A method for producing fine zirconium tetrachloride

Abstract

The application belongs to the technical field of sponge zirconium production and relates to a method for preparing and producing refined zirconium tetrachloride, which comprises the following steps: S1, boiling chlorination, a carbon powder filtering settler is connected to the gas outlet of a chlorination furnace, the gas outlet of the carbon powder filtering settler is connected to a hydrogen charging iron remover, the cavity temperature in the carbon powder filtering settler and the hydrogen charging iron remover is respectively controlled to be 400±10 DEG C, and hydrogen is introduced into the hydrogen charging iron remover; S2, condensation, the gas outlet of the hydrogen charging iron remover is sequentially connected with a first-stage condenser, a second-stage condenser and a third-stage condenser, the cavity temperature in the first-stage condenser is controlled to be 280±10 DEG C, the cavity temperature in the second-stage condenser is controlled to be 240±10 DEG C, the cavity temperature in the third-stage condenser is controlled to be 220±10 DEG C, and the condensed materials at the outlets of the condensers are all refined zirconium tetrachloride. The method can completely cancel the purification process of the traditional refined zirconium tetrachloride preparation process, and greatly saves energy, manpower and other costs.

Description

Technical Field

[0001] This invention belongs to the field of sponge zirconium production technology, specifically, it relates to a method for preparing and producing refined zirconium tetrachloride. Background Technology

[0002] In 1940, Luxembourg scientist W.J. Klauer invented the magnesothermic reduction process for producing sponge zirconium, which is currently the main industrial method for producing sponge zirconium. The Klauer process mainly includes three steps: decomposition of zircon sand and preparation of crude zirconium tetrachloride; separation of zirconium and hafnium (separation is not necessary if producing general industrial-grade sponge zirconium); and refining of zirconium tetrachloride and magnesothermic reduction to produce sponge zirconium.

[0003] Currently, the vast majority of zirconium tetrachloride preparations in the industry follow the process flow below: boiling chlorination - condensation (to obtain crude zirconium tetrachloride) - purification (to obtain refined zirconium tetrachloride). The exhaust gas generated during the condensation process is treated to meet standards before being discharged. Because the product produced by this traditional boiling chlorination followed by condensation contains unreacted petroleum coke powder and impurities such as iron and aluminum from the raw materials, i.e., crude zirconium tetrachloride, it must be purified to remove impurities and become qualified refined zirconium tetrachloride in order to meet the subsequent quality requirements for industrial production of sponge zirconium. Therefore, the existing production process has technical problems such as complex process and high production cost. Summary of the Invention

[0004] The purpose of this invention is to provide a method for producing purified zirconium tetrachloride, comprising the following steps:

[0005] S1. Boiling chlorination: A carbon powder filter settling device is connected to the gas outlet of the chlorination furnace, and the gas outlet of the carbon powder filter settling device is connected to a hydrogen-filled iron remover. The chamber temperature in the carbon powder filter settling device and the hydrogen-filled iron remover is controlled at 400±10℃ respectively, and hydrogen is introduced into the hydrogen-filled iron remover.

[0006] S2. Condensation: The outlet of the hydrogen-filled iron remover is connected in series with a primary condenser, a secondary condenser, and a tertiary condenser. The internal temperature of the primary condenser is controlled at 280±10℃, the internal temperature of the secondary condenser is 240±10℃, and the internal temperature of the tertiary condenser is 220±10℃, so that the condensate at the outlet of each condenser is refined zirconium tetrachloride.

[0007] Preferably, in step S1, the raw materials for boiling chlorination are zirconium oxide, chlorine gas, and petroleum coke.

[0008] Preferably, in step S1, the toner filter settling device includes a housing, a filter assembly, and a backflushing assembly. Both the filter assembly and the backflushing assembly are housed within the housing, with the backflushing assembly positioned above the filter assembly. The housing has an outlet pipe at its top, a discharge pipe at its bottom, and an inlet pipe on its lower side. The inlet pipe is connected to the outlet of the chlorination furnace. The discharge pipe and the outlet pipe are equipped with discharge valves. The filter assembly improves the toner yield, while the backflushing assembly prevents clogging and ensures proper functioning of the filter assembly.

