JP5658202B2 - Titanium tetrachloride production facility maintenance method and titanium tetrachloride production facility - Google Patents

Description

The present invention relates to a method and TiCl ₄ production facilities to develop a TiCl ₄ production facility to pure TiCl ₄ by distillation of crude TiCl ₄ (titanium tetrachloride) obtained by the fluidized bed, and more particularly, devices included in the production facility TiCl ₄ production facility maintenance method and TiCl ₄ which can discharge most of TiCl ₄ existing in the interior of the machine and reduce deterioration of working environment and corrosion of equipment due to generation of hydrochloric acid gas when maintenance is performed open to the atmosphere. It relates to manufacturing equipment.

Pure TiCl ₄ (pure titanium tetrachloride), which is a raw material for producing metal Ti, is usually produced from crude TiCl ₄ (crude titanium tetrachloride) produced by a fluid chlorination method. Hereinafter, “crude TiCl ₄ ” and “pure TiCl ₄ ” are also collectively referred to as “TiCl ₄ ”.

In the fluidized chlorination method, ore containing titanium oxide as a titanium source, coke is used as a reducing agent, and fluidized bed in which chlorine gas is blown from below into a layer formed in the fluidized furnace by ore and coke. The chlorination reaction proceeds to produce crude TiCl ₄ gas. The crude TiCl ₄ gas generated by the fluidized chlorination method contains oxides such as iron, aluminum, and zirconium as impurities in ores containing titanium oxide, and these oxides are chlorinated. Chloride is included as an impurity.

In the production of pure TiCl ₄ , after the crude TiCl ₄ gas obtained by the fluidized chlorination method is cooled and liquefied, pure TiCl ₄ is obtained by reducing impurities in the crude TiCl ₄ liquid in a distillation step. The distillation step can be performed, for example, by performing rectification after simple distillation. In the rectification, the purity of TiCl ₄ is removed by removing impurities in the crude TiCl ₄ liquid using a multistage distillation column or a packed column. Pure TiCl ₄ with increased

As described above, since ore containing titanium oxide contains oxides such as iron, aluminum, and zirconium as impurities, the crude TiCl ₄ gas and the crude TiCl ₄ liquid contain impurities containing chlorinated oxides as impurities. Included as Since some of the chloride contained as impurities is contained as solid particles, it grows by adhering to equipment such as heat exchangers, tanks, and piping provided in the TiCl ₄ production facility to form a scale.

For example, when a scale is formed in a heat exchanger, the heat conductivity of the scale is lower than that of the heat exchanger member, so that heating or cooling is insufficient and the heat exchange capacity of the heat exchanger is reduced. . Further, when a scale is formed by piping, an increase in pressure loss and piping blockage due to scale growth occur. As a result, energy efficiency and productivity are significantly reduced in the TiCl ₄ production facility.

To prevent energy efficiency and productivity degradation, TiCl ₄ manufacture periodically removes the scale that is formed by performing maintenance work on equipment such as heat exchangers, tanks, and piping provided in the manufacturing facility. There is a need. Conventionally, in maintenance work, after the TiCl ₄ liquid (crude TiCl ₄ or pure TiCl ₄ ) present in the equipment provided in the TiCl ₄ manufacturing facility is discharged from the equipment, the work is removed by releasing the air to the atmosphere. It was maintained by. In this case, a part of the TiCl ₄ liquid present inside the device inevitably remains inside the device without being discharged due to the device structure and operational reasons. For this reason, it was maintained by opening to the atmosphere with the TiCl ₄ liquid remaining inside the device.

In the conventional maintenance method, the TiCl ₄ liquid remaining along with the scale to be removed was discarded, but the ore and coke that are the raw materials of TiCl ₄ are expensive because they are obtained by performing a plurality of treatments, It is very uneconomical to dispose of TiCl ₄ liquid obtained from expensive raw materials. Also, when the device is opened to the atmosphere, the air flows into the device, but the moisture contained in the flowing air and the TiCl ₄ liquid remaining in the device cause the reaction shown in the following formula (1), and hydrochloric acid gas (HCl) Produce.
TiCl ₄ + 2H ₂ O → TiO ₂ + 4HCl (1)

The hydrochloric acid gas generated by the reaction shown in the above formula (1) is not only very harmful to the human body, but also causes corrosion of peripheral equipment of the TiCl ₄ manufacturing facility. For this reason, in the conventional maintenance method, the deterioration of the working environment and the corrosion of the equipment have been problems.

Various proposals have conventionally been made regarding a scale formed by equipment provided in a TiCl ₄ manufacturing facility. For example, Patent Document 1 is available. Patent Document 1, among the devices TiCl ₄ production facility is provided, is used crude TiCl ₄ liquid stored in the provided tank for temporarily storing the crude TiCl ₄ liquid level gauge and the tank in the distillation step The purpose of this is to prevent malfunctions caused by scale formation in pumps that are transported to equipment. Patent Document 1 proposes a method of preventing a scale from being formed by supplying a pure TiCl ₄ solution continuously or intermittently to a portion where a scale is formed and malfunction occurs.

When the scale formation prevention method proposed in Patent Document 1 is used, scales can be prevented from being formed in portions where pure TiCl ₄ liquid is continuously or intermittently supplied, but scales are not formed in other portions. It is formed. Accordingly, even when the scale formation prevention method proposed in Patent Document 1 is used, it is necessary to periodically perform maintenance work to remove the scale formed. The maintenance work performed to remove this scale is not studied in Patent Document 1.

JP 2006-55740 A

As described above, the crude TiCl ₄ gas obtained by fluidized bed and cooled crude TiCl ₄ liquid in TiCl ₄ production facilities to pure TiCl ₄ liquid crude TiCl ₄ liquid in distillation step, performed maintenance work Thus, it is necessary to remove the scale formed. In the conventional maintenance method, the TiCl ₄ liquid existing in the equipment included in the TiCl ₄ manufacturing facility is discharged from the equipment by a liquid feed pump and then opened to the atmosphere. In this case, a part of the TiCl ₄ liquid present inside the device inevitably remains inside the device without being discharged due to the device structure and operational reasons.

The conventional maintenance method is uneconomical because the TiCl ₄ liquid remaining inside the equipment together with the scale is discarded, and the TiCl ₄ liquid remaining inside the equipment reacts with the moisture in the atmosphere that flows in by opening to the atmosphere. Since hydrochloric acid gas is generated, the working environment is deteriorated and the equipment is corroded.

