JP2007197323A - Method for producing titanium tetrachloride - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing titanium tetrachloride, in which the cooling and temperature control of titanium tetrachloride gas and the drying of titanium tetrachloride slurry can be performed simultaneously and efficiently. <P>SOLUTION: The method for producing titanium tetrachloride comprises: a chlorination step of chlorinating a titanium ore in a chlorination furnace to produce titanium tetrachloride gas; a cooling step; a condensation step; and a distillation step. At the cooling step, the titanium tetrachloride gas produced in the chlorination furnace is brought into contact with liquid droplets, which are produced by spraying the titanium tetrachloride slurry consisting of solid impurities, liquid impurities and liquid titanium tetrachloride and have ≤300 μm volume median diameter, in a cooling tower positioned on the downstream side of the chlorination furnace to simultaneously perform the drying of the solid impurities in the titanium tetrachloride slurry and such a cooling operation that the outlet temperature of the titanium tetrachloride gas at the cooling step is kept within the boiling point of titanium tetrachloride to 200°C. The titanium tetrachloride gas is introduced into the cooling tower to the direction obliquely perpendicular to the circumferential direction of the cooling tower. The spray angle of the titanium tetrachloride slurry is 50-90°. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing titanium tetrachloride, and more particularly, for producing titanium tetrachloride by cooling titanium tetrachloride gas produced in a chlorination furnace, and for slurry drying of titanium tetrachloride. The present invention relates to a method for producing titanium chloride.

  Purified titanium tetrachloride is manufactured through the following manufacturing process. First, titanium tetrachloride gas is produced by reacting rutile or ilmenite, which is a titanium ore, and coke with a chlorine-containing gas in a chlorination furnace heated to around 1000 ° C.

  The titanium tetrachloride gas produced in the chlorination furnace is led to a cooling device and cooled to a predetermined temperature, and after most impurities are condensed and removed, it is cooled to below the boiling point of titanium tetrachloride in the condensation step, Liquid titanium tetrachloride is recovered. Since the recovered liquid titanium tetrachloride contains impurities such as ore and coke carried over from the chlorination furnace, or iron, aluminum, vanadium, etc., the titanium tetrachloride is referred to as crude titanium tetrachloride. Impurities dissolved or mixed in the crude titanium tetrachloride are removed in the distillation step to become purified titanium tetrachloride.

  The crude titanium tetrachloride is refined through a distillation process. In this process, titanium tetrachloride enriched with solid and liquid impurities (hereinafter sometimes referred to as “titanium tetrachloride slurry”) is distilled. Accumulated residual in. The titanium tetrachloride slurry remaining and accumulated in the distillation process has been discharged out of the system and treated with water.

  In the production of titanium tetrachloride, the titanium tetrachloride gas is cooled and the titanium tetrachloride slurry is dried in order to improve the production efficiency and to appropriately treat the titanium tetrachloride slurry produced as a by-product in the production process. Thus, a technique that can efficiently and stably perform the process has been desired.

  An object of the present invention is to provide a titanium tetrachloride production method capable of simultaneously and efficiently performing titanium tetrachloride gas cooling and temperature control and titanium tetrachloride slurry drying in the production of titanium tetrachloride. It is in.

  In the present invention, intensive studies have been made to solve the above-described problems. In the cooling step in the production of titanium tetrachloride, the titanium tetrachloride slurry and titanium tetrachloride gas generated in a chlorination furnace are brought into contact with each other, thereby bringing about The inventors have found that the drying of the titanium chloride slurry and the cooling of the titanium tetrachloride gas can be performed simultaneously, efficiently and stably, and the present invention has been completed.

  That is, according to the method for producing titanium tetrachloride according to claim 1 of the present invention, after the titanium ore is chlorinated in a chlorination furnace, the titanium tetrachloride is passed through a cooling step, a condensation step, and a distillation step. In the manufacturing method, the volume median diameter generated by spraying a titanium tetrachloride slurry composed of solid impurities, liquid impurities, and liquid titanium tetrachloride in a cooling tower of a cooling step located on the downstream side of the chlorination furnace is 300 μm or less. The droplets of titanium tetrachloride generated in the chlorination furnace are brought into contact with each other, the solid impurities in the titanium tetrachloride slurry are dried, and the outlet temperature of the cooling step of the titanium tetrachloride gas is equal to or higher than the boiling point of titanium tetrachloride. And simultaneously performing a cooling operation of 200 ° C. or less, and the titanium tetrachloride gas is introduced in a direction obliquely orthogonal to the circumferential direction of the cooling tower. The titanium tetrachloride slurry is solved that the spray angle and 50 ° to 90 °, by.

