CN112357885A - Purification method of single component in chloride molten salt - Google Patents
Purification method of single component in chloride molten salt Download PDFInfo
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- CN112357885A CN112357885A CN202011402962.1A CN202011402962A CN112357885A CN 112357885 A CN112357885 A CN 112357885A CN 202011402962 A CN202011402962 A CN 202011402962A CN 112357885 A CN112357885 A CN 112357885A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B9/00—General methods of preparing halides
- C01B9/02—Chlorides
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a purification method of a single component in chloride molten salt, which comprises the following steps: rectifying the fused salt through a plate rectifying tower; the temperature of the tower bottom of the plate-type rectifying tower is higher than the melting point of the chloride fused salt; the temperature of the plate rectifying tower is higher than the melting point of the reflux in the plate rectifying tower; the chloride molten salt is AlCl-containing3、ZrCl4、BeCl2、BiCl3And ZnCl2A chloride molten salt system of one of (1); a single component of AlCl3、ZrCl4、BeCl2、BiCl3Or ZnCl2. The water content of the single component purified by the purification method of the invention is below 1 ppm.
Description
Technical Field
The invention relates to a method for purifying a single component in chloride molten salt.
Background
Chlorides (e.g. AlCl)3、ZrCl4、BeCl2、BiCl3And ZnCl2) Is an important raw material for preparing the organic reaction catalyst, and the purity of the raw material influences the physical and chemical properties and the catalytic performance of the catalyst. The purification of chloride usually employs a recrystallization process in aqueous solution, so the product is more or less moist.
At present, in order to prepare a chloride with high catalytic performance, the water content in the chloride needs to be controlled.
In addition, in the preparation process of the molten salt, moisture in the chloride salt is easily converted into oxides when heated at high temperature, and the oxides have low volatility, are solidified in the molten salt and are not easy to remove.
Therefore, there is a need for a process that can purify chloride salts that overcomes the problems of the prior art for preparing chloride water.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect that water in chloride salt is not easy to remove in the prior art, and the chloride to be treated and other low-cost chlorides are prepared into multi-component molten salt or directly prepared into single-component molten salt, and then the single-component chloride with lower oxygen content is obtained by separating from the multi-component molten salt or the single-component molten salt, namely, the invention provides a method for purifying the single component in the chloride molten salt; the water content of the purified single component is below 1 ppm.
The invention solves the technical problems through the following technical scheme:
the invention provides a purification method of a single component in chloride molten salt, which comprises the following steps:
rectifying the molten salt by a plate rectifying tower;
the temperature of a tower kettle of the plate-type rectifying tower is higher than the melting point of the chloride fused salt;
the temperature of the plate column of the plate rectifying column is higher than the melting point of reflux in the plate rectifying column;
the chloride molten salt contains AlCl3、ZrCl4、BeCl2、BiCl3And ZnCl2A chloride molten salt system of one of (1);
the single component is AlCl3、ZrCl4、BeCl2、BiCl3Or ZnCl2。
Generally, the purified chloride molten salt is commonly used for organic synthesis catalysts or molten salts having a low water content.
In the invention, the mole percentage content of the single component in the chloride molten salt is preferably 1-100%.
In the present invention, it is preferable that the melting point of the chloride molten salt is changed by mixing the components in different proportions. Preferably, the melting point of the chloride molten salt is below 750 ℃, more preferably below 550 ℃. The melting point can be measured by methods conventional in the art, such as Differential Scanning Calorimetry (DSC) using a high temperature differential scanning calorimeter model DSC449F3, which is resistant to relaxation.
In the invention, preferably, the chloride molten salt contains AlCl3、ZrCl4、BeCl2、BiCl3And ZnCl2Contains one of KCl and MgCl2、CsCl、NaCl、LiCl、CaCl2A chloride molten salt system of one or more of (a).
