
Background technology
Global traditional energy is limited, it is contemplated that existing oil can only exploit about 41 years, natural gas for exploitation 67 years, coal for exploitation
192 years, therefore new energy technology becomes the strategic energy technology for ensureing China's sustainable development of socio-economy.The wherein sun
Energy heat utilization technology, as emerging energy technology, is the prior development direction of country's ENERGY PLANNING during " 12 ",
It is the major technical fields for advancing " energy saving and efficiency increasing " strategy.Using sun heat radiation energy, by optically focused heating working medium, finally obtain
High temperature and high pressure steam promotes Turbo-generator Set to generate electricity, the features such as with efficiency high, cleaning, zero carbon emission.But due to receiving
To the impact of solar radiation variations, traditional coal fired power generation is compared, the stability and continuity of solar energy thermal-power-generating is poor.Solve this
The best approach of one problem is the solar heat of absorption to be stored realization long-time, stable released by heat-storage technology
Put, final continuous, the stable electric generation for realizing being independent of solar radiation variations.
The high-performance heat accumulating that can be applicable to solar energy thermal-power-generating is prepared, is to improve solar energy thermal-power-generating efficiency, promote
Enter the important research direction of hot power generating industry development.China Salt Lake Area, particularly Chaidamu of Qinghai Province salt lake are rich in potassium, sodium
Deng salts resources, if with the rich sylvite for producing in salt lake and sodium salt as raw material, preparing the nitric acid salt system with excellent properties
Fused salt heat accumulating, the accumulation of heat for being applied to solar energy generate electricity, and will not only lift the value of China's salt lake resources, improve economical
Income, and can drive and lead the development of solar energy thermal-power-generating industry.
Unanimously think that nitrate fused salt heat accumulating is that a kind of heat accumulation with very strong application potential is situated between at present both at home and abroad
Matter, with high specific heat, low-corrosiveness, compared with operation at high temperature the features such as.But, nitrate fused salt heat accumulating is sent out in solar heat
The commercial application difficulty of electricity is larger, and the successful example in global range is fewer, hinders the industry of fused salt fused salt heat accumulating
Change application main cause be embodied in it is following some：
(1) freezing point (or fusing point) temperature of nitrate fused salt heat accumulating is higher, such as common Solar Salts bodies
System (NaNO3/KNO3:60/40) fusing point is 238 DEG C, if heat generating system part pipeline is not enough or warm due to mirror field energy
Degree skewness, is easily caused molten salt system solidification and forms " frozen pipe " phenomenon；In order to avoid the generation of this phenomenon, power station
Addition temperature compensation means is generally required in running to guarantee freezing point of the line temperature higher than molten salt system, so increasing
Energy ezpenditure, improve cost of electricity-generating.
(2) the use temperature range of existing fused salt heat accumulating is narrower so that the energy conversion of system is less efficient.Such as
HITEC Salt system (NaNO3/KNO3/NaNO2:7/53/40) fusing point relatively low (142 DEG C), but its decomposition temperature is relatively low is
535℃.Limiting one of solar energy thermal-power-generating " bottleneck " for making a breakthrough at this stage, cannot exactly to obtain fusing point low, but decomposes temperature
The higher fused salt heat accumulating of degree.
(3) heat endurance and corrosivity of fused salt heat accumulating are to be improved.The electricity of current country's solar energy thermal-power-generating
Valency is 1.5 yuan/kwh, and cost of electricity-generating is high.The reason for causing relatively costly, except above-mentioned heat accumulating fusing point is high, use temperature
It is low cause conversion efficiency of thermoelectric relatively low outside, the heat endurance of fused salt heat accumulating is poor, service life is short and to system equipment
Corrosion etc. also increase the material cost of correlation.
So can be used for the preferable heat accumulating of solar energy thermal-power-generating, should possess low melting point, high specific heat capacity, suitable material
The features such as density, excellent thermal stability and relatively low corrosivity, this is also the emphasis of those skilled in the art's research and development.
