CN113372886A - Ternary chloride molten salt with high-temperature thermal stability and preparation method thereof - Google Patents
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Abstract
The invention relates to ternary chloride molten salt with high-temperature thermal stability, which comprises 17.7-27.7 wt.% of NaCl, 6.0-25.1 wt.% of KCl and 55.1-66.1 wt.% of CaCl2. The invention also provides a preparation method of the ternary chloride molten salt, which comprises the steps of obtaining a mixture ratio based on thermodynamic calculation and experimental tests; mixing NaCl, KCl and CaCl according to a ratio2(ii) a Heating at a heating rate of 0.5-10 ℃/min, and keeping the temperature at 350 ℃ for 0.5-10h at 100 ℃ to remove the residual water in the molten salt; heating to 550-700 deg.C at a heating rate of 1-20 deg.C/min, maintaining the temperature for 0.5-24h, pouring out the molten salt in molten state, and naturally cooling to room temperature. The ternary chloride fused salt has low cost and high thermal stability, and can greatly improve the upper limit of the working temperature.
Description
Technical Field
The invention relates to molten salt, in particular to ternary chloride molten salt with high-temperature thermal stability and a preparation method thereof.
Background
The chloride molten salt has small viscosity, excellent heat transfer and storage performance and low cost, and is a very potential high-temperature heat transfer materialThe thermal heat storage medium has been widely applied to the fields of solar thermal power generation, fused salt energy storage, metallurgy and the like. Magnesium-based chloride fused salt (KCl-MgCl) in next-generation solar photo-thermal power generation system2Or NaCl-KCl-MgCl2) And NaCl-KCl-ZnCl2Has been listed as a candidate heat transfer and storage medium by the Sunshot project in the United states. However, MgCl2And ZnCl2The intrinsic hygroscopicity and higher vapor pressure of the material are saved, so that the vapor pressure of a chloride molten salt system is higher, and the thermal stability is reduced. The higher vapor pressure not only affects the safety of the photo-thermal power generation system, but also causes the system to have abnormal and complex design and sharply increases the construction cost, and directly limits the rapid development of industries such as solar thermal power generation and fused salt energy storage.
China Qinghai province has rich salt lake resources, and the NaCl resource reserves ascertained only in the Carlo salt lake are 555.4 hundred million tons, and the KCl resource reserves are 5.4 million tons. With the upgrade of industrial structure in China, the eastern chemical industry and pharmaceutical industry are gradually transferred to the western regions such as Qinghai, and the like, and a large amount of CaCl byproduct is generated in the chemical industry or pharmaceutical industry2And (4) waste liquor. CaCl2The direct discharge of the waste liquid not only causes environmental pollution, but also causes resource waste. If the valuable natural resources of the salt lake are reasonably developed and the CaCl in the chemical and pharmaceutical industries such as alkali making and the like is effectively utilized2The waste liquid can relieve the environmental pollution caused by accumulation of a large amount of molten salt and waste liquid, is beneficial to the sustainable development of local economy and society, and has important profound significance.
Mixing a plurality of different molten salt systems, and using a traditional 'frying' method is the most common method for preparing a multi-element molten salt system. The method needs a large amount of experiments, consumes a large amount of material resources and manpower, and has high cost, low efficiency and unsatisfactory effect.
In conclusion, it is necessary to design and prepare a low-cost and high-temperature heat-stable chloride molten salt system suitable for photo-thermal power generation and energy storage.
Disclosure of Invention
In order to solve the problems of large vapor pressure and the like in a chloride molten salt system in the prior art, the invention provides ternary chloride molten salt with high-temperature thermal stability and a preparation method thereof.
The ternary chloride molten salt with high temperature heat stability comprises 17.7-27.7 wt.% NaCl, 6.0-25.1 wt.% KCl and 55.1-66.1 wt.% CaCl2。
Preferably, the ternary chloride molten salt comprises 24.0-26.7 wt.% NaCl, 7.7-10.0 wt.% KCl, and 65.6-66.0 wt.% CaCl2。
Preferably, the ternary chloride molten salt is a eutectic salt.