[0009] Preferably, the filter assembly uses a 400-mesh screen, which is located in the upper middle part of the housing. Because the high-temperature airflow is very fast, it carries some solid impurities (mainly fine carbon particles), easily causing the carbon content to exceed the standard. Therefore, installing a 400-mesh screen in the upper middle part of the carbon powder filter settler can reduce the airflow velocity of the coarse zirconium tetrachloride, which helps to reduce the amount of fine carbon particles carried. At the same time, it also acts as a physical barrier against the fine carbon particles, allowing more of them to settle.

[0010] Preferably, the backflushing assembly includes a backflushing pipe located above the filter assembly. This backflushing pipe is connected to an external compressed air source, and several backflushing nozzles are evenly distributed along the pipe, pointing towards the filter assembly. Since the filter assembly may experience poor airflow after continuous operation for more than 240 hours, thus affecting production efficiency, it is necessary to clean the filter assembly by introducing high-pressure air (0.4–0.6 MPa) through the backflushing pipe after shutdown. This backflushing method, involving 20–30 minutes of air injection, thoroughly cleans the filter, making it fully reusable and reducing production costs.

[0011] Preferably, the side wall of the housing is provided with an air extraction pipe, the air extraction port of which is located below the filter assembly, and a negative pressure back-extraction valve is provided on the air extraction pipe. A jet pump is connected to the end of the air extraction pipe furthest from the air extraction port. The jet pump, through the negative pressure back-extraction valve, extracts air from the toner filter settling chamber, maintaining a constant negative pressure in the lower cavity of the toner filter settling chamber. This prevents the cleaned toner from re-adsorbing onto the filter assembly, ensuring the cleaning effect on the filter assembly.

[0012] Preferably, the hydrogen-filled iron separator includes a second housing. A partition plate is inclined downwards and to the right at the top of the inner cavity of the second housing, dividing the upper part of the inner cavity into a left and right half-cavity. The left half-cavity has a structure that is smaller at the top and larger at the bottom, while the right half-cavity has a structure that is larger at the top and smaller at the bottom. The left half-cavity also has several baffles that allow the mixed gas flow within the hydrogen-filled iron separator to form an S-shaped corridor. An inlet pipe is located at the top of the left half-cavity, and a hydrogen filling pipe is located on the upper side. The inlet pipe is connected to the outlet of the carbon powder filter settling device. An outlet pipe is located at the top of the right half-cavity, and a discharge pipe is located at the bottom of the second housing. A discharge valve is installed on the discharge pipe. The mixed gas flow is deflected and its velocity reduced within the left half-cavity by the baffles, allowing for a more complete reaction. When entering the right half-cavity, the gas flow is faster at the bottom and slower in the upper expansion section, which is more conducive to the sedimentation of FeCl2.

[0013] Preferably, the carbon powder filter settling device, the hydrogen-filled iron remover, and each stage of the cooler are equipped with a temperature control device, which includes a temperature sensor, a cooler, and a heater, thereby making it easier to accurately control the temperature inside each device.

[0014] Preferably, the outer walls of the carbon powder filter settling device, the hydrogen charging iron remover, and each stage of the cooler are all provided with a heat insulation layer, and each stage of the cooler is provided with a collection box at the bottom. A discharge pipe is provided between the collection box and the corresponding cooler. The collection box is provided with a discharge port. The upper part of the inner cavity of each condenser is also provided with a partition plate II to improve the condensation effect.

[0015] Preferably, the condensate at the outlet of each stage of the condenser has the following contents: Fe content ≤ 0.015%, Al content ≤ 0.01%, C content ≤ 0.03%, Ti content ≤ 0.005%, and Si content ≤ 0.01%, which is basically consistent with the purity of refined zirconium tetrachloride produced by traditional purification processes and fully meets the production requirements of refined zirconium tetrachloride.