The present invention has been made in view of such a situation, and it is possible to discharge most of TiCl ₄ present in the equipment, and the working environment is deteriorated due to generation of hydrochloric acid gas when maintenance is performed open to the atmosphere. and it has an object to provide a servicing method and TiCl ₄ production facilities TiCl ₄ production facility capable of reducing the corrosion of the equipment.

The present inventors examined a method of discharging the TiCl ₄ liquid present in the device without remaining in the device. As this method, a discharge port is provided at the bottom of the device to be maintained and the lower part of the side surface, and TiCl ₄ discharged from the discharge port is sent using a liquid supply pump such as a vortex pump. A method of sucking the TiCl ₄ liquid and discharging it from the discharge port is conceivable.

Here, when discharging the TiCl ₄ solution present inside device from the discharge port smoothly the TiCl ₄ liquid to be discharged from the outlet while flowing gas therein apparatus for performing discharge. As the gas flowing into the apparatus, when moisture is contained, hydrochloric acid gas is generated by the reaction shown in the above formula (1), and therefore dry air or inert gas is used. In addition, a part of the TiCl ₄ liquid present inside the device evaporates into a gas. For this reason, gas exists with the TiCl ₄ liquid inside the device.

When the TiCl ₄ liquid and the gas are present inside the device, if the TiCl ₄ liquid existing inside the device is sucked and discharged by the liquid feed pump, the liquid feed pump will eventually release the gas together with the TiCl ₄ liquid. Inhale. Since the suction force of the liquid delivery pump is significantly reduced when the gas is sucked in, the TiCl ₄ liquid remains in the apparatus even in the method of suction using the liquid delivery pump. For this reason, when maintenance is performed with the atmosphere open, deterioration of the working environment and corrosion of the equipment become a problem due to the hydrochloric acid gas generated by the reaction of the remaining TiCl ₄ liquid with moisture contained in the atmosphere.

The present inventors conducted various tests on the method of discharging TiCl ₄ remaining inside the device, and as a result of intensive studies, as a result of sucking the TiCl ₄ liquid existing inside the device from the discharge port under reduced pressure. It has been found that the remaining TiCl ₄ without being discharged can be greatly reduced, and the deterioration of the working environment and the corrosion of the equipment due to hydrochloric acid gas can be reduced.

In addition, the TiCl ₄ liquid suctioned under reduced pressure from the discharge port is collected in a TiCl ₄ liquid recovery container and separated into gas and liquid, and the liquid in the TiCl ₄ liquid recovery container is extracted and returned to the middle of the TiCl ₄ production facility. It was found that the recovered TiCl ₄ solution can be effectively used.

When the heat exchanger provided in the TiCl ₄ manufacturing facility is equipped with a heat exchanger that heats or cools the crude TiCl ₄ liquid, TiCl ₄ existing in the heat exchanger can be greatly reduced by vacuum suction. However, because of the structure of the heat exchanger and because the crude TiCl ₄ liquid is in the form of a slurry because some of the impurities are contained as solid particles, the crude TiCl ₄ liquid tends to adhere to the heat exchanger and remain. In this case, the crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the heat exchanger, and the TiCl ₄ liquid adhering to the heat exchanger is vaporized by heating the heat exchanger, and is sucked under reduced pressure as a gas. _{It has been found that if the 4} gases are liquefied by a cooler and recovered in a TiCl ₄ liquid recovery container, all of the TiCl ₄ liquid existing in the heat exchanger can be recovered.

The present invention has been completed on the basis of the above-mentioned findings, and the gist of the present invention is the following (1) to ( 2 ) TiCl ₄ production facility maintenance method and the following ( 3 ) TiCl ₄ production facility.

(1) A method for preparing a TiCl ₄ production facility in which a crude TiCl ₄ gas obtained by a fluidized bed is cooled to obtain a crude TiCl ₄ liquid, and this crude TiCl ₄ liquid is converted into a pure TiCl ₄ liquid in a distillation step. Among the equipment provided in the TiCl ₄ manufacturing facility, when the TiCl ₄ liquid is vacuumed and sucked from the outlet of the equipment targeted for maintenance and then released to the atmosphere, the TiCl ₄ liquid is vacuum suctioned from the outlet of the equipment to be repaired. The TiCl ₄ liquid recovery container is evacuated by evacuating the gas in the TiCl ₄ liquid recovery container, and the TiCl ₄ liquid recovery container is connected to the maintenance target device to thereby remove the TiCl ₄ liquid in the maintenance target device. upon vacuum suction, the suction recovered TiCl ₄ solution was gas-liquid separation in the TiCl ₄ liquid collecting container, which vacuum suction of TiCl ₄ liquid from the discharge port of the serviced device, TiCl ₄ The maintenance crude TiCl ₄ liquid from the discharge port of the heat exchanger is a target device forming equipment comprises as well as vacuum suction, is vaporized TiCl ₄ liquid adhering to the heat exchanger by heating said heat exchanger, and wherein the vacuum sucked as gas, recovered in the TiCl ₄ liquid collecting container to liquefy the TiCl ₄ gas with the installed condenser between the outlet of the serviced device to said TiCl ₄ liquid collecting container To maintain TiCl ₄ production facility.

(2) extracting the liquid in the TiCl ₄ liquid collecting container, TiCl according to (1) to by returning to the middle of TiCl ₄ production facilities, characterized by effectively using suction recovered TiCl ₄ solution ₄ How to maintain production equipment.

(3) a flow reactor to produce a by forming a fluidized layer crude TiCl ₄ gas, the cooling equipment crude TiCl ₄ gas and cooled crude TiCl ₄ liquid, pure by increasing the purity of the crude TiCl ₄ liquid a TiCl ₄ production facility and a distillation equipment to TiCl ₄ solution, there is TiCl ₄ production facilities reduced pressure TiCl ₄ liquid in a device comprising the attractable outlet, a TiCl ₄ liquid is sucked from the discharge port There are TiCl ₄ liquid collecting container for collecting, Chi lifting the this TiCl ₄ liquid collecting container pressure reducing function, the maintenance target apparatus is a heat exchanger in which the TiCl ₄ production facility is provided, the TiCl ₄ production facilities, the When the crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the heat exchanger, the heat exchanger is heated to vaporize the TiCl ₄ liquid adhering to the heat exchanger, and from the outlet of the maintenance target equipment Ti installed until l ₄ liquid collecting container, a cooler for liquefying the TiCl ₄ gas, and configured cooler as liquefied TiCl ₄ gas is collected in the TiCl ₄ liquid collecting container, A TiCl ₄ production facility further comprising:

In the maintenance method of the TiCl ₄ production facility of the present invention, most of the TiCl ₄ liquid existing in the apparatus can be discharged by sucking the TiCl ₄ liquid under reduced pressure from the discharge port of the apparatus. For this reason, when maintaining with the atmosphere open, the amount of hydrochloric acid gas generated by the remaining TiCl ₄ liquid reacting with the moisture contained in the atmosphere can be suppressed. Corrosion can be reduced.

