CN112551567B - Purification method of chloride - Google Patents
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- CN112551567B CN112551567B CN202011408338.2A CN202011408338A CN112551567B CN 112551567 B CN112551567 B CN 112551567B CN 202011408338 A CN202011408338 A CN 202011408338A CN 112551567 B CN112551567 B CN 112551567B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
- C01F7/62—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F3/00—Compounds of beryllium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/04—Halides
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/04—Halides
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a purification method of chloride. The method comprises the following steps: the mixture of inert carrier gas and chloride gas passes through chlorine-containing molten salt, the gas escaping from the surface of the chlorine-containing molten salt passes through a tower plate of a rectifying tower, and the purified chloride is collected from the top of the rectifying tower; wherein the chloride is AlCl 3 、ZrCl 4 、BeCl 2 、BiCl 3 And ZnCl 2 Any one of the above; the chlorine-containing molten salt contains NaCl, liCl, KCl and CaCl 2 CsCl, rbCl and MgCl 2 A molten salt of one or more of (a); the oxygen content in the chlorine-containing molten salt is below 400 ppm; the temperature of the chlorine-containing molten salt is 290-800 ℃ and is higher than the melting point of the chlorine-containing molten salt. The content of oxygen element in the purified chloride can be controlled below 96ppm, and the minimum content can be controlled below 1ppm, and the method can be used for preparing organic synthesis catalysts.
Description
Technical Field
The invention relates to a purification method of chloride.
Background
High purity chlorides (e.g. AlCl) 3 、ZrCl 4 、BeCl 2 、BiCl 3 And ZnCl 2 ) Is an important raw material for preparing organic reaction catalysts. However, chlorides are easy to deliquesce, have strong capability of absorbing and complexing oxygen, and are easy to form oxygen-chlorine complexes with various forms, such as ZrOCl 2 AlOCl or Zn 2 OCl 2 And the like. The oxygen element contained in the catalyst influences the physical and chemical properties of the catalyst and the catalytic performance. Therefore, in order to prepare a chloride with high catalytic performance, the oxygen content in the chloride needs to be controlled.
Therefore, there is a need in the art to develop a purification method for chlorides having a high purity and a lower oxygen content.
Disclosure of Invention
The invention aims to solve the technical problem of providing a chloride purification method in order to overcome the defect that the existing chloride preparation method is difficult to prepare high-purity chloride with the oxygen content lower than 100 ppm. The content of oxygen element in the high-purity chloride prepared by the purification method can be effectively controlled below 96ppm, and can be controlled below 1ppm at the lowest, and the method can be used for preparing organic synthesis catalysts.
The solution absorption method is a commonly used method for collecting gaseous, vapor and aerosol pollutants in air. When sampling, the air to be measured is pumped into the absorption tube filled with absorption liquid at a certain flow rate by using an air extractor. And the absorption liquid commonly used at present comprises water, aqueous solution, organic solvent and the like. The inventor of the application applies the solution absorption method to the purification of chloride, improves the purification through a great amount of experimental research, and tries to effectively remove oxygen in the chloride by adopting chlorine-containing molten salt as an absorption liquid for the first time through controlling condition parameters, so that the content of the oxygen in the chloride is controlled to be below 96ppm and at the lowest below 1ppm, and the high-purity chloride is successfully prepared.
The invention solves the technical problems through the following technical scheme.
The invention provides a purification method of chloride, which comprises the following steps: enabling a mixture of inert carrier gas and chloride gas to pass through chlorine-containing molten salt, enabling gas escaping from the surface of the chlorine-containing molten salt to pass through a tower plate of a rectifying tower, and collecting purified chloride from the top of the rectifying tower;
wherein the chloride is AlCl 3 、ZrCl 4 、BeCl 2 、BiCl 3 And ZnCl 2 Any one of (a); the chlorine-containing molten salt contains NaCl, liCl, KCl and CaCl 2 CsCl, rbCl and MgCl 2 A molten salt of one or more of (a); the content of oxygen in the chlorine-containing molten salt is below 400 ppm; the temperature of the chlorine-containing molten salt is 290-800 ℃, and the temperature of the chlorine-containing molten salt is higher than the melting point of the chlorine-containing molten salt.