Wherein, more preferably, the chloride molten salt is KCl-MgCl2-ZrCl4、CsCl-BeCl2、CsCl-ZrCl4、NaCl-ZrCl4、KCl-ZrCl4、LiCl-AlCl3、KCl-BiCl3、LiCl-ZnCl2、LiCl-KCl-CaCl2、ZrCl4、BeCl2、AlCl3、BiCl3Or ZnCl2。
Wherein, preferably, the KCl-MgCl is adopted2-ZrCl4In molten salt, KCl: MgCl2：ZrCl4The mole percentage of (1-92): (1-99): (1-99), for example (1-75): (1-72): (1-81), as another example 35: 6: 59 or 45: 52: 3.
wherein, preferably, the CsCl-BeCl2In molten salt, CsCl: BeCl2The mole percentage of (1-99): (1-99), for example (1-54): (46-99) or 84: 16, and for another example 16: 84.
wherein, preferably, when the melting point temperature of the chloride fused salt is below 750 ℃, the CsCl-ZrCl is adopted4In molten salt, CsCl: ZrCl4The mole percentage of (1-61): (39-99) or (74-99): (1-26), for example 18: 82 or 78: 22. More preferably, the CsCl-ZrCl is used when the melting point temperature of the chloride molten salt is 550 ℃ or lower4In molten salt, CsCl: ZrCl4Preferably (1-47): (53-99).
Wherein, preferably, when the melting point temperature of the chloride fused salt is below 750 ℃, the NaCl-ZrCl is adopted4In molten salt, NaCl: ZrCl4The mole percentage of (1-87): (13-99), for example 1:99 or 57: 43. More preferably, the NaCl-ZrCl is used when the melting point temperature of the chloride molten salt is 550 ℃ or lower4In molten salt, NaCl: ZrCl4The mole percentage of (1-60): (40-99) or (71-73): (27-29).
Wherein, preferably, when the melting point temperature of the chloride fused salt is below 750 ℃, the KCl-ZrCl is adopted4In molten salt, KCl: ZrCl4The mole percentage of (1-62): (38-99) or (69-94): (6-31), for example 1:99 or 43: 57. More preferably, the KCl-ZrCl is used when the melting point temperature of the chloride molten salt is 550 ℃ or lower4In molten salt, KCl: ZrCl4The mole percentage of (1-51): (49-99).
Wherein, preferably, when the melting point temperature of the chloride fused salt is below 550 ℃, the LiCl-AlCl is adopted3In molten salt, LiCl: AlCl3The mole percentage of (1-69): (31-99), for example 13: 87.
Wherein, preferably, when the melting point temperature of the chloride fused salt is below 750 ℃, the KCl-BiCl is adopted3In molten salt, KCl: BiCl3The mole percentage of (1-93): (7-99), for example 17: 83. More preferably, when the melting point temperature of the chloride molten salt is 550 ℃ or less, KCl: BiCl3The mole percentage of (1-79): (21-99), for example (1-70): (30-99).
Wherein, preferably, when the melting point temperature of the chloride molten salt is 550 ℃ or lower, the LiCl-ZnCl is used as the main component2In molten salt, LiCl: ZnCl2The mole percentage of (1-85): (15-99), for example 1: 99.
In the invention, preferably, the temperature of the tower bottom of the plate-type rectifying tower is 30-50 ℃ higher than the melting point of the chloride molten salt.
In the present invention, the temperature of the plate-type rectifying tower is preferably 5 to 50 ℃ higher than the melting point of the reflux of the plate-type rectifying tower, more preferably 30 to 50 ℃.
Wherein, preferably, the temperature of the tower kettle of the plate-type rectifying tower is 190-800 ℃. Preferably, when the single component is ZrCl4And the temperature of a tower kettle of the plate rectifying tower is 437-750 ℃.
Preferably, when the single component is AlCl3、BeCl2、BiCl3Or ZnCl2And the temperature of a tower kettle of the plate rectifying tower is 190-415 ℃.
When the chloride molten salt is prepared from the following raw materials in percentage by mole 35: 6: KCl-MgCl of 592-ZrCl4When the reflux of the plate-type rectifying tower is KCl-MgCl2Preferably, the temperature of a tower kettle of the plate type rectifying tower is 450-750 ℃, and the temperature of a tower plate of the plate type rectifying tower is 700-750 ℃; more preferably, the temperature of the tower kettle of the plate rectifying tower is 700-750 ℃, and the temperature of the tower plate of the plate rectifying tower is 700-750 ℃. Wherein, the plate type rectifying towerReflux KCl-MgCl2The melting point of (b) was 690 ℃.
When the chloride molten salt is 45 mol percent: 52: KCl-MgCl of 32-ZrCl4When the reflux of the plate-type rectifying tower is KCl-MgCl2Preferably, the temperature of a tower kettle of the plate type rectifying tower is 475-550 ℃, and the temperature of a tower plate of the plate type rectifying tower is 500-550 ℃. Wherein, the reflux of the plate-type rectifying tower is KCl-MgCl2The melting point of (B) is 480 ℃.
