JPS5940895B2 - Metal zirconium production equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides a method for reducing zirconium halides, such as reducing zirconium tetrachloride with metallic magnesium.
The present invention relates to an apparatus for producing metallic zirconium that produces zirconium sponge using a reducing agent made of an alkaline earth metal.

The present applicant previously proposed a technology for manufacturing zirconium sponges in Utility Application No. 129871/1987, but this proposed technology involves forming operating pipes in the bodies of the reaction vessel and condensation vessel, and using the process as a reaction vessel. The operation pipe of the container used as a condensation container is used as a pipe for charging the molten reducing agent and the extraction of the molten salt produced as a by-product, and the operation pipe of the container used as the condensation container is used as a pipe for exhaust.・This simplifies the work of reusing both containers and improves work efficiency.

The present invention is a further development of the above-mentioned proposed technology, and the feature of the present invention is that the central cylinder is attached to the side of an intermediate partition stand provided with a central cylinder that communicates between the reaction vessel and the condensation vessel. A branch cylinder is provided which communicates with the central cylinder, and a feeder for supplying zirconium halide and a damper for opening and closing the central cylinder are configured to be replaceable in the branch cylinder.

Therefore, the object of the present invention is to close the central cylinder that communicates the reaction vessel and the condensation vessel with a damper and integrate the two vessels and the partition stand before disassembly operation after the reduction operation and separation operation are completed. By rotating the container 180 degrees in the current state, the joint between the container and the partition stand, which had previously been used as a condensation container, can be used as a reaction container in the next operation without disassembling it, greatly reducing the disassembly and assembly work. It is an object of the present invention to provide an apparatus for producing metallic zirconium that can reduce the amount of production.

Hereinafter, the present invention will be specifically explained based on an illustrated embodiment.

The manufacturing apparatus of the embodiment includes a reaction vessel 20 and a condensation vessel 30 which are formed of equal-shaped vessels and are vertically symmetrically opposed to each other, and an intermediate partition 1 interposed between both the vessels 20 and 30. , a heating furnace 17 surrounding the outer periphery and bottom of a reaction vessel 20, and the inner spaces of these vessels 20 and 30 constitute a reaction chamber 2 and a condensation chamber 3, respectively.

The partition stand 1 is formed of a substantially cylindrical heating furnace 4, and the partition stand 1 is formed with a central cylinder 5 that vertically communicates with the central part, and a central cylinder 5 is formed so as to surround the outer peripheral part of the central cylinder 5. A sheathed heater 6 is embedded within the heating furnace 4.

Further, in the center of the central cylinder 5, a branch cylinder 7 is formed to protrude and communicate with the central cylinder 5 and extends to the outside of the side of the partition table 1, and this branch cylinder 7 is provided with halogen by a screw conveyor or the like. A feeder 8 or a damper (pulp body) 9 for supplying zirconium chloride is attached in a removable manner,
Small-diameter temperature and pressure detection tubes 16, 16 are formed parallel to the branch tube 7 at positions near the top and bottom of the branch tube 7, and these temperature detection tubes 16, 16 are communicated with the central tube 5. .

Additionally, above and below the partition stand 1 are stepped portions 10a and 10b.
Relatively large diameter recesses 11, 11 are formed at the center of the upper and lower end surfaces of the partition 1, and approximately in the middle of the internal space of the recess 11 is the center. Upper and lower ends 5a and 5b of the cylinder 5 are positioned.

Flanges 12, 12 are formed on the tips 5a and 5b, and a fusible contact plate 13 is attached to the upper 7 flange 12 of the flanges 12 and 120. It is placed and fixed so as to close the inner space, and a plate made of magnesium material is normally used as the touch plate 13.

Further, one end of a temperature detection tube 15 is opened at the upper end surface and the lower end surface of the partition table 1, and the other end of this temperature detection tube 15 is projected to the outside of the partition table 1.

On the other hand, each container 20°300 made of heat-resistant steel plate has a large-diameter dish-shaped flange 2L31 at the open end facing each other.
A peripheral wall 21a, 31a protruding toward each container 20, 30 is formed on the outer periphery of the dish-shaped flange 21.31, and a drain pipe 22.32 is formed at one location of the peripheral wall 21a, 31a. In addition to being fixed, bankings 23, 33 are extended on the sides of the dish-shaped flange 2L31 from which the peripheral walls 21a, 31a protrude.