In the present invention, the inert carrier gas may be an inert carrier gas conventionally used in the art, preferably one or more of argon, helium and nitrogen, more preferably argon.
In the present invention, the content of oxygen in the inert carrier gas may be 50ppm or less, preferably 10ppm or less, more preferably 1ppm or less.
In the present invention, the content of water in the inert carrier gas may be 50ppm or less, preferably 10ppm or less, more preferably 1ppm or less.
In the present invention, the vapor pressure of the chloride may be 100Pa or more at a temperature of 450 ℃ or less.
In the present invention, the preparation method of the chloride gas can be conventional in the field, and generally the chloride solid is prepared by heating and gasifying.
The conditions and method for heating gasification can be the conditions and method which are conventional in the operation in the field, and the heating gasification is preferably carried out in a closed container containing an external electric heater.
The temperature of the heating gasification may be a temperature conventionally set by those skilled in the art for volatilizing chloride into the chloride gas, and is preferably 120 ℃ or more, more preferably 120 to 500 ℃, for example, any one of 230 ℃, 250 ℃ and 340 ℃.
In the present invention, the content of the oxygen element in the chlorine-containing molten salt is preferably 385ppm or less, for example, any one of 79ppm, 80ppm, 85ppm, 163ppm, 166ppm, 183ppm, 227ppm, 254ppm, 336ppm and 355 ppm.
In the present invention, the melting point of the chlorine-containing molten salt may be 800 ℃ or lower, preferably 650 ℃ or lower, for example, any one of 294 ℃, 327 ℃, 348 ℃, 355 ℃, 385 ℃, 426 ℃, 554 ℃, 610 ℃, 632 ℃, 657 ℃, 714 ℃ and 771 ℃.
In the present invention, the chlorine-containing molten salt is generally in a molten liquid state when used.
In the present invention, the chlorine-containing molten salt is preferably a NaCl single-component molten salt, a LiCl single-component molten salt, a KCl single-component molten salt, or MgCl 2 Single-component molten salt or NaCl, liCl, KCl and CaCl 2 CsCl, rbCl and MgCl 2 Mixed molten salt of any two to seven kinds, preferably NaCl, liCl, KCl, caCl 2 CsCl, rbCl and MgCl 2 Any two or three of the above molten salts, preferably LiCl-NaCl-KCl molten salt, and KCl-MgCl 2 Molten salt, naCl-KCl-MgCl 2 Fused salt, naCl-KCl fused salt, liCl-NaCl fused salt, liCl-KCl-CaCl 2 Any one of molten salt, liCl-CsCl-RbCl molten salt and LiCl-KCl molten salt.
Wherein, in the LiCl-NaCl-KCl molten salt, the molar percentages of LiCl, naCl and KCl are (3-98%) calculated by taking the sum of the molar percentages of LiCl, naCl and KCl as 100%: (1-57%): (1% to 75%), preferably 56%:7%: and 37 percent.
Wherein, the KCl-MgCl 2 In molten salt, with KCl and MgCl 2 Is 100%, KCl and MgCl 2 The mole percentage of (C) can be (12-83%): (17% to 88%), preferably 68.5%:31.5% or 80%:20 percent.
Wherein, the NaCl-KCl-MgCl 2 In molten salt, with NaCl, KCl and MgCl 2 Is 100% in total, naCl, KCl and MgCl 2 The mole percentage of (1% -64%): (1-65%): (14% to 97%), preferably 13.5%:9%:77.5 percent.
Wherein, in the NaCl-KCl fused salt, the molar percentage of NaCl and KCl is (49% -51%) when the sum of the molar percentage of NaCl and KCl is 100%: (49% to 51%), preferably 50%:50 percent.