Preferably, the eutectic point (melting point) of the ternary chloride molten salt is 496.0 ± 2.0 ℃.
Preferably, the eutectic point of the ternary chloride molten salt is 495.9-496.5 ℃.
Preferably, the melting enthalpy (latent heat) of the ternary chloride molten salt is 155.0 ± 25.0J/g.
Preferably, the melting enthalpy of the ternary chloride molten salt is 160.8J/g-171.7J/g.
Preferably, the decomposition temperature of the ternary chloride molten salt is more than or equal to 700 ℃. In a preferred embodiment, the decomposition temperature of the ternary chloride molten salt is 939.0 ℃.
The invention also provides a preparation method of the ternary chloride molten salt, which comprises the following steps: s1, 17.7-27.7 wt.% NaCl, 6.0-25.1 wt.% KCl and 55.1-66.1 wt.% CaCl based on thermodynamic calculation and experimental testing2Proportioning; s2, mixing NaCl, KCl and CaCl according to the proportion2(ii) a S3, heating at a heating rate of 0.5-10 ℃/min, and keeping the temperature at 350 ℃ for 0.5-10h at 100 ℃ to remove the residual water in the molten salt; s4, heating to 550-700 ℃ at the heating rate of 1-20 ℃/min, preserving the heat for 0.5-24h at the temperature, pouring out the molten salt in a molten state, and naturally cooling to room temperature.
Preferably, the step S1 includes: s11, selecting a lattice stability parameter; s12, evaluation and optimization of phase equilibrium and thermochemical data, calculation of the intermediate KCaCl by means of the first principles of principle3The zero point energy of the phase diagram is used as an initial value of the next phase diagram optimization; s13, selecting a thermodynamic model, optimizing the action coefficient of the corresponding phase by adopting phase diagram software, and continuouslyRepeatedly calculating until the calculated value is matched with the experimental value, and constructing self-consistent reliable binary systems NaCl-KCl and NaCl-CaCl2、KCl-CaCl2Extrapolating the thermodynamic database to obtain ternary system NaCl-KCl-CaCl2The eutectic point of the ternary chloride molten salt is predicted, and the selection range of the proportion of the ternary chloride molten salt is at or near the eutectic point component.
Preferably, the steps S2-S4 are performed in a crucible. Preferably, the crucible is an alumina crucible or a quartz crucible. Preferably, the crucible is a pretreated crucible. Preferably, the crucible is pretreated by the following method: ultrasonically cleaning the crucible by adopting acetone, deionized water and absolute alcohol, placing the crucible in an oven to remove free water, and preserving the temperature for 0.2-48h at the temperature of 100-300 ℃.
Preferably, said steps S2-S4 are carried out in a glove box covered with a highly pure inert atmosphere. Preferably, the high-temperature resistance furnace is connected with a glove box, and the oxygen content of water in the glove box is less than 5 ppm.
According to the ternary chloride molten salt with high-temperature thermal stability, NaCl, KCl and CaCl are selected2The composition is low in cost and good in system economy; the proportion of each component is selected to be 17.7-27.7 wt.% of NaCl, 6.0-25.1 wt.% of KCl and 55.1-66.1 wt.% of CaCl2And the thermal stability is high. Particularly, the ternary chloride molten salt has a low melting point (496.0 +/-2.0 ℃) and a high latent heat (155.0 +/-25.0J/g), can greatly improve the upper limit of the working temperature of the molten salt, enriches a database of the heat transfer and storage performance of the molten salt, and provides a candidate medium for a molten salt heat storage system for industrial use at high temperature (more than or equal to 700 ℃). In addition, the preparation method of the ternary chloride molten salt adopts thermodynamic calculation as effective guidance for preparing the multi-element molten salt system, overcomes the defects of low efficiency, high cost and the like of the traditional dish preparation method, and is good in economy and high in efficiency by accurately designing the multi-element molten salt system according to the eutectic point ratio predicted by the thermodynamic calculation. Moreover, the preparation process of the ternary chloride molten salt is simple and easy to operate, and lays a solid foundation for large-scale preparation of the molten salt system in industry. Meanwhile, reasonably developed salt lake resources of the Qinghai and the development of photo-thermal power generation can relieveThe method has the advantages that the environmental pollution caused by local molten salt accumulation, waste liquid discharge and the like is avoided, the sustainable development of the local economic society can be driven, and the method has important significance for realizing the aims of carbon peak reaching in 2030 years and carbon neutralization in 2060 years in China.