Thus, the reaction vessel 200 and the flange 21 are brought into close contact with the upwardly opening end surface of the heating furnace 17 via the backing 23, so that the inner hole 17a of the heating furnace 17 is sealed, and the inner peripheral edge of the flange 21 is sealed. The lower part of the partition stand 1 is fitted and fixed into the reaction vessel 20 so that the partition stand 10 and the step part 10b of the partition stand 10 are in close contact with each other.

Furthermore, a condensation container 30 is placed over the top of the partition 1, and the inner peripheral edge of the flange 31 of the condensation container 30 and the step 10a on the upper side of the partition 1 are fixed in close contact with each other. The drain pipe 32 of the flange 31 functions to drain water in cooperation with a sprinkler pipe, which will be described later.

Further, on the circumferential wall of each container 20, 30 near the bottom in the middle of the body, there is an operating pipe 26, 36 consisting of straight pipes 24, 34 and L-shaped pipes 25, 35 branched from the straight pipe 24°34. The L-shaped tube 25.35 is open to the container 20.35.
It extends along the outer wall of the container 20, 300 toward the open side, and passes through the husband's flanges 21, 31, with its outer ends 27 and 37 protruding to the outside.

The outer end 27 of the L-shaped tube of the reaction vessel 20 is connected to an MgCl2 reservoir (not shown) and a connecting tube 18 which communicates selectively with the Mg melting furnace. Exhaust pipe 1 leading to the working vacuum pump
9.

In addition, the exhaust pipe 19 is provided with an operating valve 50, and the straight pipe 24 of the reaction vessel 20 and the outer end 3 of the L-shaped pipe of the condensation vessel 30 are interposed in the exhaust pipe 19.
7 is closed with a blind lid.

In addition, an air passage pipe 51 is fixedly installed on the peripheral wall of the heating furnace 170 to make the internal pressure of the furnace inner hole 17a a negative pressure in order to prevent deformation due to internal pressure fluctuations in the reaction vessel 20. This passage pipe 51 is also used for cooling separately.

In addition, a cooling water sprinkler pipe 53 is provided near the top of the condensation container 30.
And the cover is installed.

On the other hand, the damper 9 has a substantially cylindrical shape as shown in FIG. It is said to be semicircular, matching the curvature.

Further, near the end of the damper 9 on the valve body 90 side, there is a tapered part 91 having a smaller diameter on the end side.
1 is filled with a heat insulating material 92, a heater 93 is embedded in the heat insulating material 92 near the valve body 90, and an operation bundle 94 is formed at the other end of the valve body 9. A portion of the bundle 94 includes a rotational positioning guide 9.
4a is formed.

Here, the handling and operation of the embodiment manufacturing apparatus configured as above will be explained.

First, after confirming the airtightness of each part of the reaction vessel 20 and condensation vessel 30 in the coupled state by a pressure test, the reaction vessel 20 is inserted into the heating furnace 17 and coupled.

Next, the heating furnace 17 is energized or ignited to a temperature of 200°C to 30°C.
While preheating to 0°C, absorption and degassing are performed, and then Ar is passed through the reaction chamber 2 from the adjustment tube 15 until atmospheric pressure is reached, and the temperature inside the furnace is further raised to 750°C to 800°C. .

Thereafter, 80 kg of molten Mg is charged into the reaction chamber 2 through the operation pipe 26, and then ZrCl4 is passed through the feeder 8 and brought into contact with the molten Mg in the reaction chamber 2 to perform a reduction reaction.

However, when 700 kg of ZrCl4 reacted,
The Ar in the reaction chamber 2 is pressurized to 0.5 kg/cm, thereby the by-produced MgC1□ is extracted from the operation pipe 26, 80 kg of Mg is charged again, and ZrCl4
pass through and continue the reaction.

After charging 280 kg of ZrCl, MgCl2 was extracted.

Note that during this operation, the heater 6 is not energized, so that the partition plate 1 located away from the reaction vessel 20 is not catalyzed.

Next, after repeating the reaction operation cycle as described above three to five times, the feeder 8 is extracted from the branch pipe 7, and a damper 9 is attached to the branch pipe 7 in place of the feeder 8.

At this time, the valve body 90 of the damper 9 is kept in a state parallel to the axial direction of the central cylinder 5 as shown in the third diagram, and the temperature of the heating furnace 17 is raised again, and the sheathed heater 6 in the partition stand 1 is heated. Then, the partition plate 13 is melted.

This melting of the partition plate 13 brings the reaction chamber 2 and the condensation chamber 3 into communication.
This can be easily confirmed from the outside by measuring the pressure difference between and the condensing chamber 3.