Wherein, in the LiCl-NaCl fused salt, the molar percentage of LiCl and NaCl can be (41-99.9%) based on the sum of the molar percentage of LiCl and NaCl being 100%: (0.1% to 59%), preferably 72%:28 percent.
Wherein, in the LiCl-KCl fused salt, the molar percentage of LiCl and KCl is (21% -99.9%) when the sum of the molar percentage of LiCl and KCl is 100%: (0.1% to 79%), preferably 60%:40 percent.
Wherein, the LiCl-KCl-CaCl 2 In molten salt, liCl, KCl and CaCl are added 2 The sum of the mole percentages of LiCl, KCl and CaCl is 100 percent 2 The mole percentage of (C) can be (0.1% -97.0%): (0.1-93.0%): (0.1% to 73.0%), preferably 45.4%:38.1%:16.5 percent.
Wherein, in the LiCl-CsCl molten salt, the molar percentage of LiCl and CsCl can be (0.1% -99.9%) based on the sum of the molar percentage of LiCl and CsCl being 100%: (0.1% to 99.9%), preferably 58%:42 percent.
Wherein, in the LiCl-CsCl-RbCl molten salt, the molar percentages of the LiCl, the CsCl and the RbCl can be (0.1-99.8%) based on the sum of the molar percentages of the LiCl, the CsCl and the RbCl being 100%: (0.1-99.8%): (0.1% to 83.0%), preferably 56.5%:11.5%:32 percent.
In the invention, the temperature of the chlorine-containing molten salt is preferably 400-750 ℃. When the temperature of the chlorine-containing molten salt is higher than the range defined by the application, the manufacturing cost of the reactor and the external electric heater is increased due to the overhigh temperature, and the separation of the chloride and the chlorine-containing molten salt in a gas phase is not facilitated.
When the chlorine-containing molten salt is LiCl-NaCl-KCl molten salt, the molar percentage of LiCl, naCl and KCl is 56% based on the sum of the molar percentages of LiCl, naCl and KCl being 100%: 7%: at 37%, the temperature of the chlorine-containing molten salt is 352 ℃.
When the chlorine-containing molten salt is the KCl-MgCl 2 Molten salt of KCl and MgCl 2 In a molar percentage of 100%, KCl and MgCl 2 68.5%:31.5%, the temperature of the chlorine-containing molten salt is any one of 450 ℃, 600 ℃, 750 ℃ and 800 ℃.
When the chlorine-containing molten salt is the KCl-MgCl 2 Molten salt of KCl and MgCl 2 Is 100%, KCl and MgCl 2 80% by mole: when the concentration is 20%, the temperature of the chlorine-containing molten salt is 680 ℃.
When the chlorine-containing molten salt is the NaCl-KCl-MgCl 2 Molten salt of NaCl, KCl and MgCl 2 With the sum of the mole percentages of NaCl, KCl and MgCl being 100% 2 13.5%:9%:77.5 percent, the temperature of the chlorine-containing molten salt is 450 ℃.
When the chlorine-containing molten salt is the NaCl-KCl molten salt, the molar percentage of NaCl and KCl is 50% when the sum of the molar percentage of NaCl and KCl is 100%: when the concentration is 50%, the temperature of the chlorine-containing molten salt is 670 ℃.
When the chlorine-containing molten salt is the LiCl-NaCl molten salt, the molar percentage of LiCl and NaCl is 72% based on the sum of the molar percentages of LiCl and NaCl being 100%: when the concentration is 28 percent, the temperature of the chlorine-containing molten salt is 580 ℃.
When the chlorine-containing molten salt is LiCl-KCl molten salt, the molar percentage of LiCl and KCl is 60% by taking the sum of the molar percentages of LiCl and KCl as 100%: at 40%, the temperature of the chlorine-containing molten salt is 380 ℃.
When the chlorine-containing molten salt is the LiCl molten salt, the temperature of the chlorine-containing molten salt is 650 ℃.
When the chlorine-containing molten salt is the KCl molten salt, the temperature of the chlorine-containing molten salt is 800 ℃.