When the chloride molten salt is 16 mol percent: CsCl-BeCl of 842In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 320-380 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 650-700 ℃.
When the chloride molten salt is 84: CsCl-BeCl of 162When the reflux of the plate rectifying tower is CsCl, preferably, the temperature of a tower kettle of the plate rectifying tower is 650-700 ℃, and the temperature of a tower plate of the plate rectifying tower is 650-700 ℃. Wherein the melting point of the reflux material CsCl of the plate-type rectifying tower is 645 ℃.
When the chloride molten salt is 18 mol percent: CsCl-ZrCl 824In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 400-450 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 650-700 ℃.
When the chloride molten salt is 78 mol percent: CsCl-ZrCl 224When the reflux of the plate rectifying tower is CsCl, preferably, the temperature of a tower kettle of the plate rectifying tower is 700-750 ℃, and the temperature of a tower plate of the plate rectifying tower is 650-700 ℃. Wherein the melting point of the reflux material CsCl of the plate-type rectifying tower is 645 ℃.
When the chloride molten salt is in a molar percentage of 1:99 NaCl-ZrCl4In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 450-500 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 800-850 ℃.
When the chloride molten salt is 57:43 NaCl-ZrCl4In the process, the temperature of a tower kettle of the plate-type rectifying tower is preferably 800-850 ℃, andthe tower plate temperature of the plate-type rectifying tower is 800-850 ℃.
When the chloride molten salt is in a molar percentage of 1:99 KCl-ZrCl4In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 450-500 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 450-500 ℃.
When the chloride molten salt is prepared from the following raw materials in percentage by mole of 43: KCl-ZrCl of 574In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 800-850 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 800-850 ℃.
When the chloride molten salt is in a molar percentage of 1:99 LiCl-ZnCl2In the process, the temperature of the tower kettle of the plate rectifying tower is preferably 350-370 ℃, and the temperature of the tower plate of the plate rectifying tower is preferably 350-370 ℃.
When the chloride molten salt is in a molar percentage of 13:87 LiCl-AlCl3In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 200-220 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 200-220 ℃.
When the chloride molten salt is 17 mol percent: 83 KCl-BiCl3In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 200-220 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 200-220 ℃.
In the invention, generally, the chloride molten salt is added into a tower kettle of a plate-type rectifying tower to be rectified; after the rectification, collecting distillate from the tower top of the plate-type rectifying tower; and refluxing the reflux to the tower kettle of the plate-type rectifying tower, wherein the temperature of a tower plate of the plate-type rectifying tower is preferably 350-700 ℃.
In the present invention, the plate-type rectifying column may be a plate-type rectifying column conventional in the art, and is preferably a baffle rectifying column. The arrangement mode of the partition in the partition rectifying tower can be the arrangement mode conventional in the field.
In the present invention, the number of trays in the plate rectifying column may be a number conventional in the art, and is preferably 15 to 40 trays, for example, 25 or 40 trays.
In the present invention, preferably, the molten salt is stored in a molten salt storage device before being added to the plate rectifying tower.
Preferably, the molten salt storage device is further provided with a gas pipeline, and the gas pipeline is used for introducing inert gas into the molten salt storage device.
In the present invention, preferably, the collection of the product is achieved by a collection device. The collection means may be a storage vessel as is conventional in the art.
In the invention, generally, the plate-type rectifying tower and the molten salt storage device are provided with heat preservation measures, and the heat preservation measures can be conventional heat preservation methods in the field, such as heat preservation by adopting heat preservation materials.
In the invention, the lining material of the plate-type rectifying tower and the molten salt storage device is preferably a high-temperature resistant material with the temperature of above 800 ℃, such as nickel-based alloy or nickel metal.
In the invention, the plate-type rectifying tower is operated at normal pressure in the whole tower.
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:
(1) according to the purification method of the single component in the chloride molten salt, the water content of the purified single component is below 1 ppm.
(2) According to the purification method of the single component in the chloride molten salt, provided by the invention, when the chloride molten salt is the single component, the recovery rate of the purification component reaches 99%, the purity reaches 99%, and meanwhile, the water content in the purification component is below 1 ppm.
