JPH0256408B2 - - Google Patents

Description

[Detailed description of the invention] The present invention provides tetrachloride of Ti, Zr, Hf or Nb,
Molten metal Mg of metal chloride like Ta pentachloride
This invention relates to an apparatus and method for evaporating and removing by-product MgCl ₂ and residual metal Mg present in these metals by heating sponge-like metals obtained by reduction by the so-called Chlor method under reduced pressure. .

Industrial production of metals such as Ti and Zr is generally carried out by the above-mentioned Chlor method, but the sponge-like metals obtained in this way contain relatively large amounts of unreacted metal Mg and by-product MgCl ₂ . Since these substances are present, an operation to vaporize and separate Mg and MgCl ₂ by distilling them in vacuo is subsequently performed. This process involves (1) taking out the deposits consisting of these formed metals and inclusions while holding them in a removable container (inner cylinder), and placing them in the upper part of the outer cylinder of a separately provided vacuum distillation apparatus (for example, 34646) or (2)
At the bottom (described in the patent application No. 56-77461 by the applicant)
This is transferred to a heating section that has been prepared and heated from the outside to approximately 1000℃ under reduced pressure to increase the vapor pressure of Mg and MgCl ₂ and promote separation. Mg and gas in the gas phase can be removed by cooling the cooling section installed in the
A structure has been proposed in which MgCl ₂ is removed by condensation and adhesion. In these examples, an empty inner cylinder having the same structure as that used in the reduction process is housed in the cooling section, and the inner cylinder is used for the next reduction process with condensate attached to its inner surface. Furthermore, when increasing the throughput per batch, a configuration that does not use such an inner cylinder may be adopted, but in this case, (3) the reaction vessel is combined with a cooling section after the reduction process, and (4) It is known that a cooling section is arranged coaxially above the reaction vessel and partitioned in advance, and this partition is removed after the reduction process (for example, as described in Japanese Patent Publication No. 55-36254, etc.). 5) An example in which the container in which the generated metal is deposited is inverted after cooling and installed above the cooling section, and (6) an example in which the cooling section is placed above the container.

In such conventional technology, configurations (1), (2), (5), and (6) use dedicated equipment for each process, so
Each device itself can be of simple and efficient design. Particularly in cases (2) and (6) in which the heating section is placed at the bottom, it is easy to obtain a large-capacity device. However, since the inner cylinder must be moved when transitioning from the reduction process to the separation process, the labor and time required for cooling, moving, disassembling and assembling the apparatus, etc. when taking it out from the reduction apparatus, and the energy for reheating the deposits are required. is necessary. When heating the deposit from the outside
Evaporation of Mg and MgCl ₂ gradually moves from the inner cylinder wall surface to the center, but at this time, heat transfer to the center is partially or essentially through the porous sponge-like metal from which inclusions have been removed. Moreover, since it is carried out under reduced pressure, the heat transfer efficiency is extremely low, which is one of the reasons why the separation process takes a long time.

On the other hand, method (4), which does not involve transferring the deposits, has the disadvantages of cooling the deposits, moving the inner cylinder, disassembling and reassembling the device, and energy consumption for reheating the deposits. Although savings can be expected, on the other hand, there is a drawback that a complicated mechanism is required to partition the heating section and the cooling section and to open and close the partition. Furthermore, in this case, the heating section is placed below the cooling section as in (2) and (6), and the lower end of the cooling section and the upper end of the heating section are connected, but in this configuration, the condensates of Mg and MgCl ₂ Adheres to the walls of the cooling section as a solid and subsequently condenses.
The Mg and MgCl ₂ must be fixed onto this, so the vacuum separation step in this configuration is limited by the low cooling rate through this deposit. Furthermore, even once the condensate has landed, there are parts that fall into the heating section due to the primary or secondary heat rays emitted from the heating section, and as a result, even with this type of separation device, a sufficient processing speed cannot be obtained. There is.

Furthermore, if a container with Mg and MgCl ₂ deposited in the cooling section is used in the reduction process, in any of the above configurations, it is necessary to separate the heating section and cooling section and assemble it as a reduction device. The trapped air had to be replaced again using expensive Ar gas.