When the chlorine-containing molten salt is the NaCl molten salt, the temperature of the chlorine-containing molten salt is 800 ℃.
When the chlorine-containing molten salt is the MgCl 2 When the salt is fused, the temperature of the chlorine-containing fused salt is 750 ℃.
When the chlorine-containing molten salt is LiCl-KCl-CaCl 2 Molten salt of LiCl, KCl and CaCl 2 The sum of the mole percentages of LiCl, KCl and C being 100%aCl 2 45.4% by mole: 38.1%: at 16.5%, the temperature of the chlorine-containing molten salt is 370 ℃.
When the chlorine-containing molten salt is the LiCl-CsCl molten salt, the molar percentage of the LiCl and the CsCl is 58% based on the sum of the molar percentages of the LiCl and the CsCl being 100%: at 42%, the temperature of the chlorine-containing molten salt is 327 ℃.
When the chlorine-containing molten salt is the LiCl-CsCl-RbCl molten salt, the molar percentage of the LiCl, the CsCl and the RbCl is 56.5 percent based on the sum of the molar percentages of the LiCl, the CsCl and the RbCl as 100 percent: 11.5%: at 32%, the temperature of the chlorine-containing molten salt is 294 ℃.
In the present invention, the rectifying column may be a plate-type rectifying column, preferably a baffle-type rectifying column, which is conventionally used in the art.
In the present invention, the number of the plates in the rectification column may be conventional in the art, and is preferably 15 to 40, more preferably 25 to 40, for example 30 or 35.
In the present invention, the temperature of the tray in the rectifying column may be any one of 290 to 800 ℃, preferably 380 to 670 ℃, for example 294 ℃, 327 ℃, 370 ℃, 450 ℃ and 580 ℃.
In the invention, the rectifying tower can be operated under the normal pressure of the whole tower.
In the present invention, the collecting operation further comprises condensation to produce a solid purified chloride.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the method adopts a solution absorption method, takes the chlorine-containing molten salt as an absorption liquid to effectively reduce the content of oxygen in the chloride, and the content of the oxygen in the purified chloride can be reduced to be below 96ppm and at most below 1ppm, thereby effectively solving the problem that the chloride with higher purity can not be prepared in the prior art.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. Experimental procedures without specifying specific conditions in the following examples were selected in accordance with conventional procedures and conditions, or in accordance with commercial instructions.
The preparation method of the chlorine-containing molten salt in the following examples and comparative examples of the present invention is the preparation method of the mixed molten salt in the chinese patent with application number 201610892250.X, and the difference is only that the kinds and molar ratio of the chlorine-containing compounds in the chlorine-containing molten salt according to each example and comparative example are adjusted accordingly.
Examples 1 to 22 and comparative examples 1 to 2 the chlorides were purified as follows, with the specific parameters reported in table 1.
Adding 1kg of chloride into a closed evaporator, heating the evaporator by using an external electric heater, and heating and gasifying to prepare chloride gas; and (3) passing the mixture of argon and chloride gas through 1L of chlorine-containing molten salt, wherein the flow rate of the argon is 100mL/min, passing the gas escaping from the surface of the chlorine-containing molten salt through a rectifying device, collecting the purified chloride at the top of a rectifying tower, and condensing in a collector to prepare the solid purified chloride. The whole system used in the experimental process comprises an evaporator, a rectifying tower and a collector which are all sealed systems; the air tightness of the whole system is 10 by adopting helium vacuum air leakage test -4 Pa·m 3 /s。
Effects of the embodiment
The purified chlorides obtained in the above examples and comparative examples were tested for their content and purity of oxygen, and the results are shown in Table 1. In Table 1, taking example 1 as an example, the LiCl-NaCl-KCl molten salt has the molar percentage of each component of 56%:7%:37%, i.e. 56% in molar percentage of LiCl, naCl and KCl: 7%:37 percent.