In order that heat accumulating meets above-mentioned performance, it is existing in terms of the fusing point currently for reduction fused salt heat accumulating
Substantial amounts of research work.In order to reduce the fusing point of Solar Salts systems, the patent of invention of Publication No. CN101050355A is public
A kind of fusion tray of thermal transmission and storage medium and preparation method thereof is opened, the heat transfer heat storage medium of introduction includes potassium nitrate, sodium nitrate, Asia
Sodium nitrate and additive, wherein additive are mainly made up of cesium nitrate and potassium chloride.Although the method can be prepared having
Compared with the fused salt heat accumulating of low melting point and preferable heat endurance, but the cesium nitrate in additive is relatively costly, and potassium chloride
Addition can increase corrosion of the heat-storage medium to equipment and pipeline material, be unfavorable for reality of the medium in solar-thermal generating system
Using.
The patent of invention of Publication No. CN102533226A discloses a kind of nitric acid fusion tray of thermal transmission and storage medium and its system
Preparation Method and application, the heat-storage medium of the disclosure of the invention is, on the basis of sodium nitrate, potassium nitrate mixed salt, to the addition of a certain amount of
What calcium nitrate was prepared from, the medium fusing point can as little as 120 DEG C.The patent of invention of Publication No. CN103074040A discloses one
Low melting point fused salt mixt heat transfer heat storage medium is planted, the medium is by 10wt% calcium nitrate, 60-70wt% potassium nitrate, 10-20wt% nitre
Sour sodium, 10wt% natrium nitrosums composition, about 130 DEG C or so of the fusing point.Both the above heat-storage medium is by adding calcium nitrate, Asia
Sodium nitrate component, having reached reduces the purpose of eutectic temperature, but wherein the addition of calcium nitrate and natrium nitrosum will increase storage
The corrosivity of thermal medium, and the requirement to system atmosphere is improved, increase operating cost.Therefore, by a kind of simple and effective system
Preparation Method, the fusing point that Solar Salt systems are reduced while ensureing with high decomposition temperature are very important.
The content of the invention
It is an object of the invention to provide a kind of process is simple, energy consumption are low, low cost, with low melting point, high heat stability
Property nitric acid salt system fused salt heat accumulating and preparation method thereof；The heat accumulating prepared using the method, should ensure
There is under the premise of higher decomposition temperature relatively low fusing point and low-corrosiveness, and there should be very excellent heat endurance, can make
Accumulation of heat/heat transfer medium for heat generating system is applied to solar energy thermal-power-generating field.
The nitric acid salt system fused salt heat accumulating that the present invention is provided is made up of potassium nitrate and sodium nitrate, the sodium nitrate and nitre
The mass ratio of sour potassium is 30～70：30～70, the Ca in the potassium nitrate and sodium nitrate2+、Mg2+、Cl-、SO4 2-Foreign ion contains
Amount is respectively smaller than 100ppm, 100ppm, 200ppm, 300ppm.
Preferably, Ca2+、Mg2+、Cl-、SO4 2-Impurity ion content be respectively 5～50ppm, 10～60ppm, 50～
200ppm, 100～250ppm.
Preferably, the mass ratio of the sodium nitrate and potassium nitrate is 60：40.
Present invention also offers a kind of preparation method of fused salt heat accumulating, including：
(1) potassium nitrate and sodium nitrate are purified, and by the sodium nitrate and potassium nitrate after purification according to 30～70：30～70 ratio
Example mixing, obtains just batch mixing.
The raw material (sodium nitrate and potassium nitrate) for preparing nitric acid salt system fused salt heat accumulating are purified, is adopted
Sodium nitrate and potassium nitrate are the primary product that technical grade or agricultural grade, or salt field process are obtained.