TiCl ₄ production equipment of the present invention, there is TiCl ₄ liquid collecting container for collecting the TiCl ₄ solution, by which this TiCl ₄ liquid collecting container having a pressure reducing function, exhaust equipment was serviced when servicing the equipment The TiCl ₄ liquid can be easily recovered from the outlet by vacuum suction.

A configuration example of a TiCl ₄ production equipment of the present invention is a schematic diagram showing.

First, the basic configuration of TiCl ₄ production facility, with reference to the drawings showing a configuration example of a TiCl ₄ production equipment of the present invention will be described.

FIG. 1 is a schematic diagram showing a configuration example of the TiCl ₄ production facility of the present invention. TiCl ₄ production equipment shown in Figure 1, the flow reactor 10 to generate by forming a fluidized layer crude TiCl ₄ gas, cooling equipment and the resulting crude TiCl ₄ gas and cooled crude TiCl ₄ liquid (crude TiCl ₄ (Gas cooler) 20 and a distillation facility 30 for increasing the purity of the crude TiCl ₄ liquid to form a pure TiCl ₄ liquid. Further, in the figure, a pipe for sending crude TiCl ₄ or pure TiCl ₄ in the direction indicated by the arrow is indicated by a solid arrow.

The fluidized furnace 10 causes a chlorination reaction to proceed in a fluidized bed in which chlorine gas is blown from below into a layer formed in the fluidized furnace with ore and coke to generate crude TiCl ₄ gas. In the TiCl ₄ production facility shown in the figure, the crude TiCl ₄ gas generated in the fluidized furnace 10 is sent to the cyclone 11 and solids are removed, and then a cooling facility (crude TiCl ₄ gas cooler) that is a heat exchanger. ) 20 to cool to a crude TiCl ₄ solution. The obtained crude TiCl ₄ liquid is sent to a crude TiCl ₄ liquid tank and stored.

In the TiCl ₄ production facility shown in the figure, the crude TiCl ₄ solution is rectified after being simply distilled by the distillation facility 30 to become a pure TiCl ₄ solution. The distillation facility 30 includes an evaporator 31 and a simple distillation cooler 33 for simple distillation of the crude TiCl ₄ liquid sent from the crude TiCl ₄ liquid tank 21, and distillation for rectifying the simple distilled crude TiCl ₄ liquid. A tower 34 and a rectification cooler 37 are included. Further, the evaporator 31 is provided with an evaporator heater 32, and heats the crude TiCl ₄ liquid by circulating it through the evaporator heater 32.

In the distillation equipment 30 having such a configuration, crude TiCl ₄ liquid sent to the evaporator 31 from the crude TiCl ₄ liquid tank 21 is heated gasified in the evaporator 31. The crude TiCl ₄ gas gasified by the evaporator 31 is liquefied by the simple distillation cooler 33, whereby the crude TiCl ₄ liquid is simply distilled. At this time, high boiling point substances among impurities contained in the crude TiCl ₄ liquid remain in the evaporator 31 without being gasified, so that the purity of the crude TiCl ₄ liquid can be increased by simple distillation.

In the distillation column 34, the crude TiCl ₄ liquid that has been subjected to simple distillation is circulated to the distillation column heater 35 at the bottom of the column to be heated and evaporated. The crude TiCl ₄ gas generated at the bottom of the tower rises while lowering the temperature in the tower, and a part of the crude TiCl ₄ gas is taken out as pure TiCl ₄ gas from the side cut provided between the top and bottom of the distillation tower. The pure TiCl ₄ gas taken out from the side cut is sent to the rectifying cooler 37 to be cooled to become a pure TiCl ₄ liquid.

On the other hand, when the crude TiCl ₄ gas generated at the bottom of the column rises and reaches the top column without being removed from the side cut, it is extracted from the distillation column 34. The crude TiCl ₄ gas extracted at the top tower is cooled by the tower top cooler 36 to obtain a crude TiCl ₄ liquid, and then returned to the distillation tower 34. In such a distillation column 34, the high-boiling substances remaining in the simple distilled crude TiCl ₄ liquid remain in the bottom of the distillation column 34 without being gasified, so that pure TiCl ₄ gas from which impurities have been removed is removed. Can be removed from the side cut.

Evaporator heater 32 and the distillation column for the heater 35 shown in the figure is a heat exchanger, together with the crude TiCl ₄ liquid is supplied high-temperature steam, the crude TiCl ₄ liquid by high-temperature steam and heat exchanger Heat. The crude TiCl ₄ gas cooler 20, the simple distillation cooler 33, the tower top cooler 36, and the rectification cooler 37 are also heat exchangers, but in the cooler, together with the crude TiCl ₄ gas or pure TiCl ₄ gas. Cooling water is supplied, and cooling is performed by heat-exchanging high-temperature crude TiCl ₄ gas or pure TiCl ₄ gas with cooling water.

With reference to the TiCl ₄ manufacturing facility shown in FIG. 1 which has such a basic configuration, a method for maintaining the TiCl ₄ manufacturing facility of the present invention will be described below.

Maintenance method of TiCl ₄ production equipment of the present invention, the as TiCl ₄ production equipment shown in Figure 1, the crude TiCl ₄ gas obtained by fluidized bed and cooled crude TiCl ₄ liquid, crude TiCl ₄ liquid Is a method of preparing a TiCl ₄ production facility in which a pure TiCl ₄ solution is obtained in a distillation process, after the TiCl ₄ solution is suctioned from the outlet of the device 50 to be maintained among the devices provided in the TiCl ₄ production facility under reduced pressure. It is characterized by opening to the atmosphere and maintaining.