Therefore, the present invention has been made to eliminate the drawbacks associated with the prior art, and its gist is, first, to melt and hold Mg;
Essentially, by means of a removable top lid, which allows the metal to be precipitated by the reaction of the Mg with the metal chloride fed from above, and which can vaporize the by-product MgCl ₂ and residual Mg. A closed reduction and evaporation chamber and a heating furnace arranged around the same, a condensation chamber with a removable top and a removable lid installed adjacent to the reduction and evaporation chamber and capable of condensing vapors of Mg and _MgCl2 . A small chamber having a temperature controllable chamber and a cooling means for the chamber, a lid of the reduction and evaporation chamber provided inside, and a steam exhaust hole provided around the small chamber separated from the small chamber; The reduction evaporation chamber and the condensation chamber are connected by a connecting tube that is connected at both ends to the discharge hole and the lid of the condensing chamber and can maintain the entire body at a temperature at which Mg and MgCl ₂ do not solidify, and the vapor flow through the connecting tube is controlled. It is equipped with a valve that can be operated from the outside and is further provided with a means for exhausting the inside of the reduction evaporation chamber, condensation chamber, and connecting pipe, thereby vaporizing MgCl ₂ and Mg that are present together with the metal produced by the above reaction. A second aspect of the present invention relates to a reduction and purification apparatus for metal chlorides, which is characterized in that metal chlorides are guided to the upper part of a condensation chamber and collected in the chamber as a liquid phase or solid phase. In particular, the main idea is a configuration in which a second cylinder (inner cylinder) is disposed within the reduction evaporation chamber and the condensation chamber.

In the present invention, the reduction and evaporation chamber can be configured in various ways. This may consist, for example, of a single cylinder with a closed bottom, or a rostre-like bottom plate with a number of perforations inside the first cylinder (outer cylinder) which isolates the interior from the atmosphere. A second cylindrical body (inner cylinder) having an open lower end with an attached cylindrical member may be provided. In the former configuration, the amount of metal deposited per batch can be increased compared to the volume of the cylinder. In the latter case, the amount of metal produced that can be deposited is somewhat reduced, but it is easy to separate the produced metal from the by-product (MgCl ₂ ) and take it out of the room, and it is also easy to remove the inclusions vaporized during the distillation process. Since the surface area over which is released is large, the time required for this process is short. A pipe for discharging the MgCl ₂ byproduct in the form of a melt to the outside can be attached to the bottom of the cylinder. In this case, in the case of a single tube configuration, the generated metal will be deposited directly on the tube, so in order to suppress the metal from entering the tube and to facilitate the discharge of MgCl ₂ , a stand is provided to prevent the metal from entering the tube. Preferably, the deposits are kept away from the bottom surface of the body. A cooling jacket can be provided on the upper outer periphery of these single cylinders or outer cylinders, as described in Japanese Patent Application Laid-Open No. 188632/1983, in order to maintain the Mg bath surface constant and carry out the reduction reaction operation.

A removable lid is airtightly attached to the open upper end of the tube configuration. The lid has a dedicated configuration for each of the reduction evaporation chamber and the condensation chamber. The lid of the reduction and evaporation chamber has a small chamber extending axially inward in a horizontal section and closed at the top and open at the bottom, and has a steam exhaust hole partitioned from this on the outside of the small chamber. Almost in the center of the chamber is a tube extending downward for supplying TiCl ₄ and ZrCl ₄ to be reduced. This supply pipe or the sheath pipe provided coaxially on the outside thereof has a disc or cone-shaped flange at the lower part and is attached so as to be movable up and down. The flanges are then configured to close the lower end of the chamber when the tubes are lowered. The interior of this chamber can be maintained at approximately 750°C by heating from the surroundings, thus preventing clogging of the supply pipes due to solidification of chlorides and the like. Further, at the end of the purification process, a suitable cooling means such as water cooling or air cooling is provided in this small chamber in order to cool this small chamber and solidify and adhere a small amount of remaining Mg and MgCl ₂ . The steam exhaust hole is connected to the lid of the condensing chamber with or without an opening/closing means such as a valve that can be operated from the outside. The connection between the connecting pipe and the steam exhaust hole is essentially the same as in the patent application filed in 1982, which is the applicant's earlier application.
The one described in No. 189846 can be used. The connecting pipe and the opening/closing means are provided with heating means to prevent Mg and MgCl ₂ from solidifying inside. In addition to this, a tube for introducing Mg in the form of a melt into the reduction and evaporation chamber is arranged outside the lid chamber or in other parts of the lid, if necessary. A heating furnace that supplies heat to such a reduction and evaporation chamber is arranged around the cylindrical structure. Gas-fired furnaces are advantageous in terms of energy costs, but in the case of electric furnaces (for example, as detailed in Japanese Patent Application No. 56-50896), the space between the (outer) cylinder and the furnace wall is By making the space a sealed structure and filling it with inert gas such as argon, oxidation of the outside surface of the cylinder can be effectively prevented, and the pressure is maintained close to room pressure by making it positive pressure during the reduction process and negative pressure during the distillation process. By doing so, deformation of the wall material due to the pressure difference between the inside and outside of the cylinder wall can be prevented.