Preferably, the purification is at ambient temperature, sodium nitrate and potassium nitrate to be dissolved separately in deionized water, is made
Obtain solution concentration (mass fraction of solute) and be respectively 15%～45%, 10%～35%；Respectively under agitation, in evaporation
Be evaporated in vessel, treat that solution concentration is respectively reached after 50%～65%, 45%～60%, carry out crystallisation by cooling, drip washing,
The sodium nitrate being dried after being purified respectively and potassium nitrate.The purification step is carried out 1～3 time, until the Ca in solution2+、Mg2 +、Cl-、SO4 2-Impurity ion content is respectively 5～50ppm, 10～60ppm, 50～200ppm, 100～250ppm.
Preferably, the hybrid mode is：Two kinds of crystalline powder raw materials are put into into mortar or other smash and physics
In blending equipment, sufficiently crushed, stirred, using mechanism so that both reach a certain degree of being uniformly dispersed.Jing
A certain amount of heat accumulating just batch mixing is obtained after the step for crossing.
(2) just batch mixing carries out high-temperature heat treatment under the conditions of 400～500 DEG C to the heat accumulating for obtaining above-mentioned steps.
Preferably, described heat treatment is：The vessel for filling just batch mixing are placed in and can be heated in the high temperature furnace with temperature control,
With the heating rate of 5～20 DEG C/min to 400～500 DEG C afterwards, be incubated 20～60min；After insulation terminates, room is cooled to
Temperature；Above-mentioned heating process 2～5 times is repeated afterwards；The heat accumulating that room temperature obtains luming is finally cooled to, by its pulverising mill
The nitric acid salt system fused salt heat accumulating with low melting point of powder can carefully be obtained.Repeat-heating in the step for passing through
Dissolving, crystallisation by cooling process, sodium nitrate and potassium nitrate raw material can reach highly uniform blending state, be conducive to obtaining high property
Can heat accumulating.
The present invention based on solar salt systems, by sodium nitrate, the purifying technique of potassium nitrate raw material and miscellaneous
Matter ionic control, and finally control impurity ion content scope：Ca2+For 5～50ppm, Mg2+For 10～60ppm, Cl-For 50～
200ppm、SO4 2-For 100～250ppm, on the premise of ensureing compared with high decomposition temperature so that heat accumulating fusing point is substantially reduced,
And the heat endurance of solar salt system fused salt heat accumulatings is improved, and these problems are to be difficult solution by prior art
Certainly, or need to add what a certain amount of high cost additive can just be addressed；The present invention also extends heat accumulation material
Service life and operating cost.
The present invention without other components and any additive, is made based on lower-cost solar salt systems
Standby process is simple, feasible, with obviously cost advantage, this is for promoting developing rapidly, reducing for photo-thermal power generation field
Photo-thermal power generation cost has very important significance.
Description of the drawings
Material differential scanning thermometric analysis (DSC) result in Fig. 1, embodiment；
Material thermogravimetic analysis (TGA) (TG) result in Fig. 2, embodiment；
Material heat endurance experimental results in Fig. 3, embodiment.
Specific embodiment
The preferred embodiment of the application is the following is, which is used only as explanation of the invention rather than restriction.
Embodiment
(1) raw material purification
At ambient temperature, 2000g sodium nitrate (technical grade) and 800g potassium nitrate (technical grade) are dissolved in into deionized water
In so that solution concentration (mass fraction of solute) is respectively 45.0% and 25.0%；Respectively under agitation, in evaporimeter
It is evaporated in ware, treats that solution concentration respectively reaches and crystallize, drip washing, be dried point
Sodium nitrate 360.0g that Huo get be after primary purification and potassium nitrate 187.0g.
(2) foreign ion control
The operation of repeat the above steps (1) obtains the sodium nitrate 13.5g and potassium nitrate of secondary purification for 3 times afterwards, finally
11.0g.Wherein Ca in sodium nitrate2+、Mg2+、Cl-And SO4 2-Impurity ion content is 15ppm, 20ppm, 80ppm and 120ppm；Nitre
Ca in sour potassium2+、Mg2+、Cl-、SO4 2-Impurity ion content is 10ppm, 25ppm, 80ppm and 150ppm.