In FIG. 1, since the maintenance target device 50 is separated from the production line, piping for connecting the maintenance target device 50 and the TiCl ₄ manufacturing facility is omitted. In the maintenance method of the TiCl ₄ manufacturing facility of the present invention, the maintenance target device 50 can be a device through which a crude TiCl ₄ liquid or gas or a pure TiCl ₄ liquid or gas passes. For example, a heater, a cooler, or a tank 21 is used. The evaporator 31 can be a pipe connecting them. Further, the TiCl ₄ liquid sucked under reduced pressure may be either a crude TiCl ₄ liquid or a pure TiCl ₄ liquid.

As described above, when sucking the TiCl ₄ liquid from the discharge port of the device with a liquid feed pump, from the liquid feed pump is reduced significantly and the suction force sucks gas, TiCl ₄ liquid inside equipment Remains. On the other hand, development method TiCl ₄ production equipment of the present invention, by vacuum suction, even when the gas is mixed into the TiCl ₄ solution discharged from the outlet of the device, the TiCl ₄ solution while maintaining the suction force Can be aspirated.

For this reason, the maintenance method for the TiCl ₄ production facility of the present invention can discharge most of the TiCl ₄ liquid existing in the equipment. As a result, it is possible to greatly reduce the amount of TiCl ₄ liquid that is discarded together with the scale when being opened to the atmosphere. In addition, the amount of hydrochloric acid gas generated when the remaining TiCl ₄ liquid reacts with moisture contained in the atmosphere can be suppressed, and deterioration of the working environment and corrosion of equipment due to the hydrochloric acid gas can be reduced.

In particular, when the maintenance target device 50 is not a heat exchanger such as a heater or a cooler, but a device such as a tank 21, an evaporator 31, and a pipe connecting them, all TiCl ₄ liquid existing in the device is discharged. it can. In this case, when maintenance is performed with the atmosphere open, the generation of hydrochloric acid gas due to the reaction of the remaining TiCl ₄ liquid with moisture contained in the atmosphere can be completely suppressed, and the working environment is deteriorated by the hydrochloric acid gas. And corrosion of equipment can be prevented.

Since the TiCl ₄ liquid existing inside the device accumulates in the lower part of the device due to gravity, the maintenance target device 50 outlet may be provided at the bottom of the device or the lower part of the side surface.

The method of maintaining the TiCl ₄ production facility of the present invention is such that when the TiCl ₄ liquid is sucked under reduced pressure from the outlet of the maintenance target device 50, the gas in the TiCl ₄ liquid recovery container 40 is exhausted to exhaust the TiCl ₄ liquid recovery container 40. The TiCl ₄ liquid recovery container is connected to the maintenance target device 50 to reduce the pressure of the TiCl ₄ liquid in the maintenance target device 50, and the suctioned and recovered TiCl ₄ liquid is stored in the TiCl ₄ liquid recovery container 40. you gas-liquid separation.

The TiCl ₄ production facility shown in FIG. 1 has a TiCl ₄ liquid recovery container 40, and this TiCl ₄ liquid recovery container 40 has a decompression pump 41 that exhausts the gas in the recovery container. In addition, the TiCl ₄ manufacturing facility includes a pipe for sending the crude TiCl ₄ liquid discharged from the outlet of the maintenance target device 50 to the TiCl ₄ liquid recovery container 40.

In such a TiCl ₄ production facility, the inside of the TiCl ₄ liquid recovery container 40 is depressurized by evacuating the gas in the TiCl ₄ liquid recovery container 40 by the pressure reducing pump 41. In this state, the TiCl ₄ liquid recovery container is connected to the maintenance target device 50, whereby the TiCl ₄ liquid in the evaporator heater 32 is sucked under reduced pressure and recovered in the TiCl ₄ liquid recovery container 40. As described above, by using the TiCl ₄ liquid recovery container 40, the TiCl ₄ liquid existing in the apparatus can be discharged and recovered by vacuum suction.

Further, when the TiCl ₄ liquid recovered together with the gas by suction under reduced pressure is held in the TiCl ₄ liquid recovery container 40, the bubbles in the TiCl ₄ liquid rise and reach the liquid surface, so that from the recovered TiCl ₄ liquid The gas can be separated. Even when the TiCl ₄ liquid is a crude TiCl ₄ liquid in a slurry state, the TiCl ₄ liquid can be similarly recovered by sucking under reduced pressure using the TiCl ₄ liquid recovery container 40 and held in the TiCl ₄ liquid recovery container 40 for gas-liquid separation. can do.

In the maintenance method of the TiCl ₄ production facility of the present invention, it is preferable to effectively utilize the suctioned and recovered TiCl ₄ solution by extracting the liquid in the TiCl ₄ solution recovery container and returning it to the middle of the TiCl ₄ production facility. Thus, it is possible to improve the material yield in the TiCl ₄ production.

To return to the middle of TiCl ₄ production facilities, from the viewpoint of preventing a deterioration in the quality of the pure TiCl ₄ liquid prepared, TiCl ₄ liquid sucked recovered if crude TiCl ₄ liquid, the stage before being simple distillation It is preferable to return. In the TiCl ₄ production facility shown in FIG. 1, when equipment from the equipment (pipe connecting the fluid furnace 10 and the cyclone 11) arranged downstream from the fluid furnace 10 to the distillation column 34 is maintained, the equipment is sucked under reduced pressure from the equipment. It is preferable that the TiCl ₄ liquid becomes a crude TiCl ₄ liquid, and the collected rough TiCl ₄ liquid is returned to a position before the evaporator 31.

On the other hand, if the TiCl ₄ liquid collected by suction is pure TiCl ₄ liquid, it is preferable to return to the stage before rectification from the viewpoint of preventing the quality of the produced pure TiCl ₄ liquid from being reduced. It is more preferable to return to the previous stage. The TiCl ₄ production equipment shown in FIG. 1, to develop a device which is disposed downstream from the distillation column 34, the TiCl ₄ solution is vacuum suction from the apparatus, a net TiCl ₄ solution, pure TiCl ₄ which is sucked and recovered The liquid is preferably returned to a position before the distillation column 34, and more preferably returned to a position before the evaporator 31.