[0016] This invention also includes other steps or apparatuses that enable its proper implementation, all employing conventional methods in the art. Furthermore, steps or apparatuses not limited in this invention, such as chlorination furnaces and various condensers, employ existing technology in the art, and those skilled in the art can select them according to actual needs.

[0017] The working principle of this invention is as follows: One of the most significant impurities in crude zirconium tetrachloride is carbon. Carbon has a boiling point of 4827°C at standard atmospheric pressure, far exceeding that of zirconium tetrachloride and other impurities. Therefore, in the gaseous crude zirconium tetrachloride product exiting the chlorination furnace, carbon is solid and relatively easy to remove. By adding a carbon powder filter settling device at the chlorination furnace outlet and controlling the chamber temperature within the settling device at 400±10°C, the high-temperature gas flow from the chlorination furnace outlet first enters the settling device. The solid carbon powder particles naturally settle within the settling device, facilitating collection and periodic evacuation. Since zirconium tetrachloride has a boiling point of 331°C at standard atmospheric pressure, it does not undergo sublimation in the settling device and can continue flowing with the gas flow to subsequent processes.

[0018] The crude zirconium tetrachloride gas stream contains iron impurities, existing in the form of FeCl3. FeCl3 has a boiling point of 316℃ at standard atmospheric pressure, lower than that of zirconium tetrachloride. Therefore, it cannot be removed by physical methods. Thus, a hydrogen-charging iron separator needs to be added after the carbon powder filter settling tank. The temperature inside the hydrogen-charging iron separator is controlled at 400±10℃, and a certain proportion of hydrogen gas is introduced into the separator (the ratio of hydrogen charging rate to the rate of fused zirconium oxide material is 0.1–3%). After the zirconium tetrachloride gas stream enters the hydrogen-charging iron separator, the FeCl3 immediately reacts with the introduced hydrogen gas, and the iron element undergoes the following chemical reaction:

[0019] FeCl3 + 1 / 2H2 → FeCl2 + HCl

[0020] After the reaction, the iron element exists in the form of FeCl2. The boiling point of FeCl2 at standard atmospheric pressure is 1023℃, which is higher than the temperature of the cavity inside the hydrogen-charged iron separator. Therefore, it sublimates into a solid and settles at the bottom slag discharge port of the hydrogen-charged iron separator, thus achieving the purpose of iron removal.

[0021] After the hydrogen-filled iron remover, the first, second, and third stage condensers are connected. The condensation temperature of each condenser is controlled to be lower than the boiling point of zirconium tetrachloride under standard atmospheric pressure (331℃), so that zirconium tetrachloride can be fully collected in the third stage condenser. The collection process is the same as the traditional process, and will not be described in detail here.

[0022] The reason for controlling the condensing temperature of each stage of the condenser to be no lower than 220±10℃ is that impurities such as aluminum and titanium mainly exist in the gas phase in the form of chlorides. The boiling point of AlCl3 under standard atmospheric pressure is 178℃, and the boiling point of TiCl4 under standard atmospheric pressure is 135-136℃. The boiling points of other impurity chlorides are also lower than 220℃. Therefore, these impurities will not be condensed in the condenser and will be discharged into the tail gas treatment device in the form of gas for tail gas treatment. The tail gas treatment device adopts the existing technology in this field, which will not be described in detail here.

[0023] Compared with the prior art, this application has the following beneficial effects:

[0024] In this invention, the crude zirconium tetrachloride generated from the reaction in the chlorination furnace undergoes a series of processes, including carbon removal, iron removal, multi-stage condensation, and exhaust, to obtain highly pure zirconium tetrachloride. The impurities in this refined zirconium tetrachloride have the following contents: Fe content ≤0.015%, Al content ≤0.01%, C content ≤0.03%, Ti content ≤0.005%, and Si content ≤0.01%. This purity is basically consistent with that of refined zirconium tetrachloride produced by traditional purification processes. Therefore, this invention can completely eliminate the purification process in the traditional refined zirconium tetrachloride preparation process, greatly saving energy, labor, and other costs. Attached Figure Description

[0025] Figure 1 The diagram shows the overall process system of the present invention in Examples 1 to 3.