(3) According to the method for purifying the single component in the chloride fused salt, when the chloride fused salt is a plurality of components, by controlling the types and the proportion of the fused salt and controlling the tower kettle temperature and the tower plate temperature of the plate-type rectifying tower, in a preferred embodiment, the recovery rate of the purified component is 99%, the purity of the purified component is 99%, and meanwhile, the water content in the purified component is below 1 ppm.
Drawings
FIG. 1 is a schematic structural diagram of a purification apparatus for chloride molten salt in the example.
The system comprises a plate-type rectifying tower 1, a collecting device 2, a molten salt storage device 3 and a gas pipeline 4.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The preparation method of the chloride fused salt in the following embodiments of the invention is the preparation method of the mixed fused salt in the Chinese patent with the application number of 201610892250.X, and the difference is only that the component types and the molar ratio in the chloride fused salt according to the embodiments are correspondingly adjusted.
The purity of the distillate in the following examples was tested by the ICP-OES method; recovery of distillate, amount of distillate/amount of corresponding component in chloride molten salt × 100%; the water content of the distillate was measured according to GBT606-2003, Chemicals, general methods for moisture determination, Karl Fischer method.
Example 1
As shown in fig. 1, a collecting device 2 (a common storage tank in this embodiment) is connected to a plate rectifying column 1; the tower kettle of the plate-type rectifying tower is connected with a fused salt storage device 3; the molten salt storage device is also provided with a gas pipeline 4 for introducing inert gas and applying flowing power to the molten salt so as to enable the molten salt to flow into the tower kettle of the plate-type rectifying tower.
Purification was carried out according to the conditions of example 1 in table 1, i.e., the kind of chloride molten salt, mole percentage, column bottom temperature, column plate temperature and number of column plate layers: mixing the components in percentage by mole 35: 6: KCl-MgCl of 592-ZrCl4The mixed molten salt 5L is arranged in a molten salt storage device 3, and the molten salt storage device 3 and the plate rectifying tower 1 are heated to keep the molten salt in a molten state, wherein the tower kettle temperature of the plate rectifying tower 1 is 500 ℃; the molten salt stop valve is opened,introducing inert gas into a gas space above the molten salt in the molten salt storage device 3, and enabling the molten salt to enter a tower kettle of the plate-type rectifying tower 1, wherein the number of tower plates of the plate-type rectifying tower 1 is 15; and raising the temperature of the tower plate to 700 ℃, rectifying, and collecting gaseous purified zirconium tetrachloride from the tower top. The purity, recovery rate and water content of the collected zirconium tetrachloride are shown in table 1.
Examples 2 to 21
Purification was carried out according to the conditions of the respective examples in Table 1, i.e., the kind of the chloride molten salt, the mole percentage, the column bottom temperature, the tray temperature and the number of tray layers, and other operations and equipments were the same as those of example 1. The purity, recovery rate and water content of the distillate obtained are shown in Table 1.
Comparative example 1
When the temperature of the column bottom of example 19 was changed to 150 ℃ and other raw materials and conditions were kept the same as those of example 19, the chloride molten salt could not be melted, and purification could not be performed.
TABLE 1
Claims (10)
1. A method for purifying a single component in a chloride molten salt is characterized by comprising the following steps:
rectifying the molten salt by a plate rectifying tower;
the temperature of a tower kettle of the plate-type rectifying tower is higher than the melting point of the chloride fused salt;
the temperature of the plate column of the plate rectifying column is higher than the melting point of reflux in the plate rectifying column;
the chloride molten salt contains AlCl3、ZrCl4、BeCl2、BiCl3And ZnCl2A chloride molten salt system of one of (1);
the single component is AlCl3、ZrCl4、BeCl2、BiCl3Or ZnCl2。
2. The purification method of single components in chloride molten salt according to claim 1, wherein the single components are contained in the chloride molten salt in a molar percentage of 1-100%;
and/or the melting point of the chloride fused salt is lower than 750 ℃, preferably lower than 550 ℃;
and/or the chloride molten salt contains AlCl3、ZrCl4、BeCl2、BiCl3And ZnCl2Contains one of KCl and MgCl2、CsCl、NaCl、LiCl、CaCl2A chloride molten salt system of one or more of (a).