Drawings
FIG. 1 is a DSC curve of the ternary chloride molten salt system of example 1 according to the present invention;
FIG. 2 is a plot of the mass of the ternary chloride molten salt system of FIG. 1 as a function of temperature;
FIG. 3 is a DSC curve of the ternary chloride molten salt system of example 2 according to the present invention;
FIG. 4 is a DSC curve of the ternary chloride molten salt system of comparative example 1 according to the present invention;
FIG. 5 is a DSC curve of the ternary chloride molten salt system of comparative example 2 according to the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Sample preparation: adding NaCl, KCl and CaCl2The molten salt is stored in a glove box covered with high-purity inert atmosphere for standby.
The method is characterized in that a high-temperature resistance furnace in a glove box is debugged to be in an optimal state, a hearth and a furnace cover of the high-temperature resistance furnace are ensured to be clean and dry, a high-purity inert atmosphere pipeline passing in and out of the high-temperature resistance furnace is ensured to be smooth, a deionized water level of a water cooling machine connected with the high-temperature resistance furnace is ensured to be in a normal position, and the high-purity inert atmosphere passing into the glove box and the high-temperature resistance.
Equipment and consumables for preparing the molten salt in the glove box, such as an electronic balance (with the precision of 0.001g), tweezers, a weighing scoop, a salt container, crucible tongs, and drying and cleaning, are ensured for later use.
Ultrasonically cleaning the experimental crucible with acetone, deionized water and alcohol, placing the crucible in an oven for drying, and then storing the dried crucible in a glove box covered with inert atmosphere for later use.
First, an appropriate one is selected according to the characteristics of the systemA lattice stability parameter; corresponding phase equilibrium and thermochemical data were evaluated and optimized and the intermediate compound KCaCl was calculated by means of the first principles3The zero point energy of the phase diagram is used as an initial value of the next phase diagram optimization; selecting a proper thermodynamic model, optimizing the action coefficients of corresponding phases by adopting phase diagram software, continuously and repeatedly calculating until the calculated values are consistent with the experimental values, and constructing self-consistent reliable binary systems NaCl-KCl and NaCl-CaCl2、KCl-CaCl2Extrapolating the thermodynamic database to obtain ternary system NaCl-KCl-CaCl2The eutectic point of the system is obtained through prediction of the thermodynamic parameters.
Predicting the obtained NaCl-KCl-CaCl according to the thermodynamic calculation result2And selecting proper molten salt proportion at or near the eutectic point. Weighing NaCl, KCl and CaCl with proper mass in a glove box covered with high-purity inert atmosphere2Molten salt is placed in a crucible which is treated in advance, stirred and mixed uniformly, a corresponding crucible cover is covered, the crucible containing the molten salt is placed in a resistance furnace connected with a glove box, the temperature is raised at the heating rate of 0.5-10 ℃/min, the temperature is kept for 0.5-10h at the temperature of 300 ℃, then the temperature is heated to 700 ℃ for 550-24 h, then the molten salt is poured out in a molten state, and the molten salt is naturally cooled to the room temperature. The melting point of the prepared ternary chloride molten salt system is tested by adopting a Differential Scanning Calorimeter (DSC), the upper limit of the testing temperature is 620 ℃, and the heating rate in the testing process is 5-10 ℃/min.