On the other hand, the condensation chamber has almost the same structure as the reduction and evaporation chamber, except that a cooling means is provided. That is, when the reduction and evaporation chamber has a single cylinder configuration, the condensation chamber is configured with a single cylinder, and when it has an internal/external cylinder configuration, the condensation chamber is configured with an appropriate cooling means on the outside thereof. The cooling means can be achieved by immersing the entire cylinder structure in water or by wetting its outer surface with water. In addition, in the case of an inner/outer cylinder configuration, the outer cylinder may be provided with a water jacket around the outer cylinder for exclusive use for condensation.

The reduction evaporation chamber and the condensation chamber are connected by a connecting pipe, but there are valves and partition plates that are replaced each time on the connecting pipe itself or near the joint between these chambers to isolate the two chambers during the reduction process. Placed. This connecting pipe is provided with suitable heating means to prevent Mg and MgCl ₂ from solidifying. Mg that has partially liquefied inside the pipe
In order to allow MgCl ₂ to flow into the cooling chamber, it is preferable to provide a downward slope towards the cooling chamber.

The invention will now be described with reference to the accompanying drawings, which show apparatus suitable for its implementation. FIG. 1 is a vertical cross-sectional view schematically showing a reduction purification apparatus having a single cylinder configuration and FIG. 2 having an inner and outer cylinder configuration. The reduction and evaporation chamber, designated as a whole by 1 in FIG. The outer periphery of the furnace wall is tightly covered with an iron skin 4. A lid 5 that seals the open upper end of the cylinder body 2 has a central cylindrical chamber 6;
It has a gas jacket 7 surrounding the lower part of the chamber and a water cooling jacket 8 surrounding the upper part. A steam exhaust hole 9 is provided on the outer surface of the chamber 6 adjacent to the jacket 7, and the lower portion of the chamber 6 is maintained at a high temperature by high temperature gas such as burner combustion gas introduced into the jacket. An exhaust pipe 10 can also be provided on the outside of the small chamber to reduce the pressure inside the chamber. A chloride supply pipe 11 extends downward within a sheath pipe 12 substantially on the axis of the small chamber 6 . The tubes 11 and 12 can be moved up and down, and a flange 13 is fixed to the lower part of the sheath tube 12, so that the opening 14 at the lower end of the chamber is closed when the tubes 11 and 12 are lowered. One preferred example of the configuration of the inner surface of the chamber and the flange is one in which the bottom of the chamber is shaped like a funnel and the flange combined therewith is configured like a cone, as shown in FIG. The cooling jacket 8 provided at the top of the small chamber is used to open the small chamber by raising the flange 13 at the end of the refining process, as will be detailed later.
This is to cause residual Mg and MgCl ₂ to precipitate on the inner wall by cooling the small chamber. Steam exhaust hole 9
The upper part constitutes a connecting end having a valve mechanism 15, and is connected to a connecting pipe 16 on the condensing chamber side at this side. These valve mechanisms 15 and conduits 16
The surrounding area is kept at a temperature that prevents Mg and MgCl ₂ from solidifying inside by the flow of high-temperature gas. Heating can also be done by electric heating. Mg as required
A tube 17 for introducing the molten material can be provided along the wall of the cylinder as shown in this figure, or in another part, for example in the lid. Melted and held within the cylinder body 2
Mg and metal chlorides fed from above, e.g.
Metal Ti produced by reaction with TiCl ₄ is 18
On the other hand, the by-product MgCl ₂ accumulates in the form of a melt at the bottom of the cylinder, and in the example shown, it enters the inside of the cylinder from the top of the side wall and extends downward. The water is discharged from the pipe 19 to the outside of the room via the valve 20. A space (furnace space) 21 between the cylinder body 2 and the furnace 3 is sealed and pressure control means are provided.