[0026] Figure 2 for Figure 1 A magnified schematic diagram of the carbon powder filter settling device.

[0027] Figure 3 for Figure 1 A magnified schematic diagram of the hydrogen-filled iron removal device.

[0028] Figure 4 This is a process system diagram of the prior art in Comparative Example 1. Detailed Implementation

[0029] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0030] Example 1

[0031] like Figures 1-3 As shown, this application proposes a method for producing purified zirconium tetrachloride, comprising the following steps:

[0032] S1. Boiling chlorination: Zirconia, chlorine and petroleum coke, the raw materials for boiling chlorination, are added to chlorination furnace 1. Carbon powder filter settling device 2 is connected to the gas outlet of the chlorination furnace, and the gas outlet of the carbon powder filter settling device is connected to hydrogen-filled iron remover 3. The temperature of the chamber in the carbon powder filter settling device is controlled at 408.5℃ and the temperature of the chamber in the hydrogen-filled iron remover is controlled at 409.2℃. At the same time, hydrogen is introduced into the hydrogen-filled iron remover.

[0033] S2. Condensation: The outlet of the hydrogen-filled iron remover is connected in series with a primary condenser 4, a secondary condenser 5, and a tertiary condenser 6. The internal temperature of the primary condenser is controlled at 289.7℃, the internal temperature of the secondary condenser is 248.9℃, and the internal temperature of the tertiary condenser is 229.4℃, so that the condensate at the outlet of each condenser is pure zirconium tetrachloride.

[0034] Specifically, the toner filter settling device includes a housing 21, a filter assembly 22, and a backflushing assembly 23. Both the filter assembly and the backflushing assembly are housed within the housing, with the backflushing assembly positioned above the filter assembly. The housing has an outlet pipe 24 at its top, a discharge pipe 25 at its bottom, and an inlet pipe 26 on its lower side. The inlet pipe is connected to the outlet of the chlorination furnace. The discharge pipe and the outlet pipe are equipped with discharge valves. The filter assembly improves the toner yield, while the backflushing assembly prevents clogging and ensures normal operation. The backflushing assembly includes a backflushing pipe positioned above the filter assembly, connected to an external compressed air source. Several backflushing nozzles (not shown in the figure) are evenly distributed along the backflushing pipe, pointing towards the filter assembly. Since the filter assembly may experience poor ventilation after continuous operation for more than 240 hours, production efficiency may be affected. When this happens, after shutting down the furnace, high-pressure air of 0.4–0.6 MPa needs to be introduced through the reverse flushing pipe to clean the filter components. Using this reverse flushing method, which involves 20–30 minutes of air injection, the filter will be thoroughly cleaned and can be reused, thus reducing production costs.

[0035] More specifically, the filter assembly uses a 400-mesh screen, which is located in the upper middle part of the housing. Because the high-temperature airflow is very fast, it carries some solid impurities (mainly fine carbon particles), easily causing the carbon content to exceed the standard. Therefore, installing a 400-mesh screen in the upper middle part of the carbon powder filter settler can reduce the airflow velocity of the coarse zirconium tetrachloride, which helps to reduce the amount of fine carbon particles carried. At the same time, it also acts as a physical barrier against the fine carbon particles, allowing more of them to settle.