  By performing such an operation, the solid impurities and / or liquid impurities in the titanium tetrachloride slurry can be efficiently dried and the solidified impurities can be efficiently dried, and the titanium tetrachloride gas is cooled to a predetermined temperature. The impurity gas component contained in the titanium tetrachloride gas can also be selectively condensed and dried and separated and removed from the titanium tetrachloride gas.

  At this time, in the cooling step, it is preferable that the impurity component contained in the titanium tetrachloride gas is condensed and dried.

  Further, in the step of bringing the titanium tetrachloride gas into contact with the titanium tetrachloride slurry, the titanium tetrachloride gas is caused to flow vertically downward from above and sprayed with the titanium tetrachloride slurry downward from above. . In this way, by bringing the titanium tetrachloride gas and the titanium tetrachloride slurry into countercurrent contact, the titanium tetrachloride gas and the titanium tetrachloride slurry efficiently contact each other, and the titanium tetrachloride slurry is dried and the titanium tetrachloride gas is cooled. It is possible to perform sufficiently.

  Further, in the step of bringing the titanium tetrachloride gas into contact with the titanium tetrachloride slurry, the titanium tetrachloride gas is caused to flow vertically from above to below, and the titanium tetrachloride slurry is sprayed from above to below. You may make it do. In this way, by bringing the titanium tetrachloride gas and the titanium tetrachloride slurry into contact with each other in parallel, the solid matter in the titanium tetrachloride slurry and the fine solid residue deposited during the cooling of the titanium tetrachloride gas are efficiently recovered. be able to.

  Further, the titanium tetrachloride slurry can be efficiently dried by spraying the titanium tetrachloride slurry at a high pressure and bringing it into contact with the titanium tetrachloride gas.

Specifically, the spray pressure of the titanium tetrachloride slurry is that it ^{5Kg / cm 2 G~30Kg / cm 2} G.

  As described above, according to the method for producing titanium tetrachloride of the present invention, in the cooling tower, the titanium tetrachloride gas and the atomized titanium tetrachloride slurry are brought into countercurrent or cocurrent contact with each other, whereby tetrachloride is obtained. Cooling of the titanium gas and drying of the titanium tetrachloride slurry can be performed simultaneously and stably.

  Hereinafter, an embodiment of the present invention will be described with reference to the drawings. In the embodiment described below, in the present invention, titanium tetrachloride gas generated in a chlorination furnace is caused to flow vertically from below to above, while titanium tetrachloride slurry is caused to flow from above to below. It is related with the aspect which makes both counter-current contact.

  The members, arrangements, and the like described below are not intended to limit the present invention and can be variously modified within the scope of the gist of the present invention.

  1 and 2 show an embodiment of the present invention. FIG. 1 is an explanatory view showing a method for producing titanium tetrachloride according to the present invention. FIG. 2 shows an example of a production apparatus used for producing titanium tetrachloride. It is explanatory drawing shown.

  The production method of titanium tetrachloride includes a step of generating titanium tetrachloride gas in the chlorination furnace 1, a step of cooling titanium tetrachloride gas in the cooling tower 3, and the condensation of titanium tetrachloride gas in the condensation tower 7. The main steps are a step of recovering liquid titanium tetrachloride and a distillation step of purifying the liquid titanium tetrachloride to obtain purified titanium tetrachloride.

  In the cooling process, the titanium tetrachloride production method of the present example makes countercurrent contact between titanium tetrachloride gas, liquid titanium tetrachloride, and a titanium tetrachloride slurry made of a solid containing solid and liquid impurities. Thus, cooling of the titanium tetrachloride gas and drying of the titanium tetrachloride slurry can be performed simultaneously.

  In the production process of titanium tetrachloride gas, titanium ore and coke which are in a fluid state in the chlorination furnace 1 heated to about 1000 ° C. react with the chlorine gas supplied from the bottom of the chlorination furnace in fluid contact with each other. Titanium tetrachloride gas is produced. Titanium tetrachloride gas generated in the chlorination furnace 1 (including impurity gas and solid impurities, but may be simply referred to as titanium tetrachloride gas hereinafter) is guided to the cooling tower 3 via the connecting conduit 2. It is burned.