On the other hand, the condensing chamber 22 is composed of a single cylinder type cylinder 23 and a lid 24 that closes the top of the cylinder, as in the case of the reduction and evaporation chamber, and the cylinder part is immersed in water in a water tank 25. The lid 24 has a steel disc 26 and a can 27 attached below it and filled with a heat insulating material, in which an exhaust pipe 28 and a suction hole 29 are provided. The suction hole 29 is connected to the vapor extraction hole 9 of the reduction and evaporation chamber via the connecting pipe 16 and valve 15 connected thereto on the upper surface of the steel plate. Each of these parts is maintained at a temperature at which Mg and MgCl ₂ do not solidify, as described above, to direct these inclusions from the reduction evaporation chamber to the condensation chamber. The connecting pipe 16 is sloped downward toward the condensing chamber in order to allow the partially liquefied Mg or MgCl ₂ inside to flow into the condensing chamber.

On the other hand, FIG. 2 is a sectional view showing an example in which the reduction evaporation chamber 30 and the condensation chamber 31 are constructed in an inner/outer cylinder type. In this case, instead of the produced metal deposition table 18 in FIG. 1, second cylinders (inner cylinders) 34 and 35 having removable rostre-shaped bottom plates 32 and 33 at the bottom are attached to the respective lids by a common bolt. The configuration is essentially the same as that in FIG. 1, except that the first cylinder (outer cylinder) 38, 39 is supported by cylinders 36, 37 and constitutes each chamber. Here too, the condensation chamber is a water tank 40 as a cooling means.
The cylindrical part is placed in. These chambers 30, 31 are connected by a connecting pipe 41 similar to that shown in FIG.

In order to perform the reduction process in the reduction purification apparatus configured in this way, the chloride supply pipe 11 or 4 is
2 and sheath tubes 12, 43 are lowered to predetermined positions to close the lower ends of the lids 5, 36 of the reduction and evaporation chamber, and close the valves 15, 44. After introducing a predetermined amount of molten Mg through the tubes 17 and 45, a metal chloride such as TiCl ₄ is supplied to the Mg bath surface from the tubes 11 and 42 in a liquid phase or a gas phase. Due to the reaction between the two, generated metals such as Ti are deposited on the table 18 or the inner cylinder bottom plate 32. Most of the by-product _MgCl2 is continuously or intermittently removed to the outside via pipes 19,46. When the reduction process is completed, the valve between the reduction evaporation chamber and the condensation chamber is opened to connect the two chambers, and both chambers are suctioned and depressurized through the exhaust pipes 28 and 47 on the lid of the condensation chamber or other piping along with this. do. In addition, the deposit in the reduction and evaporation chamber is heated by a furnace to vaporize Mg and MgCl ₂ . The steam thus generated passes through the connecting pipes 16 and 41 into the condensation chamber and is liquefied, and further solidifies and adheres to the vessel wall or bottom. During this time, the entire area around the connecting pipes 16, 41 and the steam exhaust holes 9, 48 of the reduction evaporation chamber connected thereto is maintained at a temperature of 750°C or higher by the flow of high-temperature gas, and no solidified matter adheres to the inner surface. Prevent this from happening. This operation can be continued until Mg and MgCl ₂ present in the produced metal are essentially removed, but this separation operation can be efficiently completed in the following manner. That is, when most of these Mg and MgCl ₂ are removed, the flange 1 along with the sheath tubes 12 and 43
3, 49 to open the lower end of the lid chamber of the reduction evaporation chamber, and also open the water cooling jacket 8, 50 around the chamber.
By cooling the lid, these vapors are condensed and at least a portion of them is deposited on the inner surface of the lid. In this case, the deposits are recovered by heating the lid in the next reduction step. Refined produced metals such as Ti are obtained within a single cylinder or inner cylinder, and are recovered by decomposing the reduction and evaporation chamber. On the other hand, the inner surface is used as a condensation chamber.
A single cylinder or inner and outer cylinders to which Mg and MgCl ₂ are deposited are placed in a furnace and used as a reduction and evaporation chamber to consume or collect these deposits.