Example 1
After calibrating the electronic balance (0.001g) and adjusting the level, 26.7 wt.% NaCl, 7.7 wt.% KCl, 65.6 wt.% CaCl, respectively, were weighed in a glove box2。
Placing the Al subjected to pretreatment before extraction2O3Stirring and mixing uniformly in the crucible, covering a corresponding crucible cover, putting the crucible containing the molten salt into a resistance furnace connected with a glove box, heating at the heating rate of 2.0 ℃/min, and keeping the temperature at 100-300 ℃ for 0.5-10h to remove the water possibly remaining in the molten salt.
And then heating to 700 ℃ at the heating rate of 4.0 ℃/min, preserving the heat for 5 hours at the temperature, pouring out the molten salt in a molten state, and naturally cooling to room temperature to be tested for the melting point.
The prepared ternary chloride molten salt system is tested by DSC, the upper limit of the test temperature is 620 ℃, the heating rate is 10 ℃/min, as shown in figure 1, the shape of the melting peak is regular and is a single peak, which indicates that the molten salt with the proportion forms eutectic salt, wherein the melting point is 495.9 ℃, and the melting enthalpy is 160.8J/g.
FIG. 2 shows the variation of the quality of the ternary chloride molten salt system of this example with temperature, and the thermal decomposition temperature of the molten salt of this ratio is as high as 939 ℃.
Example 2
After calibrating the electronic balance (0.001g) and adjusting the level, 24.0 wt.% NaCl, 10.0 wt.% KCl, 66.0 wt.% CaCl were weighed in a glove box2。
Placing the Al subjected to pretreatment before extraction2O3Stirring and mixing uniformly in the crucible, covering a corresponding crucible cover, putting the crucible containing the molten salt into a resistance furnace connected with a glove box, heating at the heating rate of 2.0 ℃/min, and keeping the temperature at 100-300 ℃ for 0.5-10h to remove the water possibly remaining in the molten salt.
And then heating to 700 ℃ at the heating rate of 4.0 ℃/min, preserving the heat for 5 hours at the temperature, pouring out the molten salt in a molten state, and naturally cooling to room temperature to be tested for the melting point.
The prepared ternary chloride molten salt system is tested by DSC, the upper limit of the test temperature is 620 ℃, the temperature rise rate is 10 ℃/min, as shown in figure 2, the shape of the melting peak is regular and is a single peak, which indicates that eutectic salt is formed, wherein the melting point is 496.5 ℃, and the melting enthalpy is 171.7J/g.
Comparative example 1
After calibrating the electronic balance (0.001g) and adjusting the level, 17.6 wt.% NaCl, 22.4 wt.% KCl, 60.0 wt.% CaCl were weighed in a glove box2。
Placing the Al subjected to pretreatment before extraction2O3Stirring and mixing uniformly in a crucible, covering a corresponding crucible cover, putting the crucible containing molten salt into a resistance furnace connected with a glove box, heating at a heating rate of 2.0 ℃/min,and the temperature is kept constant at 100-300 ℃ for 0.5-10h to remove the water possibly remained in the molten salt.
And then heating to 700 ℃ at the heating rate of 4.0 ℃/min, preserving the heat for 5 hours at the temperature, pouring out the molten salt in a molten state, and naturally cooling to room temperature to be tested for the melting point.
Ternary NaCl-KCl-CaCl prepared by DSC pair2The molten salt system was tested, the upper temperature limit of the test was 620 ℃, the temperature rise rate was 10 ℃/min, as shown in fig. 3, the shape of the melting peak was regular and was a single peak, indicating that eutectic salt was formed, although the melting point was 495.0 ℃, the melting enthalpy was sharply reduced to 62.6J/g.