  In the cooling tower 3, a step in which the titanium tetrachloride gas and the titanium tetrachloride slurry are in countercurrent contact with each other is performed. In this step, the titanium tetrachloride gas is cooled, and at the same time, impurities contained in the titanium tetrachloride slurry are dried. .

  The titanium tetrachloride gas introduced from the chlorination furnace 1 to the cooling tower 3 is cooled to about 200 ° C. in countercurrent contact with the slurry of titanium tetrachloride sprayed from the top of the cooling tower 3. The cooled titanium tetrachloride gas is then led to the condensation tower 7.

  Further, the solid residue in the titanium tetrachloride slurry sprayed from the top of the cooling tower 3 is dried in contact with the high-temperature titanium tetrachloride gas introduced from the chlorination furnace 1 and deposited on the bottom of the cooling tower 3 by gravity. To do.

  Further, the liquid titanium tetrachloride in the titanium tetrachloride slurry is evaporated to become titanium tetrachloride gas, and is led to the condensation tower 7 together with the titanium tetrachloride gas introduced from the chlorination furnace 1.

  It is preferable that the outlet temperature of the titanium tetrachloride gas cooled in the cooling tower 3 is controlled in the range of the boiling point of titanium tetrachloride to 250 ° C. Preferably, the temperature is controlled in the range of 150 ° C to 200 ° C.

  This is because when the outlet temperature of the titanium tetrachloride gas exceeds 200 ° C., the amount of niobium or aluminum chloride contained in the titanium tetrachloride gas brought into the condensing tower 7 is increased and condensed in this process. This is because the concentration of niobium and aluminum in the recovered titanium tetrachloride is not preferable.

  In addition, if the temperature of the titanium tetrachloride gas at the outlet of the cooling tower 3 is controlled to 150 ° C. or less, the titanium tetrachloride slurry in the cooling tower 3 is not sufficiently dried, and white smoke in the case where the drying residue is treated with water. Cause the occurrence of

  For this reason, as described above, the outlet temperature of the titanium tetrachloride gas is preferably controlled so as to be in the temperature range of 150 ° C. to 200 ° C., and is preferably controlled to be as constant as possible.

  In order to control the outlet temperature of the titanium tetrachloride gas at a constant level, equipment for continuously detecting the outlet temperature of the cooling tower 3 and automatically controlling the spray amount of the titanium tetrachloride slurry supplied to the cooling tower 3 This can be achieved by using specifications.

  In order to be able to adjust the spraying amount of the titanium tetrachloride slurry, the titanium tetrachloride slurry supply device 9 may be configured, for example, as described below. Hereinafter, the titanium tetrachloride slurry supply device 9 provided in the cooling tower 3 will be described. The titanium tetrachloride slurry supply device 9 includes a supply pipe (not shown) and a spray nozzle connected to the supply pipe. Titanium tetrachloride slurry is supplied to the supply pipe from the distillation step via a pump and a transfer pipe as transfer means.

  The titanium tetrachloride slurry is sprayed from the spray nozzle of the titanium tetrachloride slurry supply device 9 toward the flow of the titanium tetrachloride gas rising in the cooling tower 3. A plurality of titanium tetrachloride slurry supply devices 9 are arranged, and the titanium tetrachloride slurry is sprayed from the spray nozzle of each titanium tetrachloride slurry supply device 9.

  Since the optimum flow rate for each spray nozzle is configured to be different from each other, the spray amount of the titanium tetrachloride slurry can be set by selecting an optimum spray nozzle according to the flow rate of the titanium tetrachloride gas guided from the chlorination furnace 1. It can adjust suitably.

  For example, at night when the amount of titanium tetrachloride gas generated is large, each titanium tetrachloride slurry supply device 9 equipped with a spray nozzle capable of supplying a large flow rate of titanium tetrachloride slurry is used, and the amount of titanium tetrachloride gas generated is In a small daytime, each titanium tetrachloride slurry supply device 9 provided with a spray nozzle for supplying a small flow rate of titanium tetrachloride slurry is selectively used.

  In addition, selection and switching of the spray nozzle are performed manually or automatically. In the case of performing automatically, for example, it is achieved by disposing a control device between the titanium tetrachloride slurry accumulation unit and each titanium tetrachloride slurry supply device 9.