(3) physical blending
The sodium nitrate 12.0g and potassium nitrate 8.0g of above-mentioned acquisition are blended in mortar, are ground through sufficiently, stirred
Heat accumulating just batch mixing 20.0g is obtained after mixing.
(4) high-temperature process
By above-mentioned 20.0g, just batch mixing is poured in diamond spar crucible, and high-temperature process is carried out in Muffle furnace, adding with 10 DEG C/min
Hot speed is incubated 60min after being heated to 500 DEG C；After insulation terminates, room temperature is cooled to；Above-mentioned heating process 3 is repeated afterwards
It is secondary；The heat accumulating that room temperature obtains luming is finally cooled to, the levigate nitric acid salt system fused salt storage for obtaining powder is crushed
Hot material.
Comparative example
In the present embodiment, sodium nitrate and potassium nitrate raw material are directly made without purification and the rate-determining steps of foreign ion
Fused salt heat accumulation material is prepared through physical blending, high temperature processing step with sodium nitrate (technical grade) and potassium nitrate (technical grade)
Material.
(1) physical blending
Sodium nitrate (technical grade) 12.0g and potassium nitrate (technical grade) 8.0g are blended in mortar, through sufficient
Heat accumulating just batch mixing 20.0g is obtained after grinding, stirring.
(2) high-temperature process
By above-mentioned 20.0g, just batch mixing is poured in diamond spar crucible, and high-temperature process is carried out in Muffle furnace, adding with 10 DEG C/min
Hot speed is incubated 60min after being heated to 500 DEG C；After insulation terminates, room temperature is cooled to；Above-mentioned heating process 3 is repeated afterwards
It is secondary；The heat accumulating that room temperature obtains luming is finally cooled to, the levigate nitric acid salt system fused salt storage for obtaining powder is crushed
Hot material.
Differential scanning thermometric analysis (DSC), heat have been carried out to the heat accumulating that embodiment 1 and comparative example 1 prepare
Zero-g aircraft (TG) and heat endurance experiment test, as a result as Figure 1-3.
Can be seen that in result shown in Fig. 1：Compared to comparative example, heat accumulating prepared by embodiment method it is molten
Point reduces nearly 3 DEG C, and the method for illustrating present invention introduction is obvious for the fusing point for reducing molten salt system heat accumulating has
Effect.
Result shown in Fig. 2 can be seen that：The upper limit of the heat accumulating prepared compared to comparative example, embodiment method
25 DEG C or so are risen using temperature, illustrates that the method for present invention introduction can be in the fusing point for reducing molten salt system heat accumulating
Meanwhile, the effect of temperature range is used with SC service ceiling temperature, extension is lifted.
Fig. 3 is heat endurance experiment test of the heat accumulating for preparing of embodiment and comparative example under the conditions of 450 DEG C
As a result, it can be seen that the heat endurance of embodiment is substantially better than comparative example, illustrate prepared by the method for present invention introduction
Heat accumulating in addition to it can extend using temperature range, moreover it is possible to be obviously improved material heat endurance, for extend storage
Hot material service life has very important effect.
Claims (3)
1. a kind of nitric acid salt system fused salt heat accumulating, it is characterised in that the nitric acid salt system fused salt heat accumulating is by nitric acid
The mass ratio of potassium and sodium nitrate composition, the sodium nitrate and potassium nitrate is 30～70：30～70, the Ca2+、Mg2+、Cl-、SO4 2-
The content of ion is respectively 5～50ppm, 10～60ppm, 50～200ppm, 100～250ppm；
The heat accumulating is prepared as follows：
1) potassium nitrate and sodium nitrate are purified, and the sodium nitrate and potassium nitrate after purification is mixed according to 30～70: 30～70 ratio
Close, obtain just batch mixing；
2) by step 1) just batch mixing carries out high-temperature heat treatment under the conditions of 400～500 DEG C for the heat accumulating that obtains；
The high-temperature heat treatment is that the vessel for filling just batch mixing are placed in and can be heated in the high temperature furnace with temperature control, with 5～20
DEG C/heating rate of min afterwards, is incubated 20～60min to 400～500 DEG C；After insulation terminates, room temperature is cooled to；Afterwards
Repeat above-mentioned heating process 2～5 times；It is finally cooled to room temperature；
The purification is at ambient temperature, sodium nitrate and potassium nitrate to be dissolved separately in deionized water so that its solution matter
Amount concentration is respectively 15%～45%, 10%～35%；Distinguish under agitation afterwards, be evaporated in evaporator boat, treat
Solution concentration is respectively reached after 50%～65%, 45%～60%, then carry out crystallisation by cooling, drip washing, drying carried respectively
Sodium nitrate and potassium nitrate after pure；
The purification step is carried out 1～3 time, until the Ca in solution2+、Mg2+、Cl-、SO4 2-Impurity ion content be respectively 5～
50ppm, 10～60ppm, 50～200ppm, 100～250ppm.
