Zinc ion lewis acid molten salt method for purifying crude ZrCl4

Abstract

The invention relates to the technical field of sponge zirconium production, in particular to a zinc ion Lewis acid molten salt method for purifying crude ZrCl4, which comprises the following steps: step 1, respectively placing enough ZnCl2, NaCl and KCl in a drying box for drying, setting the drying temperature of the drying box to be 105 DEG C, setting the working time of the drying box to be 10 hours, and separately storing ZnCl2, NaCl and KCl after drying is completed. By arranging a heat insulation shell, a heating bin, a screening plate, a sealing top cover, a driving motor, a heating device, a heat conduction shaft, a stirring rod and a scraping plate and combining a zinc ion lewis acid molten salt method for purifying crude ZrCl4, the crude ZrCl4 can be purified, the total mass percentage of Zr is increased to 36%, the total mass percentage of Fe is reduced to 0.004%, and the purity of ZrCl4 is improved. According to the method, the total mass percentage of Al is reduced to 0.001%, the purification effect on Fe and Al impurities in coarse ZrCl4 is obvious, and the purity of elemental zirconium generated by reducing the purified ZrCl4 is high, and the crystallinity is good.

Description

Technical Field

[0001] The invention relates to the technical field of sponge zirconium production, in particular to a method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt. Background Art

[0002] The production process of nuclear-grade sponge zirconium mainly includes four steps: zircon sand decomposition and zirconium oxychloride preparation, zirconium hafnium separation and zirconium oxide preparation, zirconium tetrachloride (ZrCl4) refining, magnesium thermal reduction and distillation finishing. Crude ZrCl4 is an important intermediate raw material for the preparation of metallic zirconium. It is generally prepared by carbon chlorination of zirconium oxide (electrofused desiliconized zirconium, zirconium ore). The crude ZrCl4 obtained by chlorination contains impurities such as iron, aluminum, silicon, titanium and their chloride impurities, so the crude ZrCl4 needs to be purified.

[0003] At present, there are two main methods for purifying crude ZrCl4: hydrogen purification and molten salt purification. However, the existing hydrogen purification process has problems such as high risk factor and high Al impurity content, so it is seldom used. Molten salt purification of crude ZrCl4 generally adopts NaCl-KCl molten salt system, but this system has the problem of poor removal effect of Fe and Al impurities. In order to reduce the Al impurity content that is difficult to remove in the traditional boiling chlorination method and meet the precision requirements of high-grade Zr precursors, it is necessary to improve the molten salt purification process of crude ZrCl4. Therefore, a zinc ion Lewis acid molten salt method for purifying crude ZrCl4 is proposed to solve the above problems. Summary of the invention

[0004] The object of the present invention is to provide a method for purifying crude ZrCl4 using a zinc ion Lewis acid molten salt, so as to solve the problem that the NaCl-KCl molten salt system for purifying crude ZrCl4 has poor removal effect on Fe and Al impurities.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt comprises the following steps:

[0007] Step 1: Place sufficient amounts of ZnCl2, NaCl, and KCl in a drying oven for drying. The drying temperature of the drying oven is set to 105°C, and the working time of the drying oven is set to 10h. After drying, ZnCl2, NaCl, and KCl are stored separately;

[0008] Step 2: Take out a certain amount of ZnCl2, NaCl, and KCl, mix them evenly in a mass ratio of 1:0.5:0.5, and then heat the mixed raw materials to maintain a high temperature of more than 800.7°C to obtain a zinc ion Lewis acid molten salt system, referred to as ZnCl2-0.5NaCl-0.5KCl molten salt system;

[0009] Step 3: The crude ZrCl4 is melted in a ZnCl2-0.5NaCl-0.5KCl molten salt system, and zirconium and impurities of aluminum, sodium, and potassium react with the molten salt to form Na2ZrCl4, K2ZrCl6, Zn(Al)Na0.5K0.5Cl6, and ZnNa0.5K0.5ZrCl7 complex salts respectively;

[0010] Step 4: Continue heating to raise the temperature of the molten salt. Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 complex salts are stable and do not decompose at high temperatures, while Na2ZrCl4 and K2ZrCl6 are decomposed into sodium, potassium and ZrCl4 at high temperatures, thereby obtaining pure ZrCl4.