  The control device is equipped with a control unit and a program for executing processing for adjusting the supply amount of the titanium tetrachloride slurry to each titanium tetrachloride slurry supply device 9 according to the outlet temperature of the titanium tetrachloride gas. And according to a program, the presence or absence of the slurry supply to each titanium tetrachloride slurry supply apparatus 9 and its supply amount are adjusted. In addition to the outlet temperature of the titanium tetrachloride gas, a spray nozzle is selected in advance according to the amount of titanium tetrachloride gas produced in the chlorination furnace 1 and a predetermined time zone, and the titanium tetrachloride slurry It is good also as a structure which adjusts supply_amount | feed_rate.

  In this way, an appropriate amount of titanium tetrachloride slurry is sprayed on the cooling tower 3 in accordance with the amount of titanium tetrachloride gas discharged from the chlorination furnace 1, cooling the titanium tetrachloride gas, and drying the titanium tetrachloride slurry. Is performed in a well-balanced manner, and the outlet temperature of the titanium tetrachloride gas is kept constant.

  In addition, if the titanium tetrachloride slurry supply device 9 which is not used is exposed to high temperature titanium tetrachloride gas in the cooling tower 3 as it is, the solid contained in the titanium tetrachloride slurry remaining in the spray nozzle or the supply pipe It is conceivable that the slurry is solidified and the spray nozzle or the supply pipe is blocked and the slurry spray cannot be resumed.

  For this reason, about the titanium tetrachloride slurry supply apparatus 9 which is not used, it is preferable to always distribute | circulate inert gas, such as nitrogen gas. Thereby, obstruction | occlusion of a spray nozzle and a supply pipe | tube can be prevented.

  Alternatively, after spraying the titanium tetrachloride slurry, purified titanium tetrachloride formed through a distillation process may be supplied in a short time to clean the spray nozzle and the supply pipe. Alternatively, a drain removing portion may be provided in the supply pipe, and the accumulated matter in the supply pipe may be periodically extracted.

  Furthermore, when the titanium tetrachloride slurry is not supplied, it is one of effective means for preventing the nozzle blockage that the titanium tetrachloride slurry supply device 9 is retracted outside the cooling tower 3. is there. In this case, a storage unit for the titanium tetrachloride slurry supply device 9 is provided, and when the titanium tetrachloride slurry is not supplied, the storage unit may be positioned.

  When retracting the titanium tetrachloride slurry supply device 9 to the storage portion, using a gate valve or a seal member, air from the outside enters the cooling tower 3 as the titanium tetrachloride slurry supply device 9 moves, Alternatively, it is preferable to prevent the titanium tetrachloride gas in the cooling tower 3 from leaking outside. Further, by taking such a configuration, the spray nozzle can be prevented from coming into contact with the high-temperature titanium tetrachloride gas, which is effective in preventing the spray nozzle from being blocked.

  Various types of spray nozzles can be used as the titanium tetrachloride slurry supply device 9. From the viewpoint of sufficiently drying the titanium tetrachloride slurry, fine droplets can be obtained as much as possible and clogging is possible. It is desirable to select an appropriate spray nozzle.

  In addition, it is preferable to select a spray nozzle having a characteristic that the particle size of the spray droplets hardly changes regardless of the supply amount of the titanium tetrachloride slurry. Furthermore, the spray nozzle which can ensure the high flow volume with the droplet of the sprayed titanium tetrachloride slurry being a fine particle is preferable.

  The titanium tetrachloride slurry collides with the inner wall of the cooling tower 3 by configuring the spray angle of the titanium tetrachloride slurry sprayed from the spray nozzle to be 30 ° to 100 °, preferably 50 ° to 90 °. This is suitable for preventing the solid matter from adhering to the inner surface of the cooling tower.

  From the viewpoint of sufficiently drying the titanium tetrachloride slurry droplets sprayed from the top of the cooling tower 3, it is preferable to increase the specific surface area and increase the contact area with the high temperature gas. . Specifically, the volume median diameter is preferably 400 μm or less, more preferably 300 μm or less. However, if an excessively fine droplet is to be generated, it is necessary to reduce the diameter of the spray nozzle, and as a result, the nozzle may be blocked. Therefore, it is better to select a nozzle with a lower limit of about several tens of μm. Realistic. As the spray nozzle, a general spray nozzle for spray drying can be used. However, since a solid slurry is used as a spray medium, it is preferable to select a material having wear resistance.