[0036] In this embodiment, the side wall of the housing is provided with an air extraction pipe 27. The air extraction port of the air extraction pipe is located below the filter assembly, and a negative pressure back-extraction valve is provided on the air extraction pipe. The end of the air extraction pipe away from the air extraction port is connected to a jet pump (not shown in the figure). The jet pump is used to extract air from the toner filter settling device through the negative pressure back-extraction valve, so that the lower cavity of the toner filter settling device is always kept in a negative pressure state, preventing the cleaned toner from being re-adsorbed on the filter assembly, thereby ensuring the cleaning effect of the filter assembly. The hydrogen-filled iron separator includes a second housing 31. A partition plate 32 is inclined downwards and to the right at the top of the inner cavity of the second housing, dividing the upper part of the inner cavity into a left and right half-cavity. The left half-cavity has a structure that is smaller at the top and larger at the bottom, while the right half-cavity has a structure that is larger at the top and smaller at the bottom. The left half-cavity also has several baffles 33 that allow the mixed gas flow within the hydrogen-filled iron separator to form an S-shaped corridor. An inlet pipe 34 is located at the top of the left half-cavity, and a hydrogen filling pipe 37 is located on the upper side. The inlet pipe 34 is connected to the outlet of the carbon powder filter settling device. An outlet pipe 35 is located at the top of the right half-cavity, and a discharge pipe 38 is located at the bottom of the second housing. A discharge valve 38 is installed on the discharge pipe 38. The mixed gas flow is deflected and its velocity reduced within the left half-cavity by the baffles, allowing for a more complete reaction. When entering the right half-cavity, the gas flow velocity is faster in the lower part and slower in the upper expanded section, which is more conducive to the sedimentation of FeCl2.

[0037] Furthermore, the carbon powder filter settling device, the hydrogen-filled iron remover, and each stage of the cooler are all equipped with a temperature control device (not shown in the figure). The temperature control device includes a temperature sensor, a cooler, and a heater. The temperature sensor, cooler, and heater all adopt existing technology and will not be described in detail here. The temperature control device is more conducive to accurately controlling the internal temperature of each device. The outer walls of the carbon powder filter settling device, the hydrogen-filled iron remover, and each stage of the cooler are all equipped with a heat insulation layer 36, and each stage of the cooler is equipped with a collection box 37 at the bottom. A discharge pipe 38 is provided between the collection box and the corresponding cooler. The collection box is equipped with a discharge port (not shown in the figure). The upper part of the inner cavity of each condenser is also equipped with a partition plate 39 to improve the condensation effect.

[0038] In this embodiment, the condensate at the outlet of each stage of the condenser has the following contents: Fe content ≤ 0.015%, Al content ≤ 0.01%, C content ≤ 0.03%, Ti content ≤ 0.005%, and Si content ≤ 0.01%. This is basically consistent with the purity of refined zirconium tetrachloride produced by the traditional purification process, and fully meets the production requirements of refined zirconium tetrachloride.

[0039] The working principle of this invention is as follows: One of the most significant impurities in crude zirconium tetrachloride is carbon. Carbon has a boiling point of 4827°C at standard atmospheric pressure, far exceeding that of zirconium tetrachloride and other impurities. Therefore, in the gaseous crude zirconium tetrachloride product exiting the chlorination furnace, carbon is solid and relatively easy to remove. By adding a carbon powder filter settling device at the chlorination furnace outlet and controlling the chamber temperature within the filter settling device at 408°C, the high-temperature gas flow from the chlorination furnace outlet first enters the carbon powder filter settling device. The solid carbon powder particles naturally settle within the filter settling device, facilitating collection and periodic evacuation. Since zirconium tetrachloride has a boiling point of 331°C at standard atmospheric pressure, it does not undergo sublimation in the carbon powder filter settling device and can continue flowing with the gas flow to subsequent processes.

[0040] The crude zirconium tetrachloride gas stream contains iron impurities, existing in the form of FeCl3. FeCl3 has a boiling point of 316℃ at standard atmospheric pressure, lower than that of zirconium tetrachloride. Therefore, it cannot be removed by physical methods. Thus, a hydrogen-charging iron separator needs to be added after the carbon powder filter settling tank. The temperature inside the hydrogen-charging iron separator is controlled at 409.2℃, and a certain proportion of hydrogen gas is introduced into the separator (the ratio of hydrogen charging rate to the rate of fused zirconium oxide material is 0.1–3%). After the zirconium tetrachloride gas stream enters the hydrogen-charging iron separator, the FeCl3 immediately reacts with the introduced hydrogen gas, and the iron element undergoes the following chemical reaction:

[0041] FeCl3 + 1 / 2H2 → FeCl2 + HCl

[0042] After the reaction, the iron element exists in the form of FeCl2. The boiling point of FeCl2 at standard atmospheric pressure is 1023℃, which is higher than the temperature of the cavity inside the hydrogen-charged iron separator. Therefore, it sublimates into a solid and settles at the bottom slag discharge port of the hydrogen-charged iron separator, thus achieving the purpose of iron removal.