Example 1 Using the apparatus configuration essentially shown in FIG.
Metallic Ti was produced by Mg reduction of TiCl ₄ .
The cylinder has an inner diameter of 1.8m and a length of 5.6m, with a wall thickness of 32mm.
Made of SUS410 stainless steel, it was placed in an electric furnace with an outer diameter of 2.8 m and a height of approximately 6.2 m, surrounded by an iron shell. The space inside the furnace, that is, the space between the cylinder and the furnace, was configured to be airtight. The lid has a maximum inner diameter of 1.3m and a length of 2.6m.
It has a small chamber with a cooling water jacket in the upper part around it, and the lower part is heated by the flow of combustion gas from the furnace and burner. A cylindrical body with the same structure as above is used for the condensation chamber, and an exhaust pipe is placed through the insulation layer on the bottom of the lid, and a connecting pipe with an inner diameter of 40 cm attached to the top is connected to the steam exhaust hole of the reduction evaporation chamber. A burner was installed in a jacket connected to the connecting end and provided around its outer periphery to allow combustion gas to flow.

In this equipment, approximately 9 tons of molten Mg was introduced into the reduction evaporation chamber under an argon atmosphere, and the inside was heated to approximately 800 kg.
After raising the temperature to ℃, liquid TiCl ₄ was supplied at a rate of 400 kg/hour to carry out a reaction. While intermittently discharging by-produced MgCl ₂ from the bottom of the cylinder, a total of 25 tons of TiCl 4 was charged over 60 hours, and the injection of TiCl ₄ was stopped.
Mg and MgCl ₂ were discharged from the bottom of the cylinder. After evacuating the condensing chamber, the valve at the end of the connecting pipe was opened to connect it to the reduction evaporation chamber. The steam outlet and connecting tubes were maintained at approximately 800° C. by sending a stream of burner combustion gases to a gas jacket in the lid of the reduction evaporation chamber. Furthermore, the temperature of the reduction and evaporation chamber was raised to approximately 1000°C by a surrounding furnace, while water was filled in the container containing the condensation chamber and circulated. In addition, the furnace space around the reduction and evaporation chamber was evacuated and the pressure was reduced. A heating operation was performed for about 70 hours under these conditions, and the evaporated Mg and MgCl ₂ were deposited on the inner surface of the cylinder of the condensation chamber. At this time, when the amount of Mg etc. passing through decreases and the temperature rise in the connecting pipe slows down, the valve of the steam exhaust hole is closed, while the chloride supply pipe etc. is raised to open the small chamber, and water is poured into the jacket around this. At the same time, cooling air is sent to the gas jacket to cool the small chamber and remove any remaining Mg and
MgCl ₂ vapor was solidified and attached near the small chamber.

The operation was carried out according to the above procedure, and in the end, about 6.2 tons of
Ti was recovered from the cylinder. A condensation chamber lid was installed on the cylinder from which the Ti was removed, and it was used as a condensation chamber in the next step. In addition, after cooling the cylindrical body to which Mg or MgCl ₂ was attached, the lid was quickly replaced with one for the reduction evaporation chamber, and the lid was used as the reduction evaporation chamber.

The above-mentioned cylindrical body could be subjected to the reduction purification process more than 50 times in total.

Example 2 Using the apparatus configuration essentially shown in FIG.
Metallic Ti was produced by Mg reduction of TiCl ₄ .
The inner diameter of the reduction evaporation chamber outer cylinder made of SUS316 stainless steel is
It has a cylindrical shape with a length of 1.7 m, a length of 4.5 m, and a wall thickness of 32 mm. Inside, an inner cylinder made of SUS430 stainless steel with an inner diameter of 1.6 m, a length of 3.7 m, and a wall thickness of 19 mm is suspended from the lid, making the entire outer diameter 2.5 m. ,
It was placed in an electric furnace with a height of 5 m and covered with an iron shell. The space inside the furnace between the outer cylinder and the furnace was configured to be airtight. On the other hand, the condensing chamber outer cylinder is of the same construction as that of the reduction and evaporation chamber, and is supported within it by a lid of essentially the same construction as in Example 1, and is supported within it by a lid of essentially the same construction as that of the reduction and evaporation chamber. The tube was hung essentially empty using bolts. Inner diameter installed on the condensing chamber lid
The 40 cm connecting tube was equipped with a jacket around the circumference for passing the burner combustion gases and was connected to the steam outlet at the end.