When the crude TiCl ₄ liquid is recovered by vacuum suction and stored in the TiCl ₄ liquid recovery container, impurities contained as solid particles in the crude TiCl ₄ liquid adhere to and accumulate on the bottom of the TiCl ₄ liquid recovery container and are provided at the bottom. There is a concern of obstructing the extraction of the crude TiCl ₄ liquid by closing the outlet.

For this reason, in the maintenance method of the TiCl ₄ production facility of the present invention, when the crude TiCl ₄ liquid is sucked under reduced pressure when the TiCl ₄ liquid is sucked under reduced pressure from the outlet of the maintenance target device 50, the TiCl ₄ liquid recovery container is stirred. It is preferable to use a TiCl ₄ liquid recovery container having a function. As a result, it is possible to prevent the impurities contained in the recovered crude TiCl ₄ liquid from adhering to and depositing on the bottom of the TiCl ₄ liquid recovery container and block the discharge port to inhibit the extraction of the crude TiCl ₄ liquid. Can dispel concerns.

The stirring function of the TiCl ₄ liquid recovery container can be realized by bubbling for blowing a gas into the crude TiCl ₄ liquid in the recovery container or by mechanical stirring that rotates a stirrer in the recovery container. Since the slurry-like crude TiCl ₄ liquid is inferior in fluidity, it is preferable to employ mechanical stirring. As shown in FIG. 1, the rotating blade 40a rotating along the horizontal plane is used as a stirring bar. It is more preferable to employ mechanical agitation in which 40a is disposed in the vicinity of the bottom surface of the collection container. This is because by arranging the rotary blade 40a rotating along the horizontal plane in the vicinity of the bottom surface of the collection container, the impurities attached to the bottom surface can be efficiently reflowed.

Here, a heat exchanger such as a heater or a cooler is generally provided with a plurality of heat transfer tubes in order to perform heat exchange with high efficiency, or fins are provided on the outer periphery of the heat transfer tubes. Further, as described above, the crude TiCl ₄ liquid is in a slurry form because some of the impurities are contained as solid particles. For this reason, when the crude TiCl ₄ liquid existing inside the heat exchanger is sucked under reduced pressure, the crude TiCl ₄ liquid tends to adhere to the heat exchanger and remain.

Therefore, development method TiCl ₄ production equipment of the present invention, serviced device 50 is a heat exchanger der to heat or cool the crude TiCl ₄ liquid is, for vacuum suction of TiCl ₄ liquid from the discharge port maintenance target apparatus 50 At this time, the crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the heat exchanger, and the TiCl ₄ liquid adhering to the heat exchanger is vaporized by heating the heat exchanger, and is sucked under reduced pressure as a gas. it recovered by TiCl ₄ liquid collecting container 40 by the installed cooling device from the discharge port until TiCl ₄ liquid collecting container 40 (suction gas cooler 42) by liquefying the TiCl ₄ gas.

The crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the heat exchanger, and the TiCl ₄ liquid adhering to the heat exchanger is vaporized by heating the heat exchanger, and is sucked under reduced pressure as a gas. All the TiCl ₄ liquid present in the heat exchanger can be discharged from the heat exchanger. Furthermore, if recovered by liquefying the TiCl ₄ gas is TiCl ₄ liquid collecting container 40 by the installed condenser between the outlet of the maintenance target apparatus 50 to the TiCl ₄ liquid collecting container 40 (suction gas cooler 42) All the TiCl ₄ liquid existing inside the heat exchanger can be recovered.

When vacuum suction is performed from a discharge port of a device such as a heat exchanger or a tank, the pressure inside the device is also reduced, so that a part of the TiCl ₄ liquid present in the device is gasified due to a decrease in boiling point. However, in the state where heating is not performed, cooling with latent heat of vaporization causes the temperature inside the device to drop, so that most of the TiCl ₄ liquid present inside the device is not gasified only by vacuum suction. Therefore, heating the heat exchanger is effective in efficiently gasifying and efficiently discharging the TiCl ₄ liquid existing in the equipment.

In this way, the crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the heat exchanger, and the TiCl ₄ liquid adhering to the heat exchanger is vaporized by heating the heat exchanger, and the air is sucked under reduced pressure as a gas. When the operator opens the scale and performs the scale removal work, the water can be washed without generating hydrochloric acid gas. For this reason, for example, it becomes possible to remove the scale by inserting the nozzle of the high pressure washer into the heat transfer tube of the heat exchanger and washing it with water, and the working efficiency can be greatly improved.

The heat exchanger for heating or cooling the crude TiCl ₄ liquid, said at TiCl ₄ production equipment shown in Figure 1, fluidized furnace crude TiCl ₄ gas cooler 20 to the crude TiCl ₄ gas obtained is cooled in the evaporator 31 An evaporator heater 32, a simple distillation cooler 33 that cools the crude TiCl ₄ gas sent from the evaporator 31, and a distillation tower that circulates and heats the crude TiCl ₄ liquid at the bottom of the distillation tower 34. This corresponds to the tower heater 36 for cooling the crude TiCl ₄ gas extracted from the top tower portion of the heating heater 35 and the distillation tower 34.

Since the boiling point of TiCl ₄ is 136 ° C., the heat exchanger can be heated by supplying heated steam of about 160 ° C. as high-temperature steam in the case of a heater. It can be performed by supplying heated steam at about 160 ° C. instead of cooling water.

The heating of the heat exchanger, be performed after discharge of crude TiCl ₄ liquid by vacuum suction has been completed, may be performed simultaneously with the discharge of crude TiCl ₄ liquid by vacuum suction. Whether the heat exchanger is heated after the discharge of the crude TiCl ₄ liquid by vacuum suction or at the same time, the TiCl ₄ gas is discharged from the outlet of the heat exchanger after the crude TiCl ₄ liquid is discharged. Discharged.

For this reason, a path from the discharge port of the maintenance target device 50 to the TiCl ₄ liquid recovery container 40 in the TiCl ₄ manufacturing facility, which passes through the suction gas cooler 42, and a path that does not pass through the suction gas cooler 42. A means for switching is provided, and when the crude TiCl ₄ liquid is sucked under reduced pressure, the switching means is operated so as not to pass through the suction gas cooler 42, and when TiCl ₄ gas is sucked under reduced pressure, the switching means is operated to suck. It is preferable that the path passes through the gas cooler 42. As a result, the crude TiCl ₄ liquid and TiCl ₄ gas sucked under reduced pressure can be efficiently processed.