Comparative example 2
After calibrating the electronic balance (0.001g) and adjusting the level, 19.8 wt.% NaCl, 25.2 wt.% KCl, 55.0 wt.% CaCl were weighed into a glove box2。
Placing the Al subjected to pretreatment before extraction2O3Stirring and mixing uniformly in the crucible, covering a corresponding crucible cover, putting the crucible containing the molten salt into a resistance furnace connected with a glove box, heating at the heating rate of 2.0 ℃/min, and keeping the temperature at 100-300 ℃ for 0.5-10h to remove the water possibly remaining in the molten salt.
And then heating to 700 ℃ at the heating rate of 4.0 ℃/min, preserving the heat for 5 hours at the temperature, pouring out the molten salt in a molten state, and naturally cooling to room temperature to be tested for the melting point.
Ternary NaCl-KCl-CaCl prepared by DSC pair2The molten salt system was tested at an upper temperature limit of 620 ℃ and a temperature rise rate of 10 ℃/min, as shown in fig. 4, the shape of the melting peak was regular and was a single peak, indicating that eutectic salt was formed, but the melting point increased to 530.2 ℃ and the enthalpy of fusion was also reduced to 91.5J/g.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
1. The ternary chloride molten salt with high-temperature thermal stability is characterized by comprising 17.7-27.7 wt.% of NaCl, 6.0-25.1 wt.% of KCl and 55.1-66.1 wt.% of CaCl2。
2. The ternary chloride molten salt of claim 1, comprising 24.0-26.7 wt.% NaCl, 7.7-10.0 wt.% KCl, and 65.6-66.0 wt.% CaCl2。
3. The ternary chloride molten salt according to claim 1, characterized in that it is a eutectic salt.
4. The ternary chloride molten salt according to claim 3, characterized in that it has a eutectic point of 496.0 ± 2.0 ℃.
5. The ternary chloride molten salt according to claim 4, characterized in that it has a eutectic point of 495.9 ℃ -496.5 ℃.
6. The ternary chloride molten salt according to claim 3, characterized by having a melting enthalpy of 155.0 ± 25.0J/g.
7. The ternary chloride molten salt according to claim 6, characterized by having a melting enthalpy of 160.8J/g-171.7J/g.
8. The ternary chloride molten salt according to claim 1, wherein the decomposition temperature of the ternary chloride molten salt is not less than 700 ℃.
9. The method for the preparation of ternary chloride molten salt according to any one of claims 1 to 8, characterized in that it comprises the following steps:
s1, 17.7-27.7 wt.% NaCl, 6.0-25.1 wt.% KCl and 55.1-66.1 wt.% CaCl based on thermodynamic calculation and experimental testing2Proportioning;
s2, mixing NaCl, KCl and CaCl according to the proportion2；
S3, heating at a heating rate of 0.5-10 ℃/min, and keeping the temperature at 350 ℃ for 0.5-10h at 100 ℃ to remove the residual water in the molten salt;
s4, heating to 550-700 ℃ at the heating rate of 1-20 ℃/min, preserving the heat for 0.5-24h at the temperature, pouring out the molten salt in a molten state, and naturally cooling to room temperature.
10. The method for preparing a composite material according to claim 9, wherein the step S1 includes:
s11, selecting a lattice stability parameter;
s12, evaluation and optimization of phase equilibrium and thermochemical data, calculation of the intermediate KCaCl by means of the first principles of principle3The zero point energy of the phase diagram is used as an initial value of the next phase diagram optimization; s13, selecting a thermodynamic model, optimizing the action coefficients of corresponding phases by adopting phase diagram software, continuously and repeatedly calculating until the calculated values are consistent with the experimental values, and constructing self-consistent reliable binary systems of NaCl-KCl and NaCl-CaCl2、KCl-CaCl2Extrapolating the thermodynamic database to obtain ternary system NaCl-KCl-CaCl2The eutectic point of the ternary chloride molten salt is predicted, and the selection range of the proportion of the ternary chloride molten salt is at or near the eutectic point component.
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