3. The purification method of single component in chloride molten salt according to claim 2, characterized in that the chloride molten salt is KCl-MgCl2-ZrCl4、CsCl-BeCl2、CsCl-ZrCl4、NaCl-ZrCl4、KCl-ZrCl4、LiCl-AlCl3、KCl-BiCl3、LiCl-ZnCl2、ZrCl4、BeCl2、AlCl3、BiCl3Or ZnCl2；
Preferably, the KCl-MgCl is adopted2-ZrCl4In molten salt, KCl: MgCl2：ZrCl4The mole percentage of (1-92): (1-99): (1-99), for example (1-75): (1-72): (1-81), as another example 35: 6: 59 or 45: 52: 3;
preferably, the CsCl-BeCl2In molten salt, CsCl: BeCl2The mole percentage of (1-99): (1-99), for example (1-54): (46-99) or 84: 16, and for another example 16: 84;
preferably, the CsCl-ZrCl is used when the melting point temperature of the chloride molten salt is 750 ℃ or lower4In molten salt, CsCl: ZrCl4The mole percentage of (1-61): (39-99) or (74-99): (1-26), for example 18: 82 or 78: 22; more preferably, the CsCl-ZrCl is used when the melting point temperature of the chloride molten salt is 550 ℃ or lower4In molten salt, CsCl: ZrCl4Is preferably (1-47)：(53-99)。
4. The purification method of a single component in a chloride molten salt according to claim 3, characterized in that the NaCl-ZrCl is used when the melting point temperature of the chloride molten salt is 750 ℃ or less4In molten salt, NaCl: ZrCl4The mole percentage of (1-87): (13-99), for example 1:99 or 57: 43; preferably, the NaCl-ZrCl is used when the melting point temperature of the chloride molten salt is 550 ℃ or lower4In molten salt, NaCl: ZrCl4The mole percentage of (1-60): (40-99) or (71-73): (27-29);
preferably, the KCl-ZrCl is used when the melting point temperature of the chloride molten salt is below 750 DEG C4In molten salt, KCl: ZrCl4The mole percentage of (1-62): (38-99) or (69-94): (6-31), for example 1:99 or 43: 57; more preferably, the KCl-ZrCl is used when the melting point temperature of the chloride molten salt is 550 ℃ or lower4In molten salt, KCl: ZrCl4The mole percentage of (1-51): (49-99);
preferably, when the melting point temperature of the chloride molten salt is 550 ℃ or lower, the LiCl-AlCl is adopted3In molten salt, LiCl: AlCl3The mole percentage of (1-69): (31-99), e.g., 13: 87;
preferably, the KCl-BiCl is used when the melting point temperature of the chloride molten salt is below 750 DEG C3In molten salt, KCl: BiCl3The mole percentage of (1-93): (7-99), e.g., 17: 83; more preferably, when the melting point temperature of the chloride molten salt is 550 ℃ or less, KCl: BiCl3The mole percentage of (1-79): (21-99), for example (1-70): (30-99);
preferably, when the melting point temperature of the chloride molten salt is 550 ℃ or less, the LiCl-ZnCl is used as the material2In molten salt, LiCl: ZnCl2The mole percentage of (1-85): (15-99), for example 1: 99.
5. The purification method of a single component in a chloride molten salt according to claim 1, wherein the temperature of a tower kettle of the plate rectifying tower is 190-800 ℃;
preferably, the temperature of a tower kettle of the plate-type rectifying tower is 30-50 ℃ higher than the melting point of the chloride fused salt;
preferably, the temperature of the plate of the plate rectifying tower is 5-50 ℃ higher than the melting point of the reflux of the plate rectifying tower, and more preferably 30-50 ℃;
preferably, when the single component is ZrCl4When the temperature is high, the temperature of a tower kettle of the plate type rectifying tower is 437-750 ℃;
preferably, when the single component is AlCl3、BeCl2、BiCl3Or ZnCl2When the temperature is higher than the set temperature, the temperature of a tower kettle of the plate rectifying tower is 190-415 ℃;
when the chloride molten salt is prepared from the following raw materials in percentage by mole 35: 6: KCl-MgCl of 592-ZrCl4When the reflux of the plate-type rectifying tower is KCl-MgCl2Preferably, the temperature of a tower kettle of the plate type rectifying tower is 450-750 ℃, and the temperature of a tower plate of the plate type rectifying tower is 700-750 ℃; more preferably, the temperature of a tower kettle of the plate type rectifying tower is 700-750 ℃, and the temperature of a tower plate of the plate type rectifying tower is 700-750 ℃; wherein, the reflux of the plate-type rectifying tower is KCl-MgCl2The melting point of (b) is 690 ℃;