[0011] Step 5: The presence of Zn element can be detected by energy dispersive spectrometer (EDS). Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 are both ionic compounds and can be removed by water system;

[0012] The above steps require a crude ZrCl purification device, including a fixed sleeve, an insulating shell and a sealed top cover, the bottom of the fixed sleeve is fixedly connected with three support rods, the bottom of the support rods is fixedly connected with a base, the upper side of the base is provided with a receiving cup, the inner side of the fixed sleeve is fixedly connected with an insulating shell, the front half of the bottom of the insulating shell is provided with a discharge port, the inner side of the insulating shell is fixedly connected with a heating bin, the front half of the bottom of the heating bin is fixedly connected with a discharge switch valve, the front half of the bottom of the insulating shell is fixedly connected with a positioning tube, the outer side of the positioning tube is spirally connected with a mounting tube, and the bottom of the mounting tube is fixedly connected with a screening plate, The top of the heat-insulating shell is spirally connected with a sealing top cover, the front half of the sealing top cover is provided with a feed port, the top front half of the sealing top cover is fixedly connected with a feed switch valve, the top of the sealing top cover is fixedly connected with a handle, the top middle position of the sealing top cover is fixedly connected with a driving motor, the bottom main shaft of the driving motor is fixedly connected with a heating device, the outer side of the heating device is rotatably connected to the sealing top cover, the bottom of the heating device is fixedly connected with a heat-conducting shaft, the side of the heat-conducting shaft is fixedly connected with a plurality of stirring rods, the relatively outer sides of the stirring rods are fixedly connected with a scraper, and the top and bottom of the scraper are fixedly connected to the heat-conducting shaft through a connecting hole.

[0013] Preferably, the chemical reaction formula of the zinc ion Lewis acid molten salt method for purifying crude ZrCl4 is as follows:

[0014] AlCl3+ZnCl2 / 0.5NaCl / 0.5KCl→Zn(Al)Na 0.5 K 0.5 Cl6;

[0015] ZrCl4+ZnCl2 / 0.5NaCl / 0.5KCl→ZnNa 0.5 K 0.5 ZrCl7.

[0016] Preferably, the upper half of the base is provided with a rectangular groove, the bottom of the material receiving cup is located in the rectangular groove of the base, and the heat-insulating outer shell and the sealing top cover both have high heat insulation properties.

[0017] Preferably, the discharge switch valve is located directly above the discharge port, the positioning tube is located directly below the discharge port, a threaded protrusion is provided on the outer side of the positioning tube, and a threaded groove is provided on the inner side of the mounting tube.

[0018] Preferably, a rotating groove is provided in the middle of the sealing top cover, the heating device is located in the rotating groove of the sealing top cover, and the feed switch valve is located directly above the feed port.

[0019] Preferably, the heat conduction axis is distributed vertically, the stirring rods are distributed horizontally, the stirring rods are distributed equidistantly in the upper and lower directions, and connection holes are provided at the middle positions of the top and bottom of the scraper.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] In the present invention, by setting up a heat-insulating shell, a heating bin, a screening plate, a sealing top cover, a driving motor, a heating device, a heat-conducting shaft, a stirring rod and a scraper, in combination with a zinc ion Lewis acid molten salt method for purifying crude ZrCl4, crude ZrCl4 can be purified, the total weight percentage of Zr is increased to 36%, the total weight percentage of Fe element is reduced to 0.004%, and the total weight percentage of Al is reduced to 0.001%. The method has obvious purification effect on Fe and Al impurities in crude ZrCl4, and the purified ZrCl4 is reduced to generate single zirconium with high purity and good crystallinity. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0023] Figure 2 This is a schematic diagram of the structure of the material receiving component of the present invention;

[0024] Figure 3It is a cross-sectional view of the internal structure of the present invention;

[0025] Figure 4 It is a cross-sectional view of the shell assembly structure of the present invention;

[0026] Figure 5 It is a cross-sectional view of the cover assembly structure of the present invention;

[0027] Figure 6 It is a schematic diagram of the structure of the heating component of the present invention.