In this device, the reduction evaporation chamber is set to an argon atmosphere, approximately 7 tons of molten Mg is introduced, and the inner cylinder is heated to approximately 800 tons.
After raising the temperature to 0.degree. C., liquid TiCl ₄ was supplied at a rate of 400 kg/hour to perform a reaction operation. produce by-products
approximately 50 min while intermittently discharging _MgCl2 from the bottom of the outer cylinder.
After charging a total of 20 tons over a period of time, the injection of TiCl ₄ was stopped. All the Mg and MgCl ₂ remaining under the bottom plate were discharged, and the bolts suspending the inner cylinder were turned to lower the inner cylinder a little to form a gap between it and the bottom surface of the lid. After evacuating the condensing chamber and heating the lid and connecting pipe of the reduction evaporation chamber to approximately 800°C, the valve was opened and the chamber was connected to the condensing chamber immersed in a water tank. The reduction and evaporation chamber was heated to about 950 to 1000° C. to evaporate Mg and MgCl ₂ and lead them to the condensation chamber, where they were condensed and deposited on the inner cylinder wall surface. At this time, in the reduction evaporation chamber, the temperature of the entire chamber was raised to approximately 800°C by heating by the surrounding furnace and high-temperature gas (combustion gas) was fed into the gas jacket, and at the same time the pressure in the surrounding furnace space was reduced. The refining operation was carried out in this manner, and when the temperature rise in the conduit slowed down due to a decrease in the amount of Mg etc. passing through about 80 hours after the start of temperature rise, the valve of the steam exhaust hole was closed while the chloride supply pipe was raised. The chamber was opened, and the chamber was cooled by running water through the jacket around it, causing the Mg and MgCl ₂ vapors remaining in the chamber to solidify and adhere to the vicinity of the chamber.

Next, the reduction and evaporation chamber was cooled, the connecting bolts were removed, the lid was removed, and finally the inner cylinder was taken out. In the end, approximately 5 tons of Ti sponge were recovered from this inner cylinder. The inner cylinder of the condensation chamber still had Mg and MgCl ₂ attached to it, and the lid was replaced with one for the reduction and evaporation chamber, and the lid was placed in the outer cylinder for the next reduction process. On the other hand, the inner cylinder from which the produced Ti was taken was fitted with a condensation chamber lid and used for the next refining process.

The above-mentioned outer cylinder withstood repeated reduction and purification processes more than 50 times.

In both of the above examples, the total time required for the patch cycle, including the reduction and purification steps as well as the disassembly and assembly of the cylinder, was approximately 10 days in Example 2, for example.
This represents a significant improvement over the approximately 15 days required to produce the same amount of Ti sponge in a conventional configuration in which the reduction and purification steps were performed in separate cylinders.

As can be understood from the above explanation, in the present invention, 1. Since the metal produced in the reduction process can be immediately subjected to the purification process, that is, the vacuum distillation operation, without being transferred, the labor required for switching the process is reduced. Savings in time and energy for cooling and subsequent reheating previously required in conjunction with transport are achieved.

2 When performing the refining process, as in the past, the cylindrical body that holds the deposits to be treated and the cylindrical body to which the condensate is attached are combined in the axial direction, integrated, and charged into the furnace (or This eliminates the need for heavy-duty cranes, which were previously indispensable. buildings can accommodate larger capacity equipment.

3 In conventional equipment, unreacted chloride (e.g. TiCl ₄ ) remaining inside the cylinder sometimes leaked into the atmosphere when the equipment was disassembled during the transition from the reduction process to the purification process. There were no accidents and environmental pollution was prevented in this respect.

4. The problem of solidified matter (Mg and MgCl ₂ ) falling into the evaporation section, which often occurred in the vacuum distillation equipment configuration that has been widely used in the past, with the cooling section on the top and the evaporation section on the bottom, has been fundamentally solved. From this aspect as well, processing time has been shortened.