In the maintenance method of the TiCl ₄ manufacturing facility of the present invention, a plurality of devices such as a heat exchanger and a tank 21 evaporator 31 are used, and the devices that have been repaired are connected to the production line, and the devices targeted for maintenance are separated from the production line. It is preferable to maintain. This is because it is possible to prevent the TiCl ₄ production facility including the fluidized furnace 10 from being stopped due to maintenance work.

In the TiCl ₄ production facility maintenance method of the present invention, a general liquid feed pump can be used as a pump for feeding the TiCl ₄ liquid to the equipment. As the liquid feeding pump, it is preferable to use a spiral pump because the TiCl ₄ liquid can be sent efficiently and inexpensively.

Next, the TiCl ₄ production facility of the present invention will be described with reference to the configuration example of the TiCl ₄ production facility of the present invention shown in FIG.

TiCl ₄ production equipment of the present invention, the flow reactor 10 to generate by forming a fluidized layer crude TiCl ₄ gas, cooling equipment (crude TiCl ₄ gas cooler crude TiCl ₄ gas and cooled crude TiCl ₄ liquid ) 20 and a distillation facility 30 for increasing the purity of the crude TiCl ₄ liquid to obtain a pure TiCl ₄ liquid, a TiCl ₄ manufacturing facility that can discharge the TiCl ₄ liquid to a device equipped with the TiCl ₄ manufacturing facility under reduced pressure. There is an outlet, there is a TiCl ₄ liquid collecting container 40 for collecting the TiCl ₄ liquid is sucked from the discharge port, the TiCl ₄ liquid collecting container 40 is characterized by having a pressure reducing function.

TiCl ₄ production equipment of the present invention, there is TiCl ₄ liquid collecting container 40 for collecting the TiCl ₄ solution, by the TiCl ₄ liquid collecting container 40 has a pressure reducing function, the vacuum suction can discharge when servicing the equipment The TiCl ₄ liquid can be easily sucked and recovered from the outlet of the device 50 having the outlet. For this reason, when opening and maintaining the atmosphere, it is possible to suppress the generation of hydrochloric acid gas due to the reaction of the remaining TiCl ₄ liquid with the moisture contained in the atmosphere. Corrosion can be reduced.

The pressure reducing function of the TiCl ₄ liquid recovery container 40 can be realized by providing a pressure reducing pump 41 for exhausting the gas in the recovery container as in the TiCl ₄ manufacturing facility shown in FIG. As the decompression pump 41, a generally circulated vacuum pump can be used. Among the vacuum pumps, the water ring pump is inexpensive and can be used in an acidic atmosphere. Therefore, it is preferable to use a water ring pump as the pressure reducing pump 41.

In the TiCl ₄ production facility shown in FIG. 1, only the maintenance target device 50 is connected to the TiCl ₄ liquid recovery container 40 by piping, but all maintenance for the purpose of removing scales is in the subsequent stage from the fluidized furnace 10. It is necessary to do it regularly with other equipment. In order to recover the TiCl ₄ liquid from a plurality of devices by suction under reduced pressure, the TiCl ₄ production facility of the present invention has a discharge port capable of suctioning the TiCl ₄ liquid at a plurality of devices, and the TiCl ₄ liquid recovery container 40 is piped. It is preferable to provide a switching means that is connected to the discharge ports of a plurality of devices and cuts off the connection with the devices other than the device to be maintained among the plurality of devices connected to the TiCl ₄ liquid recovery container 40.

Thus, by operating the switching means, the TiCl ₄ liquid can be sequentially recovered from the discharge ports of a plurality of devices. As a result, the number of TiCl ₄ liquid recovery containers 40 can be reduced, and maintenance work can be performed efficiently, so that the equipment cost and work time can be reduced.

In order to confirm the effect of the TiCl ₄ production facility maintenance method and TiCl ₄ production facility of the present invention, the following tests were conducted.

[Test conditions]
In this test, the flow reactor 10 shown in FIG. 1, by increasing the flow reactor 10 cooled equipment crude TiCl ₄ gas obtained is cooled in (crude TiCl ₄ gas cooler) 20, the purity of the crude TiCl ₄ liquid A TiCl ₄ production facility having a distillation facility 30 for pure TiCl ₄ liquid was used. In this test, two evaporator heaters were arranged, one evaporator heater was connected to the TiCl ₄ production facility, and the other maintained evaporator heater was disconnected from the TiCl ₄ production facility. In this state, one evaporator heater was separated from the TiCl ₄ manufacturing facility to be the maintenance target device 50, and the other evaporator heater 32 that had been maintained was connected to the TiCl ₄ manufacturing facility.

In the comparative example, the crude TiCl ₄ liquid discharged from the discharge port provided at the bottom of the maintenance target device 50 (evaporator heater separated from the TiCl ₄ manufacturing facility) is converted into TiCl ₄ using a liquid feed pump (not shown). By feeding to the liquid recovery container 40, the TiCl ₄ liquid existing inside the device was sucked and discharged from the discharge port. Thereafter, maintenance work was performed in which the maintenance target device 50 was opened to the atmosphere and the scale was removed by washing with water.

At this time, the sucked crude TiCl ₄ liquid was sent directly to the TiCl ₄ liquid recovery container 40 without operating the suction gas cooler 42 by operating a switching means (not shown). In addition, suction was performed without supplying high-temperature steam to the maintenance target device 50 and heating it with the stirring function of the TiCl ₄ liquid recovery container stopped. Furthermore, the crude TiCl ₄ liquid in the recovered TiCl ₄ liquid recovery container was subjected to gas-liquid separation and then was not returned to the middle of the TiCl ₄ production facility.

A spiral pump was used as the liquid feed pump. Further, in order to smoothly discharge the crude TiCl ₄ liquid, dry air was supplied from the upper part of the maintenance target device 50, and the air pressure at the upper part of the maintenance target device 50 was maintained at the same value as the atmospheric pressure.