[0028] In the figure: 1. fixing sleeve; 2. supporting rod; 3. base; 4. collecting cup; 5. heat-insulating shell; 6. discharging port; 7. heating chamber; 8. discharging switch valve; 9. positioning tube; 10. mounting tube; 11. screening plate; 12. sealing top cover; 13. feeding port; 14. feeding switch valve; 15. lifting handle; 16. driving motor; 17. heating device; 18. heat-conducting shaft; 19. stirring rod; 20. scraper. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by directional words such as "front, back, up, down, left, right", "lateral, vertical, perpendicular, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the drawings. They are only for the convenience of describing the present invention and simplifying the description. Unless otherwise specified, these directional words do not indicate or imply that the devices or elements referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of the present invention. The directional words "inside and outside" refer to the inside and outside relative to the contours of each component itself.

[0031] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. If not otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the present invention.

[0032] See also Figure 1-6 , the present invention provides a technical solution:

[0033] A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt comprises the following steps:

[0034] Step 1: Place sufficient amounts of ZnCl2, NaCl, and KCl in a drying oven for drying. The drying temperature of the drying oven is set to 105°C, and the working time of the drying oven is set to 10h. After drying, ZnCl2, NaCl, and KCl are stored separately;

[0035] Step 2: Take out a certain amount of ZnCl2, NaCl, and KCl, mix them evenly in a mass ratio of 1:0.5:0.5, and then heat the mixed raw materials to maintain a high temperature of more than 800.7°C to obtain a zinc ion Lewis acid molten salt system, referred to as ZnCl2-0.5NaCl-0.5KCl molten salt system;

[0036] Step 3: The crude ZrCl4 is melted in a ZnCl2-0.5NaCl-0.5KCl molten salt system, and zirconium and impurities of aluminum, sodium, and potassium react with the molten salt to form Na2ZrCl4, K2ZrCl6, Zn(Al)Na0.5K0.5Cl6, and ZnNa0.5K0.5ZrCl7 complex salts respectively;

[0037] Step 4: Continue heating to raise the temperature of the molten salt. Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 complex salts are stable and do not decompose at high temperatures, while Na2ZrCl4 and K2ZrCl6 are decomposed into sodium, potassium and ZrCl4 at high temperatures, thereby obtaining pure ZrCl4.

[0038] Step 5: The presence of Zn element can be detected by energy dispersive spectrometer (EDS). Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 are both ionic compounds and can be removed by water system.

[0039] The above steps require a crude ZrCl4 purification device, including a fixed sleeve 1, an insulating shell 5 and a sealed top cover 12. The bottom of the fixed sleeve 1 is fixedly connected with three support rods 2, the bottom of the support rods 2 is fixedly connected with a base 3, the upper side of the base 3 is provided with a receiving cup 4, the inner side of the fixed sleeve 1 is fixedly connected with an insulating shell 5, the front half of the bottom of the insulating shell 5 is provided with a discharge port 6, the inner side of the insulating shell 5 is fixedly connected with a heating bin 7, the bottom front half of the heating bin 7 is fixedly connected with a discharge switch valve 8, the bottom front half of the insulating shell 5 is fixedly connected with a positioning tube 9, the outer side of the positioning tube 9 is spirally connected with a mounting tube 10, the bottom of the mounting tube 10 is fixedly connected with a screening plate 11, the top of the insulating shell 5 A sealing top cover 12 is spirally connected to the top, a feeding port 13 is provided on the front half of the sealing top cover 12, a feeding switch valve 14 is fixedly connected to the front half of the top of the sealing top cover 12, a handle 15 is fixedly connected to the top of the sealing top cover 12, a driving motor 16 is fixedly connected to the middle position of the top of the sealing top cover 12, a heating device 17 is fixedly connected to the bottom main shaft of the driving motor 16, the outer side of the heating device 17 is rotatably connected to the sealing top cover 12, a heat-conducting shaft 18 is fixedly connected to the bottom of the heating device 17, a plurality of stirring rods 19 are fixedly connected to the side of the heat-conducting shaft 18, a scraper 20 is fixedly connected to the relatively outer side of the stirring rod 19, and the top and bottom of the scraper 20 are fixedly connected to the heat-conducting shaft 18 through connecting holes.