In order to spray the slurry of fine droplets described above, it is also important to select an appropriate back pressure in addition to reducing the diameter of the spray nozzle. In the present invention, it is preferable that the back pressure and ^{5Kg / cm 2 G~30Kg / cm 2} G or so. By selecting such a back pressure, the fine titanium tetrachloride slurry droplets as described above can be generated.

  On the other hand, while the titanium tetrachloride gas introduced from the chlorination furnace 1 to the cooling tower 3 is cooled, chloride gas components such as iron, aluminum, niobium and manganese contained in the titanium tetrachloride gas are condensed and dried. And settles at the bottom of the cooling tower 3. In addition, fine powders such as ore and coke contained in the titanium tetrachloride gas discharged from the chlorination furnace 1 are simultaneously separated and settled.

  The dry residue deposited on the bottom of the cooling tower 3 is extracted out of the system and then subjected to water treatment in the solid residue treatment facility 8. The dry residue is intermittently extracted out of the system by a powder cutting device (not shown) installed at the bottom of the cooling tower 3.

  When introducing the titanium tetrachloride gas into the cooling tower 3, the titanium tetrachloride gas is introduced in a direction obliquely orthogonal to the circumference of the cooling tower 3 to form a swirling upward flow in the cooling tower 3. You may do it.

  As described above, the titanium tetrachloride gas is swirled and raised, and when the titanium tetrachloride slurry is sprayed, the titanium tetrachloride gas and the liquid titanium tetrachloride slurry can be more uniformly heat exchanged. The cooling of the gas and the drying of the titanium tetrachloride slurry can be suitably performed simultaneously.

  Further, by forming such a swirl flow, it is possible to suppress the residue in the titanium tetrachloride gas from being fixedly grown on the inner wall of the cooling tower 3.

  In order to cool the titanium tetrachloride gas more efficiently, a jacket is provided around the cooling tower 3 and a cooling gas is allowed to flow there, and the outer wall temperature is maintained at 200 ° C. to 400 ° C. Cooling from the surroundings may be promoted.

  The titanium tetrachloride gas from which the impurity component has been removed in the cooling tower 3 is guided to the condensation tower 7 and cooled to the boiling point of titanium tetrachloride or less to recover liquid titanium tetrachloride. The liquid titanium tetrachloride may be called crude titanium tetrachloride because it contains some solid impurities or liquid impurities.

  Cooled liquid titanium tetrachloride is sprayed from the top of the condensation tower 7. The titanium tetrachloride gas introduced into the condensing tower 7 is brought into contact with the cooled liquid titanium tetrachloride and subjected to heat exchange to obtain liquid crude titanium tetrachloride.

  In the condensation tower 7, liquid titanium tetrachloride is sprayed as described above, and the titanium tetrachloride gas is cooled by providing a water cooling jacket or the like. The crude titanium tetrachloride condensed in the condensation tower 7 is sent to the distillation process. The remaining gas from which the titanium tetrachloride gas has been condensed and removed in the condensing tower 7 is guided to an exhaust gas treatment facility for processing.

  The crude titanium tetrachloride sent to the distillation step is passed through a rectification tower (not shown) to remove impurities and become purified titanium tetrachloride. On the other hand, impurities separated during purification are by-produced in the form of titanium tetrachloride slurry. This titanium tetrachloride slurry is returned to the cooling tower 3 and spray-dried as described above.

  Note that a gas cyclone 5 can be interposed between the cooling tower 3 and the condensation tower 7 via conduits 4 and 6. By providing the gas cyclone 5, it becomes possible to effectively remove solids and impurities contained in the titanium tetrachloride gas discharged from the cooling tower 3.

  That is, while the titanium tetrachloride gas generated in the chlorination furnace 1 passes through the cooling tower 3, most of solids and impurities precipitated during cooling are settled and separated. However, since the titanium tetrachloride gas flows in the cooling tower 3 from below to above, when the resistance of the titanium tetrachloride gas flow is larger than the gravity, the deposited impurities do not settle and the cooling tower 3 To the condensing tower 7 downstream.

  The fine particle residue brought into the condensing tower 7 is led to a distillation step as crude titanium tetrachloride together with liquefied titanium tetrachloride, and purified. In the distillation step, the fine particle residue is separated as titanium tetrachloride slurry, so that if the amount of fine particle residue brought into the condensing tower 7 increases, the amount of titanium tetrachloride slurry dried in the cooling tower 3 also increases. become. For this reason, before entering the condensing tower 7, it is preferable to discharge the fine particle residue out of the system as much as possible.