when the chloride molten salt is 45 mol percent: 52: KCl-MgCl of 32-ZrCl4When the reflux of the plate-type rectifying tower is KCl-MgCl2Preferably, the temperature of a tower kettle of the plate type rectifying tower is 475-550 ℃, and the temperature of a tower plate of the plate type rectifying tower is 500-550 ℃;
when the chloride molten salt is 16 mol percent: CsCl-BeCl of 842In the process, the temperature of a tower kettle of the plate type rectifying tower is preferably 320-380 ℃, and the temperature of a tower plate of the plate type rectifying tower is preferably 650-700 ℃;
when the chloride molten salt is 84: CsCl-BeCl of 162When the reflux of the plate rectifying tower is CsCl, preferably, the temperature of a tower kettle of the plate rectifying tower is 650-700 ℃, and the temperature of a tower plate of the plate rectifying tower is 650-700 ℃;
when the chloride molten salt is 18 mol percent: CsCl-ZrCl 824Preferably, the temperature of a tower kettle of the plate type rectifying tower is 400-450 ℃, and the temperature of a tower plate of the plate type rectifying tower is 650-700 ℃;
when the chloride molten salt is 78 mol percent: CsCl-ZrCl 224When the reflux of the plate rectifying tower is CsCl, preferably, the temperature of a tower kettle of the plate rectifying tower is 700-750 ℃, and the temperature of a tower plate of the plate rectifying tower is 650-700 ℃;
when the chloride molten salt is in a molar percentage of 1:99 NaCl-ZrCl4Preferably, the temperature of a tower kettle of the plate type rectifying tower is 450-500 ℃, and the temperature of a tower plate of the plate type rectifying tower is 800-850 ℃;
when the chloride molten salt is 57:43 NaCl-ZrCl4Preferably, the temperature of a tower kettle of the plate type rectifying tower is 800-850 ℃, and the temperature of a tower plate of the plate type rectifying tower is 800-850 ℃;
when the chloride molten salt is in a molar percentage of 1:99 KCl-ZrCl4Preferably, the temperature of a tower kettle of the plate type rectifying tower is 450-500 ℃, and the temperature of a tower plate of the plate type rectifying tower is 450-500 ℃;
when the chloride molten salt is prepared from the following raw materials in percentage by mole of 43: KCl-ZrCl of 574Preferably, the temperature of a tower kettle of the plate type rectifying tower is 800-850 ℃, and the temperature of a tower plate of the plate type rectifying tower is 800-850 ℃;
when the chloride molten salt is in a molar percentage of 1:99 LiCl-ZnCl2Preferably, the temperature of a tower kettle of the plate type rectifying tower is 350-370 ℃, and the temperature of a tower plate of the plate type rectifying tower is 350-370 ℃;
when the chloride molten salt is in a molar percentage of 13:87 LiCl-AlCl3Preferably, the temperature of a tower kettle of the plate type rectifying tower is 200-220 ℃, and the temperature of a tower plate of the plate type rectifying tower is 200-220 ℃;
when the chloride molten salt is 17 mol percent: 83 KCl-BiCl3Preferably, the temperature of the tower kettle of the plate-type rectifying tower is higherThe temperature is 200-220 ℃, and the temperature of the plate rectifying tower is 200-220 ℃.
6. The purification method of a single component in a chloride molten salt according to claim 1, wherein a tray temperature of the plate rectifying tower is 350-700 ℃;
and/or the plate rectifying tower has 15-40 plates, such as 25 or 40 plates.
7. The method for purifying a single component in chloride molten salt according to claim 1, characterized in that the chloride molten salt is stored in a molten salt storage device before being added to the plate rectifier.
8. The method for purifying single components in chloride molten salt according to claim 7, characterized in that lining materials of the plate rectifying tower and the molten salt storage device are high-temperature materials which are resistant to oxygen-free elements above 800 ℃, such as nickel-based alloy or nickel metal.
9. The method for purifying a single component in chloride molten salt according to claim 7, wherein the molten salt storage device is further provided with a gas passage for introducing inert gas to convey the molten salt in the molten salt storage device to a tower kettle of the plate rectifying tower.
10. The purification method of a single component in chloride molten salt according to claim 1, characterized in that distillate is collected from the tower top of the plate rectifying tower after rectification, and the collection of the distillate is realized through a collection device.