[0040] Further, the chemical reaction formula of the zinc ion Lewis acid molten salt method for purifying crude ZrCl4 is as follows:

[0041] AlCl3+ZnCl2 / 0.5NaCl / 0.5KCl→Zn(Al)Na 0.5 K 0.5 Cl6;

[0042] ZrCl4+ZnCl2 / 0.5NaCl / 0.5KCl→ZnNa 0.5 K 0.5 ZrCl7.

[0043] Furthermore, a rectangular groove is provided in the upper part of the base 3, and the bottom of the receiving cup 4 is located in the rectangular groove of the base 3. The heat-insulating outer shell 5 and the sealing top cover 12 both have high heat insulation properties.

[0044] Furthermore, the discharge switch valve 8 is located directly above the discharge port 6 , the positioning tube 9 is located directly below the discharge port 6 , a threaded protrusion is provided on the outer side of the positioning tube 9 , and a threaded groove is provided on the inner side of the mounting tube 10 .

[0045] Furthermore, a rotation groove is provided in the middle of the sealing top cover 12 , the heating device 17 is located in the rotation groove of the sealing top cover 12 , and the feed switch valve 14 is located directly above the feed port 13 .

[0046] Furthermore, the heat conduction shaft 18 is distributed vertically, the stirring rods 19 are distributed horizontally, the stirring rods 19 are distributed equidistantly in the upper and lower directions, and connection holes are provided at the middle positions of the top and bottom of the scraper 20 .