2. energy storage material according to claim 1, it is characterised in that the mass ratio of the sodium nitrate and potassium nitrate is 60：
40。
3. a kind of method for preparing nitric acid salt system fused salt heat accumulating, including：
1) potassium nitrate and sodium nitrate are purified, and by the sodium nitrate and potassium nitrate after purification according to 30～70：30～70 ratio is mixed
Close, obtain just batch mixing；
2) by step 1) just batch mixing carries out high-temperature heat treatment under the conditions of 400～500 DEG C for the heat accumulating that obtains；
The purification is at ambient temperature, sodium nitrate and potassium nitrate to be dissolved separately in deionized water so that its solution matter
Amount concentration is respectively 15%～45%, 10%～35%；Distinguish under agitation afterwards, be evaporated in evaporator boat, treat
Solution concentration is respectively reached after 50%～65%, 45%～60%, then carry out crystallisation by cooling, drip washing, drying carried respectively
Sodium nitrate and potassium nitrate after pure；
The purification step is carried out 1～3 time, until the Ca in solution2+、Mg2+、Cl-、SO4 2-Impurity ion content be respectively 5～
50ppm, 10～60ppm, 50～200ppm, 100～250ppm；
The high-temperature heat treatment is that the vessel for filling just batch mixing are placed in and can be heated in the high temperature furnace with temperature control, with 5～20
DEG C/heating rate of min afterwards, is incubated 20～60min to 400～500 DEG C；After insulation terminates, room temperature is cooled to；Afterwards
Repeat above-mentioned heating process 2～5 times；It is finally cooled to room temperature.
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| CN105419732B (en) * | 2015-12-09 | 2019-03-08 | 西安工程大学 | A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material |
| CN107312502A (en) * | 2016-04-27 | 2017-11-03 | 中国科学院青海盐湖研究所 | A kind of ternary nitric acid fused salt heat accumulating and preparation method thereof |
| CN106276984B (en) * | 2016-07-22 | 2018-04-13 | 中国科学院青海盐湖研究所 | A kind of preparation method of potassium nitrate |
| CN109114647A (en) * | 2018-08-21 | 2019-01-01 | 镇江裕太防爆电加热器有限公司 | A kind of power plant heat accumulation power generation heating system |
| CN109796940A (en) * | 2019-02-22 | 2019-05-24 | 广州特种承压设备检测研究院 | A kind of mixed chloride fused salt of high thermal conductivity and its preparation method and application |
| CN113817451A (en) * | 2020-01-21 | 2021-12-21 | 山西沃锦新材料股份有限公司 | Preparation method of nitrate system binary molten salt |
| CN111995990B (en) * | 2020-07-31 | 2021-10-15 | 华北电力大学 | Multi-element molten salt with melting point close to room temperature and preparation method thereof |
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| Title |
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| 《Effect of nanoparticles on heat capacity ofnanofluids based on molten salts as PCM for thermal energy storage》;Manila Chieruzzi etc.;《Nanoscale Research Letters》;20131029;第2页左栏倒数第1-7行 * |
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