In Example 1 of the present invention, first, the crude TiCl ₄ liquid discharged from the discharge port of the maintenance target device 50 (evaporator heater separated from the TiCl ₄ production facility) is converted into TiCl using a liquid feed pump (not shown). By sending it to the _4- liquid recovery container 40, the TiCl ₄ liquid present in the apparatus was sucked and discharged from the discharge port as much as possible. Subsequently, the gas in the TiCl ₄ liquid recovery container 40 is evacuated by the decompression pump 41 to reduce the pressure in the TiCl ₄ liquid recovery container, and the TiCl ₄ liquid recovery container is connected to the maintenance target device 50 to be maintained. The crude TiCl ₄ liquid in the device 50 was sucked under reduced pressure. When vacuum suction, as the vacuum pump 41 by using the water ring pump to evacuate the gas TiCl ₄ liquid collecting container, serviced device 50 while depressurizing the internal pressure of the TiCl ₄ liquid collecting container to 2.5kPa And connected. The other conditions were the same as those in the comparative example.

In Invention Example 2, the crude TiCl ₄ liquid in the TiCl ₄ liquid recovery container was returned to the middle of the TiCl ₄ production facility. Specifically, the crude TiCl ₄ liquid discharged from the bottom of the TiCl ₄ liquid recovery container was returned to the position in front of the evaporator 31 by a spiral pump which is a liquid feed pump (not shown). The test conditions other than these were the same as those of Example 1 of the present invention.

In Example 3 of the present invention, the stirring function of the TiCl ₄ liquid recovery container is operated. Specifically, a rotating blade rotating along a horizontal plane is used as a stirring bar, and the rotating blade is disposed in the vicinity of the bottom surface of the recovery container. Mechanical agitation was performed. The other test conditions were the same as those of Example 2 of the present invention.

In Example 4 of the present invention, the crude TiCl ₄ liquid is sucked from the outlet of the maintenance target device 50 under reduced pressure, and the TiCl ₄ liquid adhering to the maintenance target device 50 is vaporized by heating the maintenance target device 50 to reduce the pressure as gas. Aspirated. Specifically, after the discharge of the crude TiCl ₄ liquid by vacuum suction was completed, heating was performed by supplying heated steam of about 160 ° C. to the maintenance target device 50 (the evaporator heater separated from the TiCl ₄ manufacturing facility). .

Further, by operating a switching means (not shown), the crude TiCl ₄ liquid sucked under reduced pressure is sent to the TiCl ₄ liquid recovery container 40 without passing through the suction gas cooler 42, and the crude TiCl ₄ gas sucked under reduced pressure is sucked. After being cooled via the gas cooler 42, it was sent to the TiCl ₄ liquid recovery container 40. The test conditions other than these were the same as those in Invention Example 3.

In both the comparative example and the inventive example, the amount of the recovered crude TiCl ₄ liquid was measured.

Table 1 shows the test conditions and test results of the comparative example and the inventive example, respectively. Test conditions include vacuum suction processing, processing to return the crude TiCl ₄ liquid in the TiCl ₄ liquid recovery container to the TiCl ₄ manufacturing facility, stirring function of the TiCl ₄ liquid recovery container, and equipment to be maintained (evaporation separated from the TiCl ₄ manufacturing facility) Regarding the heat treatment of the device heater, a circle mark is shown when the treatment is performed or the function is used, and a cross mark is shown when the treatment is performed or the function is not used. Moreover, as a test result, the loss amount of TiCl ₄ liquid, the working environment after opening to the atmosphere, the state of equipment corrosion, and the clogged state of the outlet of the TiCl ₄ liquid recovery container are shown.

Here, the amount of loss TiCl ₄ solution, based on the recovery of the maintenance target equipment present invention could recover all the crude TiCl ₄ liquid present in the (TiCl ₄ production evaporator heater is disconnected from the facility) in Example 4 Calculated as Specifically, the recovery of the present invention Example 4 and the amount of loss TiCl ₄ solution calculates a difference between the amount of TiCl ₄ solution was returned to TiCl ₄ production facilities in each test. The loss amount of the TiCl ₄ solution calculated in this way is shown in Table 1 as relative values with the comparative example being 100.

In addition, the meanings of the symbols in the “Working environment after opening to the atmosphere and the state of equipment corrosion” shown in Table 1 are as follows.
○: Indicates that the work environment was not deteriorated and the equipment was not corroded.
(Triangle | delta): Although the deterioration of working environment and corrosion of an apparatus were recognized, it shows that it was slight.
X: Indicates that the working environment was remarkably deteriorated and the equipment was severely corroded.

The meanings of symbols in the column “TiCl ₄ liquid recovery container outlet closure” shown in Table 1 are as follows.
◯: Indicates that the entire amount of the TiCl ₄ liquid in the collection container was discharged without blocking the discharge port.
△: Although outlet is temporarily closed, indicating that the total amount of TiCl ₄ liquid recovery container has been discharged.
-: The process of returning the crude TiCl ₄ liquid in the recovery container to the middle of the TiCl ₄ production facility was not performed, and thus the clogging state of the discharge port was not evaluated.

[Test results]
From the results shown in Table 1, in the comparative example, when the crude TiCl ₄ liquid is sucked and collected by the liquid feed pump, and the maintenance work 50 is opened to the atmosphere and the scale is removed by washing with water, Since a large amount of hydrogen chloride gas was generated, the working environment was significantly deteriorated and the equipment was severely corroded. That is, in the comparative example, a considerable amount of the crude TiCl ₄ liquid remains in the maintenance target device 50 (the evaporator heater separated from the TiCl ₄ production facility), and the crude TiCl ₄ liquid is discarded together with the scale to be removed by washing with water. It was.

In Example 1 of the present invention, a slight amount of hydrogen chloride gas was generated during maintenance work in which the crude TiCl ₄ liquid was sucked and collected by vacuum suction, and the maintenance target device 50 was opened to the atmosphere and the scale was removed by washing with water. As a result, deterioration of the working environment and corrosion of the equipment were observed, but were slight. As described above, in Example 1 of the present invention, compared with Comparative Example 1, the working environment is deteriorated and the state of corrosion of the equipment is improved. Therefore, most of the TiCl ₄ liquid existing inside the equipment can be discharged by vacuum suction. It became clear that deterioration of working environment and corrosion of equipment due to hydrochloric acid gas could be reduced.