[0047] Working process: the discharge switch valve 8, feed switch valve 14, drive motor 16 and heating device 17 of the device are all electrical instruments. The device is provided with an external controller, and the operating states of the discharge switch valve 8, feed switch valve 14, drive motor 16 and heating device 17 can be adjusted by manually operating the external controller. The above are all prior arts. Before use, the device should be stably fixed and powered on; sufficient amounts of ZnCl2, NaCl and KCl are placed in a drying oven for drying, the drying temperature of the drying oven is set to 105°C, and the working time of the drying oven is set to 10h. After drying, ZnCl2, NaCl and KCl are stored separately; a certain amount of ZnCl2, NaCl and KCl are taken out, and ZnCl2, NaCl and KCl are placed in a drying oven for drying; the temperature of the drying oven is set to 105°C, and the working time of the drying oven is set to 10h. Cl and KCl are mixed evenly in a mass ratio of 1:0.5:0.5, and then the mixed raw materials are poured into the heating chamber 7 inside the heat-insulating shell 5, the sealing top cover 12 is fixed to the top of the heat-insulating shell 5 by holding the handle 15, and the external controller is manually operated to start the driving motor 16 and the heating device 17, and the heat-conducting shaft 18 is heated by the heating device 17. The heat-conducting shaft 18 can quickly transfer heat to the raw materials, so that the raw materials are heated and maintained at a high temperature of more than 800.7°C. At the same time, the heating device 17 and the heat-conducting shaft 18 are driven to rotate by the driving motor 16, and then the stirring rod 19 and the scraper 20 are rotated. The stirring rod 19 can continuously stir the raw materials, and the scraper 20 can scrape the raw materials on the inner wall of the heating chamber 7. The raw materials are in a molten state and After being fully mixed, a zinc ion Lewis acid molten salt system, referred to as a ZnCl2-0.5NaCl-0.5KCl molten salt system, can be obtained; the feed switch valve 14 is opened by manually operating the external controller, and the crude ZrCl4 is added into the heating bin 7 through the feed port 13, so that the crude ZrCl4 is melted in the ZnCl2-0.5NaCl-0.5KCl molten salt system, and then the feed switch valve 14 is closed, and zirconium and impurities such as aluminum, sodium and potassium form Na2ZrCl4, K2ZrCl6, Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 complex salts with the molten salt respectively; the heating is continued by the heating device 17 and the heat-conducting shaft 18, so that the molten salt mixture in the heating bin 7 continues to heat up, and Zn(Al )Na0.5K0.5Cl6, ZnNa0.5K0.5ZrCl7 complex salts are stable and do not decompose at high temperatures, while Na2ZrCl4 and K2ZrCl6 are decomposed into sodium, potassium and ZrCl4 at high temperatures, thereby obtaining pure ZrCl4; the presence of Zn element can be detected by energy dispersant EDS, Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 are both ionic compounds and soluble in water, and it is only necessary to open the feed switch valve 14 again, and inject clean distilled water into the heating chamber 7 through the feed port 13, at which time the drive motor 16 is in the starting state, and the stirring rod 19 continues to stir, so that Zn(Al)Na0.5K0.5Cl6, ZnNa0.5K0.5ZrCl7 are ionic compounds and soluble in water, and it is only necessary to open the feed switch valve 14 again, and inject clean distilled water into the heating chamber 7 through the feed port 13, and at this ...5ZrCl7 quickly dissolves in water, and then the external controller is manually operated to open the discharge switch valve 8, and the liquid is discharged from the heating bin 7 through the discharge port 6. Since the insulation shell 5 is supported and fixed on the top of the base 3 by the fixed sleeve 1 and the support rod 2, the receiving cup 4 is located directly below the insulation shell 5, and the positioning tube 9 fixed to the bottom of the insulation shell 5 and the mounting tube 10 with the screening plate 11 are spirally connected, so the liquid can be filtered through the screening plate 11, and the solution carrying Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 flows into the receiving cup 4 on the upper side of the base 3, while the solid particles remain in the heating bin 7; turn off the drive motor 16 and the heating device 17, and after a period of time, the solution carrying Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 cools down and is poured into the waste liquid tank. At this time, the solid in the heating bin 7 has also cooled down. , after placing a new receiving cup 4 on the upper side of the base 3, remove the mounting tube 10 and the screening plate 11, and pour out the solid containing ZrCl4 to obtain high-purity ZrCl4; the main components of crude ZrCl4 before purification are ZrCl4, ZrO2, HfO2, C, AlCl3, FeCl3, SiC, etc., among which the total mass percentage of Zr is about 27%, the total mass percentage of Fe element is 0.02%, and the total mass percentage of A1 is about 0.16%. After the operation of this method, the total mass percentage of Zr is increased to 36%, the total mass percentage of Fe element is reduced to 0.004%, and the total mass percentage of Al is reduced to 0.001%. This method has obvious purification effect on Fe and Al impurities in crude ZrCl4. After purification, ZrCl4 is reduced to generate single zirconium with high purity and good crystallinity. .

[0048] This article uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. The above is only a preferred implementation of the present invention. It should be pointed out that due to the limitations of textual expression and the objective existence of infinite specific structures, ordinary technicians in this technical field can make several improvements, modifications or changes without departing from the principles of the present invention, and can also combine the above technical features in an appropriate manner; these improvements, modifications, changes or combinations, or the direct application of the inventive concept and technical solution to other occasions without improvement, should be regarded as the protection scope of the present invention.