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|---|---|---|---|---|
| US11931763B2 (en) | 2019-11-08 | 2024-03-19 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB771144A (en) * | 1954-04-16 | 1957-03-27 | Nat Lead Co | Improvements in or relating to the purification of zirconium tetrachloride |
| US4222998A (en) * | 1978-05-26 | 1980-09-16 | Warman International Limited | Production of bismuth trichloride |
| GB2150549A (en) * | 1983-12-01 | 1985-07-03 | Pavel Hurt | Process for the separate recovery of metal chlorides from complex ores etc |
| US4749448A (en) * | 1986-12-18 | 1988-06-07 | Westinghouse Electric Corp. | Zirconium and hafnium tetrachloride separation by extractive distillation with molten zinc chloride calcium and/or magnesium chloride solvent |
| WO1989010897A1 (en) * | 1988-05-06 | 1989-11-16 | Sommers James A | Ultra high purity halides and their preparation |
| CN1561401A (en) * | 2001-10-03 | 2005-01-05 | 优米科尔公司 | Chloride melt process for the separation and recovery of zinc |
| CN101155759A (en) * | 2005-04-04 | 2008-04-02 | 日本轻金属株式会社 | High-purity anhydrous aluminum chloride and process for production thereof |
| CN101638249A (en) * | 2009-09-04 | 2010-02-03 | 石政君 | Zirconium tetrachloride purification method |
| CN102107875A (en) * | 2009-12-24 | 2011-06-29 | 北京有色金属研究总院 | Method for preparing silicon tetrachloride for optical fiber |
| CN107311213A (en) * | 2017-07-13 | 2017-11-03 | 中国恩菲工程技术有限公司 | The preparation method of high-purity water aluminium chloride of nothing three |
| CN111321425A (en) * | 2020-03-19 | 2020-06-23 | 东北大学 | Molten salt chlorination TiCl production4Comprehensive recycling method of discharged waste salt |
| CN111455406A (en) * | 2020-04-10 | 2020-07-28 | 上海太洋科技有限公司 | Preparation method of high-purity beryllium chloride and nuclear pure-grade metal beryllium |
-
2020
- 2020-12-02 CN CN202011402962.1A patent/CN112357885A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB771144A (en) * | 1954-04-16 | 1957-03-27 | Nat Lead Co | Improvements in or relating to the purification of zirconium tetrachloride |
| US4222998A (en) * | 1978-05-26 | 1980-09-16 | Warman International Limited | Production of bismuth trichloride |
| GB2150549A (en) * | 1983-12-01 | 1985-07-03 | Pavel Hurt | Process for the separate recovery of metal chlorides from complex ores etc |
| US4749448A (en) * | 1986-12-18 | 1988-06-07 | Westinghouse Electric Corp. | Zirconium and hafnium tetrachloride separation by extractive distillation with molten zinc chloride calcium and/or magnesium chloride solvent |
| WO1989010897A1 (en) * | 1988-05-06 | 1989-11-16 | Sommers James A | Ultra high purity halides and their preparation |
| CN1561401A (en) * | 2001-10-03 | 2005-01-05 | 优米科尔公司 | Chloride melt process for the separation and recovery of zinc |
| CN101155759A (en) * | 2005-04-04 | 2008-04-02 | 日本轻金属株式会社 | High-purity anhydrous aluminum chloride and process for production thereof |
| CN101638249A (en) * | 2009-09-04 | 2010-02-03 | 石政君 | Zirconium tetrachloride purification method |
| CN102107875A (en) * | 2009-12-24 | 2011-06-29 | 北京有色金属研究总院 | Method for preparing silicon tetrachloride for optical fiber |
| CN107311213A (en) * | 2017-07-13 | 2017-11-03 | 中国恩菲工程技术有限公司 | The preparation method of high-purity water aluminium chloride of nothing three |
| CN111321425A (en) * | 2020-03-19 | 2020-06-23 | 东北大学 | Molten salt chlorination TiCl production4Comprehensive recycling method of discharged waste salt |
| CN111455406A (en) * | 2020-04-10 | 2020-07-28 | 上海太洋科技有限公司 | Preparation method of high-purity beryllium chloride and nuclear pure-grade metal beryllium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11931763B2 (en) | 2019-11-08 | 2024-03-19 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
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