The method of example 1 in the Chinese patent with the application number of 201410184920.3 is adopted to test the content of oxygen element in chloride, and the test instrument is an oxygen analyzer with the model number of RO600 produced by LECO company. Testing the purity of the purified chloride by adopting an ICP-OES method; the method for testing the melting point is Differential Scanning Calorimetry (DSC), and the instrument model is a high-temperature differential scanning calorimeter of relaxation-resistant DSC449F3 type.
TABLE 1
In table 1, "-" represents that the operation was not performed or the effect data was not tested.
In comparative example 1, the temperature of the chlorine-containing molten salt was 450 ℃ at which KCl-MgCl was maintained 2 The molten salt was not melted and purification treatment was not performed.
As can be seen from the above table, the content of oxygen in the chloride after purification in the examples of the present invention is significantly lower than that in the chloride after purification in the comparative examples.
Claims (11)
1. A method for purifying chloride is characterized by comprising the following steps: enabling a mixture of inert carrier gas and chloride gas to pass through chlorine-containing molten salt, enabling gas escaping from the surface of the chlorine-containing molten salt to pass through a tower plate of a rectifying tower, and collecting purified chloride from the top of the rectifying tower;
wherein the chloride is AlCl 3 、ZrCl 4 、BeCl 2 、BiCl 3 And ZnCl 2 Any one of (a) to (b); the chlorine-containing molten salt contains NaCl, liCl, KCl and CaCl 2 CsCl, rbCl and MgCl 2 A molten salt of one or more of (a); the content of oxygen in the chlorine-containing molten salt is below 400 ppm; the temperature of the chlorine-containing molten salt is 290-800 ℃, and the temperature of the chlorine-containing molten salt is higher than the melting point of the chlorine-containing molten salt;
the content of oxygen in the inert carrier gas is below 50 ppm; the content of water in the inert carrier gas is below 50 ppm; the preparation method of the chloride gas is that the chloride solid is prepared by heating and gasifying;
the rectifying tower is a clapboard rectifying tower; the number of the tower plates is 25 to 40; the temperature of the tower plate is 380 to 670 ℃.
2. The method for purifying a chloride according to claim 1, wherein the inert carrier gas is one or more of argon, helium and nitrogen; the vapor pressure of the chloride is 100Pa or more at a temperature of 450 ℃ or less.
3. The method of claim 2, wherein the inert carrier gas is argon; the content of oxygen in the inert carrier gas is less than 10 ppm; the content of water in the inert carrier gas is less than 10 ppm; the heating gasification is carried out in a closed container containing an external electric heater; the temperature of heating and gasification is above 120 ℃.
4. A method for purifying a chloride as claimed in claim 3, wherein the inert carrier gas has an oxygen content of 1ppm or less; the content of water in the inert carrier gas is less than 1 ppm; the temperature of heating and gasifying is 120 to 500 ℃.
5. The method for purifying a chloride according to claim 1, wherein the content of the oxygen element in the chlorine-containing molten salt is 385ppm or less;
the melting point of the chlorine-containing molten salt is below 800 ℃;
the chlorine-containing molten salt is in a molten liquid state when in use;
the temperature of the chlorine-containing molten salt is 400 to 750 ℃;
the chlorine-containing molten salt contains NaCl, liCl, KCl and CaCl 2 CsCl, rbCl and MgCl 2 Mixed molten salt of any two to three of them.
6. The method for purifying a chloride according to claim 5, wherein the chlorine-containing molten salt has a melting point of 650 ℃ or lower; the chlorine-containing molten salt is LiCl-NaCl-KCl molten salt or KCl-MgCl 2 Molten salt, naCl-KCl-MgCl 2 Molten salt, naCl-KCl molten salt, liCl-NaCl molten salt, liCl-KCl-CaCl 2 Any one of molten salt, liCl-CsCl-RbCl molten salt and LiCl-KCl molten salt.