[0043] After the hydrogen-filled iron remover, the first, second, and third stage condensers are connected. The condensation temperature of each condenser is controlled to be lower than the boiling point of zirconium tetrachloride under standard atmospheric pressure (331℃), so that zirconium tetrachloride can be fully collected in the third stage condenser. The collection process is the same as the traditional process, and will not be described in detail here.

[0044] The reason for controlling the condensing temperature of each stage of the condenser to be no lower than 220±10℃ is that impurities such as aluminum and titanium mainly exist in the gas phase in the form of chlorides. The boiling point of AlCl3 under standard atmospheric pressure is 178℃, and the boiling point of TiCl4 under standard atmospheric pressure is 135-136℃. The boiling points of other impurity chlorides are also lower than 220℃. Therefore, these impurities will not be condensed in the condenser and will be discharged into the tail gas treatment device in the form of gas for tail gas treatment. The tail gas treatment device adopts the existing technology in this field, which will not be described in detail here.

[0045] Using the above method for one day of continuous production, 2428 kg of primary condensate, 770 kg of secondary condensate, and 201 kg of tertiary condensate were produced. The analysis results are as follows:

[0046]

[0047] Example 2

[0048] The only difference between this embodiment and Embodiment 1 is that the chamber temperature in the carbon powder filter settling device is controlled at 401.1℃, the chamber temperature in the gas-filled iron remover is 398.2℃, the chamber temperature in the first-stage condenser is 278.9℃, the chamber temperature in the second-stage condenser is 240.0℃, and the chamber temperature in the third-stage condenser is 220.4℃. After one day of continuous production, 2583 kg of first-stage condensate, 775 kg of second-stage condensate, and 194 kg of third-stage condensate are produced.

[0049] The results of the laboratory analysis are as follows:

[0050]

[0051] Example 3

[0052] The only difference between this embodiment and Embodiment 1 is that the chamber temperature in the carbon powder filter settling device is controlled at 390.2℃, the chamber temperature in the gas-filled iron remover is controlled at 390.6℃, the chamber temperature in the first-stage condenser is controlled at 271.5℃, the chamber temperature in the second-stage condenser is controlled at 232.1℃, and the chamber temperature in the third-stage condenser is controlled at 212.0℃. After one day of continuous production, 2674 kg of first-stage condensate, 783 kg of second-stage condensate, and 186 kg of third-stage condensate are produced.

[0053] The results of the laboratory analysis are as follows:

[0054]

[0055]

[0056] Comparative Example 1

[0057] like Figure 4 As shown, using the existing production method (omitting the purification process), continuous production for one day is carried out with the following process parameters controlled: the cavity temperature in the first-stage condenser is 281.3℃, the cavity temperature in the second-stage condenser is 242.3℃, and the cavity temperature in the third-stage condenser is 221.0℃, producing 2699kg of first-stage condensate, 831kg of second-stage condensate, and 220kg of third-stage condensate.

[0058] Analysis revealed that the Fe content did not meet the requirement of ≤0.015%, the Al content did not meet the requirement of ≤0.01%, the C content did not meet the requirement of ≤0.03%, the Ti content basically met the requirement of ≤0.005%, and the Si content did not meet the requirement of ≤0.01%. Specific analytical results are as follows:

[0059]

[0060] Therefore, it was determined that the products of Examples 1-3 were all refined zirconium tetrachloride. The product of Comparative Example 1, however, was crude zirconium tetrachloride and needed to be transferred to the purification workshop for further processing.