Claims

1. A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt, characterized in that: The following steps are involved: Step 1: Place sufficient amounts of ZnCl2, NaCl, and KCl in a drying oven for drying. The drying temperature of the drying oven is set to 105°C, and the working time of the drying oven is set to 10h. After drying, ZnCl2, NaCl, and KCl are stored separately; Step 2: Take out a certain amount of ZnCl2, NaCl, and KCl, mix them evenly in a mass ratio of 1:0.5:0.5, and then heat the mixed raw materials to maintain a high temperature of more than 800.7°C to obtain a zinc ion Lewis acid molten salt system, referred to as ZnCl2-0.5NaCl-0.5KCl molten salt system; Step 3: The crude ZrCl4 is melted in a ZnCl2-0.5NaCl-0.5KCl molten salt system, and zirconium and impurities of aluminum, sodium, and potassium react with the molten salt to form Na2ZrCl4, K2ZrCl6, Zn(Al)Na0.5K0.5Cl6, and ZnNa0.5K0.5ZrCl7 complex salts respectively; Step 4: Continue heating to raise the temperature of the molten salt. Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 complex salts are stable and do not decompose at high temperatures, while Na2ZrCl4 and K2ZrCl6 are decomposed into sodium, potassium and ZrCl4 at high temperatures, thereby obtaining pure ZrCl4. Step 5: The presence of Zn element can be detected by energy dispersive spectrometer (EDS). Zn(Al)Na0.5K0.5Cl6 and ZnNa0.5K0.5ZrCl7 are both ionic compounds and can be removed by water system; The above steps require a crude ZrCl4 purification device, comprising a fixed sleeve (1), an insulating outer shell (5) and a sealing top cover (12), characterized in that the bottom of the fixed sleeve (1) is fixedly connected to three support rods (2), the bottom of the support rods (2) is fixedly connected to a base (3), the upper side of the base (3) is provided with a receiving cup (4), the inner side of the fixed sleeve (1) is fixedly connected to an insulating outer shell (5), the front half of the bottom of the insulating outer shell (5) is provided with a discharge port (6), the inner side of the insulating outer shell (5) is fixedly connected to a heating bin (7), the front half of the bottom of the heating bin (7) is fixedly connected to a discharge switch valve (8), the front half of the bottom of the insulating outer shell (5) is fixedly connected to a positioning tube (9), the outer side of the positioning tube (9) is spirally connected to a mounting tube (10), the bottom of the mounting tube (10) is fixedly connected to a screening plate (11), and the insulating The top of the housing (5) is spirally connected to a sealing top cover (12), the front half of the sealing top cover (12) is provided with a feed port (13), the front half of the top of the sealing top cover (12) is fixedly connected to a feed switch valve (14), the top of the sealing top cover (12) is fixedly connected to a handle (15), the middle of the top of the sealing top cover (12) is fixedly connected to a driving motor (16), the bottom main shaft of the driving motor (16) is fixedly connected to a heating device (17), the outer side of the heating device (17) is rotatably connected to the sealing top cover (12), the bottom of the heating device (17) is fixedly connected to a heat-conducting shaft (18), the side of the heat-conducting shaft (18) is fixedly connected to a plurality of stirring rods (19), the opposite outer sides of the stirring rods (19) are fixedly connected to a scraper (20), and the top and bottom of the scraper (20) are fixedly connected to the heat-conducting shaft (18) through a connecting hole.

2. A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt according to claim 1, characterized in that: The chemical reaction formula of the zinc ion Lewis acid molten salt method for purifying crude ZrCl4 is as follows: <h2 style=";text-align:left;direction:ltr">AlCl3+ZnCl2 / 0.5NaCl / 0.5KCl→Zn(Al)Na<h2 style=";text-align:left;direction:ltr"> 0.5 <h2 style=";text-align:left;direction:ltr"> K<h2 style=";text-align:left;direction:ltr"> 0.5 <h2 style=";text-align:left;direction:ltr"> Cl6; ZrCl4+ZnCl2 / 0.5NaCl / 0.5KCl→ZnNa 0.5 K 0.5 ZrCl7。 3. A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt according to claim 1, characterized in that: The upper part of the base (3) is provided with a rectangular groove, the bottom of the material receiving cup (4) is located in the rectangular groove of the base (3), and the heat-insulating outer shell (5) and the sealing top cover (12) both have high heat insulation properties.

4. A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt according to claim 1, characterized in that: The discharge switch valve (8) is located directly above the discharge port (6), and the positioning tube (9) is located directly below the discharge port (6). The outer side of the positioning tube (9) is provided with a threaded protrusion, and the inner side of the mounting tube (10) is provided with a threaded groove.

5. A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt according to claim 1, characterized in that: A rotating groove is provided in the middle of the sealing top cover (12), the heating device (17) is located in the rotating groove of the sealing top cover (12), and the feed switch valve (14) is located directly above the feed port (13).

6. A method for purifying crude ZrCl4 using zinc ion Lewis acid molten salt according to claim 1, characterized in that: The heat-conducting shaft (18) is distributed vertically, the stirring rods (19) are distributed horizontally, the stirring rods (19) are distributed equidistantly in the upper and lower directions, and the scraper (20) is provided with connection holes at the middle positions of the top and bottom.

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