7. The purification method of chloride according to claim 6, characterized in that in the LiCl-NaCl-KCl fused salt, the molar percentages of LiCl, naCl and KCl are (3% -98%) based on the sum of the molar percentages of LiCl, naCl and KCl being 100%: (1% -57%): (1% -75%);
the KCl-MgCl 2 In molten salt, with KCl and MgCl 2 Is 100%, KCl and MgCl 2 The molar percentage of (12% -83%): (17% -88%);
the NaCl-KCl-MgCl 2 In molten salt, with NaCl, KCl and MgCl 2 With the sum of the mole percentages of NaCl, KCl and MgCl being 100% 2 The mole percentage of (1% -64%): (1% -65%): (14% -97%);
in the NaCl-KCl fused salt, the molar percentage of NaCl to KCl is (49% -51%) when the sum of the molar percentages of NaCl and KCl is 100%: (49% -51%);
in the LiCl-NaCl molten salt, the molar percentage of LiCl and NaCl is (41% -99.9%) when the sum of the molar percentages of LiCl and NaCl is 100%: (0.1% -59%);
in the LiCl-KCl fused salt, the molar percentage of LiCl and KCl is (21% -99.9%) when the sum of the molar percentages of LiCl and KCl is 100%: (0.1% -79%);
the LiCl-KCl-CaCl 2 In molten salt, using LiCl, KCl and CaCl 2 The sum of the mole percentages of LiCl, KCl and CaCl is 100 percent 2 The mole percentage of (0.1% -97.0%): (0.1% -93.0%): (0.1% -73.0%);
in the LiCl-CsCl molten salt, the molar percentage of LiCl and CsCl is (0.1% -99.9%) based on the sum of the molar percentages of LiCl and CsCl being 100%: (0.1% -99.9%);
in the LiCl-CsCl-RbCl molten salt, the mol percentages of LiCl, csCl and RbCl are (0.1% -99.8%) based on the sum of the mol percentages of LiCl, csCl and RbCl being 100%: (0.1% -99.8%): (0.1% -83.0%).
8. The method for purifying chloride according to claim 7, wherein in the LiCl-NaCl-KCl fused salt, the molar percentages of LiCl, naCl and KCl are 56% in terms of the sum of the molar percentages of LiCl, naCl and KCl being 100%: 7%:37 percent;
the KCl-MgCl 2 In molten salt, with KCl and MgCl 2 Is 100%, KCl and MgCl 2 68.5%:31.5% or 80%:20 percent;
the NaCl-KCl-MgCl 2 In molten salt, with NaCl, KCl and MgCl 2 With the sum of the mole percentages of NaCl, KCl and MgCl being 100% 2 13.5%:9%:77.5 percent;
in the NaCl-KCl fused salt, the molar percentage of NaCl and KCl is 50% when the sum of the molar percentage of NaCl and KCl is 100%: 50 percent;
in the LiCl-NaCl molten salt, the molar percentage of LiCl and NaCl is 72% based on the sum of the molar percentages of LiCl and NaCl being 100%: 28%;
in the LiCl-KCl molten salt, the molar percentage of LiCl and KCl is 60% in terms of the sum of the molar percentages of LiCl and KCl being 100%: 40 percent;
the LiCl-KCl-CaCl 2 In molten salt, liCl, KCl and CaCl are added 2 The sum of the mole percentages of LiCl, KCl and CaCl is 100 percent 2 45.4% by mole: 38.1%:16.5 percent;
in the LiCl-CsCl molten salt, the molar percentage of LiCl and CsCl is 58% based on the sum of the molar percentages of LiCl and CsCl being 100%: 42%;
in the LiCl-CsCl-RbCl molten salt, the molar percentage of LiCl, csCl and RbCl is 56.5 percent based on the sum of the molar percentages of LiCl, csCl and RbCl as 100 percent: 11.5%:32 percent.