[0061] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for producing purified zirconium tetrachloride, characterized in that, Includes the following steps: S1. Boiling chlorination: A carbon powder filter settling device is connected to the gas outlet of the chlorination furnace, and the gas outlet of the carbon powder filter settling device is connected to a hydrogen-filled iron remover. The chamber temperature in the carbon powder filter settling device and the hydrogen-filled iron remover is controlled at 400±10℃ respectively, and hydrogen is introduced into the hydrogen-filled iron remover. The hydrogen-filled iron separator includes a housing 2. A partition plate 1 is inclined to the lower right at the top of the inner cavity of the housing 2. The partition plate 1 divides the upper part of the inner cavity of the housing 2 into a left half cavity and a right half cavity, making the left half cavity form a structure that is smaller at the top and larger at the bottom, and the right half cavity form a structure that is larger at the top and smaller at the bottom. The left half cavity is also provided with several baffles that can make the mixed airflow in the hydrogen-filled iron separator form an S-shaped corridor. The top of the left half cavity is provided with an air inlet pipe 2, and the upper side is provided with a hydrogen filling pipe. The air inlet pipe 2 is connected to the air outlet of the carbon powder filter settling device. The top of the right half cavity is provided with an air outlet pipe 2. The bottom of the housing 2 is provided with a discharge pipe 2, and the discharge pipe 2 is provided with a discharge valve 2. S2. Condensation: The outlet of the hydrogen-filled iron remover is connected in series with a primary condenser, a secondary condenser, and a tertiary condenser. The internal temperature of the primary condenser is controlled at 280±10℃, the internal temperature of the secondary condenser is 240±10℃, and the internal temperature of the tertiary condenser is 220±10℃, so that the condensate at the outlet of each condenser is refined zirconium tetrachloride.

2. The method for producing refined zirconium tetrachloride according to claim 1, characterized in that: In step S1, the raw materials for boiling chlorination are zirconium oxide, chlorine gas, and petroleum coke.

3. The method for producing refined zirconium tetrachloride according to claim 1, characterized in that: In step S1, the carbon powder filter settling device includes a housing, a filter assembly, and a backflushing assembly. The filter assembly and the backflushing assembly are both located inside the housing, with the backflushing assembly positioned above the filter assembly. The housing has an outlet pipe at the top and a discharge pipe at the bottom. The lower side has an inlet pipe connected to the outlet of the chlorination furnace. The discharge pipe has a discharge valve and the outlet pipe has an outlet valve.

4. The method for producing refined zirconium tetrachloride according to claim 3, characterized in that: The filter assembly uses a 400-mesh screen, which is located in the upper middle part of the housing.

5. The method for producing refined zirconium tetrachloride according to claim 3, characterized in that: The backflush assembly includes a backflush pipe located above the filter assembly. The backflush pipe is connected to an external compressed air source and has several backflush nozzles evenly distributed on it, facing the filter assembly.

6. The method for producing refined zirconium tetrachloride according to claim 3, characterized in that: The side wall of the housing is provided with an air extraction pipe, the air extraction port of the air extraction pipe is located below the filter assembly, and a negative pressure back-extraction valve is provided on the air extraction pipe. The end of the air extraction pipe away from the air extraction port is connected to a jet pump.

7. The method for producing refined zirconium tetrachloride according to claim 1, characterized in that: The carbon powder filter settling device, the hydrogen-filled iron remover, and each stage of the cooler are all equipped with a temperature control device, which includes a temperature sensor, a cooler, and a heater.

8. The method for producing refined zirconium tetrachloride according to claim 7, characterized in that: The outer walls of the carbon powder filter settling device, the hydrogen charging iron remover, and each stage of the cooler are all provided with a heat insulation layer, and each stage of the cooler is provided with a collection box at the bottom. A discharge pipe is provided between the collection box and the corresponding cooler. The collection box is provided with a discharge port. The upper part of the inner cavity of each condenser is also provided with a partition plate.

9. The method for producing refined zirconium tetrachloride according to any one of claims 1 to 8, characterized in that, The condensate at the outlet of each condenser has the following contents: Fe content ≤ 0.015%, Al content ≤ 0.01%, C content ≤ 0.03%, Ti content ≤ 0.005%, and Si content ≤ 0.01%.

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