5. Lower chlorides, which often occur at the end of the reduction process in conventional methods and cause a decrease in yield and ignition of the produced metal, are no longer produced, and the yield and quality of the product are improved.

[Brief explanation of drawings]

FIGS. 1 and 2 are schematic cross-sectional views showing an example of an apparatus configuration according to the present invention. In the figures, main parts are indicated by the following reference numerals. 1... Reduction evaporation chamber, 2... Cylindrical body, 3... Furnace, 5
... Lid, 9 ... Steam exhaust hole, 11 ... Chloride supply pipe, 15 ... Valve, 16 ... Connection pipe, 17 ...
Mg introduction pipe, 19...MgCl ₂ discharge pipe, 22... Condensation chamber, 23... Cylindrical body, 24... Lid, 25... Water tank, 29... Suction hole, 30... Reduction evaporation chamber, 31
... Condensation chamber, 34, 35 ... Inner cylinder, 36, 37...
... Lid, 38, 39 ... Outer cylinder, 40 ... Water tank, 41
... Connection pipe, 42 ... Chloride supply pipe, 45 ...
Mg introduction pipe, 46...MgCl ₂ discharge pipe.

Claims (1)

[Scope of Claims] 1. An upper part capable of melting and retaining Mg and precipitating metal by reaction of the Mg with a metal chloride supplied from above, and capable of vaporizing by-product MgCl and residual Mg. A reduction and evaporation chamber essentially sealed by a removable lid and a heating furnace disposed around the reduction and evaporation chamber are provided adjacent to the reduction and evaporation chamber for condensing Mg and MgCl ₂ vapors. It has a condensation chamber whose upper part is sealed with a removable lid, a temperature-controllable chamber having a cooling means for the chamber, and a lid of the reduction evaporation chamber provided inside, and a temperature-controllable chamber around the chamber from which the chamber is cooled. It has a steam exhaust hole provided at a distance, and both ends are connected to the exhaust hole and the lid of the condensation chamber, and the whole is made of Mg and
The reduction evaporation chamber and the condensation chamber are connected by a connecting tube that can be maintained at a temperature at which MgCl ₂ does not solidify, and has an externally operable valve for controlling vapor flow through the connecting tube, The chamber, the condensation chamber, and the connecting pipe are equipped with a means for evacuating the inside of the chamber, and the MgCl ₂ and Mg present together with the metal produced by the above reaction are vaporized and guided to the upper part of the condensation chamber, and are introduced into the chamber as a liquid phase or a solid phase. 1. A reduction and purification device for metal chlorides, characterized in that the metal chlorides are collected using a metal chloride. 2. It essentially consists of an outer cylinder with a closed lower end and an inner cylinder fitted with a bottom plate having a large number of perforations, and holds Mg molten inside and allows the Mg to be mixed with metal chloride supplied from the upper part of the inner cylinder. The reaction can precipitate the metal and produce by-product _MgCl2 and residual
A reduction evaporation chamber capable of vaporizing Mg, the upper part of which is essentially sealed with a removable lid, and a heating furnace disposed around the reduction evaporation chamber, which is provided adjacent to the reduction evaporation chamber and has the same structure as the inner cylinder. a condensing chamber containing a second inner cylinder and essentially sealed by a removable top lid, cooling the second inner cylinder and containing MgCl ₂ and metal
It has a means for liquefying or solidifying Mg, and has a temperature controllable small chamber with a lid of the reduction evaporation chamber installed inside, and a steam exhaust hole provided around the small chamber separated from the small chamber. The reduction evaporation chamber and the condensation chamber are connected by a connecting tube that is connected at both ends to the discharge hole and the lid of the condensing chamber and can maintain the entire body at a temperature at which Mg and MgCl ₂ do not solidify, and the vapor flow through the connecting tube is controlled. It has a valve that can be operated from the outside for the purpose of removing metal chlorides from the Mg
was precipitated together with the metal produced by the reduction reaction.
MgCl ₂ and residual Mg are vaporized and guided to the open upper part of the second inner cylinder in the condensing chamber through a connecting pipe, and the metal chloride is deposited on the inner wall surface of the inner cylinder as a liquid or solid phase to be recovered. Equipment for reducing and refining things.