9. The method for purifying chloride according to claim 1, wherein when the chlorine-containing molten salt is LiCl-NaCl-KCl molten salt, the molar percentage of LiCl, naCl and KCl is 56% based on the sum of the molar percentages of LiCl, naCl and KCl being 100%: 7%: when the concentration is 37%, the temperature of the chlorine-containing molten salt is 352 ℃;
when the chlorine-containing molten salt is KCl-MgCl 2 Molten salt of KCl and MgCl 2 (iii) the sum of the mole percentages is 100%, KCl and MgCl 2 68.5%:31.5%, the temperature of the chlorine-containing molten salt is any one of 450 ℃, 600 ℃, 750 ℃ and 800 ℃;
when the chlorine-containing molten salt is KCl-MgCl 2 Molten salt of KCl and MgCl 2 (iii) the sum of the mole percentages is 100%, KCl and MgCl 2 The molar percentage of (A) is 80%: when the concentration is 20%, the temperature of the chlorine-containing molten salt is 680 ℃;
when the chlorine-containing molten salt is NaCl-KCl-MgCl 2 Molten salt of NaCl, KCl and MgCl 2 With the sum of the mole percentages of NaCl, KCl and MgCl being 100% 2 13.5%:9%: at 77.5%, the temperature of the chlorine-containing molten salt is 450 ℃;
when the chlorine-containing molten salt is NaCl-KCl molten salt, the mol percentage of NaCl and KCl is 50% when the sum of the mol percentage of NaCl and KCl is 100%: when the concentration is 50%, the temperature of the chlorine-containing molten salt is 670 ℃;
when the chlorine-containing molten salt is LiCl-NaCl molten salt, the molar percentage of LiCl and NaCl is 72% based on the sum of the molar percentages of LiCl and NaCl being 100%: when the concentration is 28%, the temperature of the chlorine-containing molten salt is 580 ℃;
when the chlorine-containing molten salt is LiCl-KCl molten salt, the molar percentage of LiCl and KCl is 60% when the sum of the molar percentages of LiCl and KCl is 100%: when the concentration is 40%, the temperature of the chlorine-containing molten salt is 380 ℃;
when the chlorine-containing molten salt is LiCl molten salt, the temperature of the chlorine-containing molten salt is 650 ℃;
when the chlorine-containing molten salt is KCl molten salt, the temperature of the chlorine-containing molten salt is 800 ℃;
when the chlorine-containing molten salt is NaCl molten salt, the temperature of the chlorine-containing molten salt is 800 ℃;
when the chlorine-containing molten salt is MgCl 2 When the salt is fused, the temperature of the chlorine-containing fused salt is 750 ℃;
when the chlorine-containing molten salt is LiCl-KCl-CaCl 2 Molten salt of LiCl, KCl and CaCl 2 The sum of the mole percentages of LiCl, KCl and CaCl is 100 percent 2 45.4%:38.1%: when the concentration is 16.5%, the temperature of the chlorine-containing molten salt is 370 ℃;
when the chlorine-containing molten salt is LiCl-CsCl molten salt, the molar percentage of LiCl and CsCl is 58% based on the sum of the molar percentages of LiCl and CsCl being 100%: when the concentration is 42%, the temperature of the chlorine-containing molten salt is 327 ℃;
when the chlorine-containing molten salt is LiCl-CsCl-RbCl molten salt, the molar percentage of the LiCl, the CsCl and the RbCl is 56.5 percent based on the sum of the molar percentages of the LiCl, the CsCl and the RbCl as 100 percent: 11.5%: at 32%, the temperature of the chlorine-containing molten salt is 294 ℃.
10. The method for purifying chlorides according to claim 1, wherein said rectification column is operated at atmospheric pressure.
11. The method for purifying a chloride as claimed in any one of claims 1 to 10, further comprising the step of condensing after the collecting operation to obtain a solid purified chloride.
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| EP4055623A4 (en) | 2019-11-08 | 2023-12-13 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
| CN113372886A (en) * | 2021-07-01 | 2021-09-10 | 中国科学院上海应用物理研究所 | Ternary chloride molten salt with high-temperature thermal stability and preparation method thereof |
| CN113772724A (en) * | 2021-10-20 | 2021-12-10 | 辽宁华锆新材料有限公司 | Method and equipment for preparing refined zirconium tetrachloride by molten salt purification method |
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