In Example 2 of the present invention, the recovered crude TiCl ₄ liquid was returned to the middle of the TiCl ₄ production facility, and the loss of the TiCl ₄ liquid was reduced to 10. At this time, the quality of the obtained pure TiCl ₄ was confirmed, which was equivalent to the case where the recovered crude TiCl ₄ liquid was not returned to the middle of the TiCl ₄ production facility. Therefore, by returning the recovered crude TiCl ₄ liquid in the middle of TiCl ₄ production facilities, it was found that can effectively utilize the recovered crude TiCl ₄ liquid. Further, in Example 2 of the present invention, the stirring function was stopped when the crude TiCl ₄ liquid was discharged from the discharge port of the TiCl ₄ liquid recovery container, and as a result, the discharge port was temporarily blocked. The whole amount of TiCl ₄ liquid was discharged

In Example 3 of the present invention, the stirring function of the TiCl ₄ liquid recovery container was operated, and as a result, the entire amount of the crude TiCl ₄ liquid in the recovery container was discharged without closing the discharge port. Therefore, it was confirmed that the concern that the TiCl ₄ liquid recovery container has a stirring function could block the outlet and obstruct the extraction of the crude TiCl ₄ liquid could be eliminated.

In the present invention example 4, the crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the maintenance target device 50, the maintenance target device 50 (heater for evaporator separated from the TiCl ₄ manufacturing facility) is heated, and the TiCl sucked under reduced pressure is further heated. _{The 4} gases were liquefied with a cooler and recovered in a TiCl ₄ liquid recovery container. In the present invention example 4, the TiCl ₄ loss is reduced from 10 to 0 as compared with the present invention examples 2 and 3, and the maintenance target device 50 (heater for evaporator separated from the TiCl ₄ production facility) is opened to the atmosphere. Deterioration of work environment and corrosion of equipment were not observed during maintenance work to remove scale by washing with water.

These, together with the maintenance target equipment if a heat exchanger for heating or cooling the crude TiCl ₄ liquid to vacuum suction the crude TiCl ₄ liquid from the discharge port of the heat exchanger, the heat exchanger by heating the heat exchanger It was revealed that all the TiCl ₄ liquid existing inside the heat exchanger can be discharged from the heat exchanger if the TiCl ₄ liquid adhering to the vessel is vaporized and sucked under reduced pressure as a gas.

In the maintenance method of the TiCl ₄ production facility of the present invention, most of the TiCl ₄ liquid existing in the apparatus can be discharged by sucking the TiCl ₄ liquid under reduced pressure from the discharge port of the apparatus. For this reason, when maintaining with the atmosphere open, the amount of hydrochloric acid gas generated by the remaining TiCl ₄ liquid reacting with the moisture contained in the atmosphere can be suppressed. Corrosion can be reduced.

TiCl ₄ production equipment of the present invention, there is TiCl ₄ liquid collecting container for collecting the TiCl ₄ solution, by which this TiCl ₄ liquid collecting container having a pressure reducing function, exhaust equipment was serviced when servicing the equipment The TiCl ₄ liquid can be easily recovered from the outlet by vacuum suction.

Therefore, the TiCl ₄ production facility maintenance method and TiCl ₄ production facility of the present invention can be effectively used for the production of TiCl ₄ .

10: Fluidized furnace, 11: Cyclone, 20: Crude TiCl ₄ gas cooler (cooling equipment),
21: Crude TiCl ₄ liquid tank 30: Distillation equipment 31: Evaporator
32: heater for evaporator, 33: cooler for simple distillation, 34: distillation tower,
35: heater for distillation tower, 36: tower top cooler, 37: cooler for rectification,
40: TiCl ₄ liquid recovery container, 40a: rotor blade, 41: pump for pressure reduction,
42: Suction gas cooler, 50: Equipment subject to maintenance

Claims (3)

The crude TiCl ₄ gas obtained by fluidized bed was cooled to crude TiCl ₄ liquid, a method of servicing a TiCl ₄ production facility to pure TiCl ₄ liquid in a crude TiCl ₄ liquid distillation step,
Among the equipment provided in the TiCl ₄ production facility, the TiCl ₄ liquid is decompressed and sucked from the outlet of the equipment targeted for maintenance, and then released to the atmosphere, and maintained.
When the TiCl ₄ liquid is suctioned from the outlet of the maintenance target device under reduced pressure, the TiCl ₄ liquid recovery container is depressurized by exhausting the gas in the TiCl ₄ liquid recovery container, and this TiCl ₄ liquid recovery container is used as the maintenance target. By connecting with the device, the TiCl ₄ liquid in the maintenance target device is sucked under reduced pressure,
The TiCl ₄ liquid collected by suction is gas-liquid separated in the TiCl ₄ liquid recovery container,
When vacuum suctioning the TiCl ₄ liquid from the outlet of the maintenance target device, the crude TiCl ₄ liquid is vacuum suctioned from the outlet of the heat exchanger that is the maintenance target device of the TiCl ₄ manufacturing facility, and the heat exchanger The TiCl ₄ liquid adhering to the heat exchanger is vaporized by heating, and sucked under reduced pressure as a gas,
Of TiCl ₄ production facilities and recovering in the TiCl ₄ liquid collecting container to liquefy the TiCl ₄ gas with the installed condenser between the outlet of the serviced device to said TiCl ₄ liquid collecting container Maintenance method. Withdrawn liquid in the TiCl ₄ liquid collecting container, by returning to the middle of TiCl ₄ production facilities, of TiCl ₄ Plant according to claim 1, characterized in that the effective use of suction recovered TiCl ₄ solution Maintenance method. A flow reactor to produce a by forming a fluidized layer crude TiCl ₄ gas, the crude TiCl ₄ and cooling equipment to be cooled crude TiCl ₄ liquid gas, the crude TiCl ₄ liquid pure TiCl ₄ liquid to increase the purity of the A TiCl ₄ production facility having a distillation facility,
TiCl ₄ has manufacturing facility comprises TiCl ₄ solution under a reduced pressure suction can discharge port device, there is TiCl ₄ liquid collecting container for collecting the TiCl ₄ liquid is sucked from the discharge port, the TiCl ₄ liquid collecting container is reduced pressure It has a function
The maintenance target device is a heat exchanger provided in the TiCl ₄ production facility,
The TiCl ₄ production facility is
Means for heating the heat exchanger and evaporating the TiCl ₄ liquid adhering to the heat exchanger when the crude TiCl ₄ liquid is sucked under reduced pressure from the outlet of the heat exchanger;
A cooler that is installed between the outlet of the maintenance target device and the TiCl ₄ liquid recovery container and liquefies TiCl ₄ gas so that the liquefied TiCl ₄ gas is recovered in the TiCl ₄ liquid recovery container A TiCl ₄ production facility, further comprising a cooler configured as described above.

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