  Inserting the gas cyclone 5 between the cooling tower 3 and the condensing tower 7 is effective in separating and removing the fine particle residue contained in the titanium tetrachloride gas discharged from the cooling tower 3. Since the amount of residue circulating in the interior can be reduced, this provides a favorable situation where the amount of titanium tetrachloride slurry to be treated can also be reduced.

  In addition, when the treatment of titanium tetrachloride slurry becomes a problem as compared with the temperature control of titanium tetrachloride gas due to variations in the type of ore and the process, the titanium tetrachloride gas generated in the chlorination furnace 1 is supplied to the cooling tower 3. It is preferable to flow from the top to the bottom, and also to flow the titanium tetrachloride slurry from the top to the bottom, and to bring both into contact with each other.

  That is, by bringing the high temperature titanium tetrachloride gas and the titanium tetrachloride slurry into contact with each other in parallel, the solid matter in the titanium tetrachloride slurry and the fine solid residue precipitated during the cooling of the titanium tetrachloride gas are 3 can be efficiently recovered at the bottom. Therefore, the escape of the fine particle residue to the condensation tower 7 located downstream of the cooling tower 3 can be suppressed, and the amount of the residue remaining in the system can also be suppressed.

Titanium tetrachloride was produced by the production method of the present invention.
15,000 L / min of chlorine gas was supplied to the chlorination furnace, and the titanium tetrachloride slurry was sprayed from the top of the cooling tower in the cooling step. The spray amount of the titanium tetrachloride slurry was automatically controlled so that the outlet temperature of the cooling tower became constant at around 200 ° C.

  As a result, it was possible to control the target temperature within a range of ± 10 ° C. Further, the residue collected at the bottom of the cooling tower was in a dry state, and white smoke was hardly generated during water treatment.

It is explanatory drawing which shows the manufacturing method of the titanium tetrachloride of this invention. It is explanatory drawing which shows an example of the manufacturing apparatus used for manufacture of titanium tetrachloride.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Chlorination furnace 2 Connection pipe | tube 3 Cooling tower 4 Pipe | tube 5 Gas cyclone 6 Pipe | tube 7 Condensing tower 8 Solid residue processing equipment 9 Titanium tetrachloride slurry supply apparatus S Titanium tetrachloride manufacturing apparatus

Claims (6)

In a method for producing titanium tetrachloride through chlorination of titanium ore in a chlorination furnace, followed by a cooling step, a condensation step, and a distillation step,
In the cooling tower of the cooling step located on the downstream side of the chlorination furnace, a droplet having a volume median diameter of 300 μm or less generated by spraying a titanium tetrachloride slurry comprising solid impurities, liquid impurities, and liquid titanium tetrachloride; Titanium tetrachloride gas generated in a chlorination furnace is contacted, the solid impurities in the titanium tetrachloride slurry are dried, and the outlet temperature of the cooling step of the titanium tetrachloride gas is equal to or higher than the boiling point of titanium tetrachloride and 200 ° C. The titanium tetrachloride gas is introduced in a direction obliquely orthogonal to the circumferential direction of the cooling tower, and the titanium tetrachloride slurry has a spray angle of 50. A method for producing titanium tetrachloride, characterized in that the angle is set to ° to 90 °.   The method for producing titanium tetrachloride according to claim 1, wherein in the cooling step, the impurity component contained in the titanium tetrachloride gas is condensed and dried.   In the step of bringing the titanium tetrachloride gas into contact with the titanium tetrachloride slurry, the titanium tetrachloride gas is allowed to flow vertically downward from above, and the titanium tetrachloride slurry is sprayed downward from above. The method for producing titanium tetrachloride according to claim 1.   In the step of bringing the titanium tetrachloride gas into contact with the titanium tetrachloride slurry, the titanium tetrachloride gas is allowed to flow downward from the vertical direction, and the titanium tetrachloride slurry is sprayed downward from above. The method for producing titanium tetrachloride according to claim 1.   The method for producing titanium tetrachloride according to any one of claims 1 to 4, wherein the titanium tetrachloride slurry is sprayed at a high pressure and brought into contact with the titanium tetrachloride gas. The four manufacturing method of titanium tetrachloride of claims 1 to 5, wherein any spraying pressure of titanium chloride slurry, characterized in that a ^{5Kg / cm 2 G~30Kg / cm 2} G.

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