After the above confirmation, the operation valve 50 is opened to start exhaustion, and the condensation vessel 30 is cooled by water spraying from the water sprinkler pipe 53. During this vacuum separation operation, the temperature of the reaction chamber 2 is kept at 900°C.
Keep it at ~1000°C.

During this period, the reaction chamber 2 operates as shown in Figure 4a.
The MgCl2 and Mg that evaporate from the condensing chamber 3 are deprived of heat and condense on the inner wall of the same chamber 3. This separation operation is completed in about 10 hours, and as a result of the above operation, about 800
kg of zirconium sponge can be produced.

Note that during the separation operation, the central cylinder 5 is heated by the sheathed heater 6, and the vicinity of the valve body 90 of the damper 9 is heated by the heater 93, so MgCl2 and Mg in the central cylinder 5 are condensed. It is reliably sent into the condensation chamber 3 without any problems.

After the separation operation is completed, the reaction vessel 20 is taken out from the heating furnace 17, and the damper 9 is moved as shown in FIG.
is rotated 90 degrees to close the central cylinder 5, and then the reaction vessel 20, condensation vessel 30, and intermediate partition 1 are rotated 180 degrees while being integrated.

The extraction operation of the reaction container 20 is carried out by lifting the container 20 with a crane or the like, or by lowering or disassembling the heating furnace 17, or the like.

In this way, the interior of the central cylinder 5 in the partition stand 1 is closed and has been used as the reaction vessel 20 until now, and the vessel in which the zirconium sponge is produced is positioned above, and has been used as the condensation vessel 30 until now. A container with MgCl2 and Mg adhered to the inner wall is positioned below.

Next, as shown in FIG. 4C, the container thus positioned above and used as the reaction container 2 until now is separated from the partition stand 1, and an empty container is placed on the partition stand 1 in place of this container. Place and fix it on.

During the separation/assembly of the containers, the container located below containing MgCl2 and Mg is placed under the damper 9.
This provides a seal with the outside air and prevents the crust from falling.

Next, as shown in FIG. 4d, the damper 9 and the feeder 8 can be replaced again to prepare for the next operation of the apparatus.

As explained above, according to the present invention, the middle part of the central cylinder is formed in the intermediate partition interposed between the reaction vessel and the condensation vessel, and serves as a passageway for communicating between the reaction vessel and the condensation vessel. A branch pipe is provided in communication with the central pipe, and a feeder for supplying zirconium halide and a damper for opening and closing the central pipe are installed in the branch pipe so that they can be exchanged, so that reduction and separation operations can be performed. Before the dismantling operation is completed, the central cylinder is closed off with a damper, and the reaction vessel, condensation vessel, and partition stand are rotated 180 degrees as a single unit, allowing the vessel to be used as a condensation vessel until now. without disassembling the joint between the and the partition stand.
This has the advantage that it can be used as it is as a reaction vessel during the next operation.

Therefore, it is possible to provide a metal zirconium manufacturing apparatus that can significantly reduce disassembly and assembly work.

Furthermore, since a large amount of Mg remaining in the condensing vessel acts as a new reducing agent in the reaction vessel, there is an effect of reducing the amount of reducing agent, and the ignitable Mg in the vessel is isolated from the outside air by the damper. This has the effect that there is no risk of combustion.

In addition, in conventional metal zirconium production equipment in which reduction and separation are generally carried out in the same furnace, a damper that closes the reaction vessel and the condensation vessel and a feeder for supplying zirconium halide are installed separately, resulting in a complex structure. be.

However, if the damper and the feeder insertion port for supplying zirconium halide are shared by the branch cylinder as in the present invention, the structure is significantly simplified and the maintenance of the apparatus can be reduced.

Since the time when this damper is used and the time when the feeder for supplying zirconium halide is used are different, there is no problem in operation.

Furthermore, unlike the feeders and dampers that are fixed, they can be removed, so they can be repaired at another location or replenished with zirconium halide.

When the reaction vessel, condensation vessel, and central cylinder are rotated as one unit as described above, the damper is simply inserted into the center of rotation, which has the effect of significantly facilitating the rotation operation.

[Brief explanation of the drawing]

Fig. 1 is a cross-sectional view of a metal zirconium manufacturing apparatus showing an embodiment of the present invention, Fig. 2 is an external view of a damper, and Fig. 3 shows the joint state of the branch pipe and the feeder, and the branch pipe and the damper. FIG. 4 is an explanatory diagram showing the operating state of the reaction vessel, the condensation vessel, and the partition stand. 1...Middle partition stand, 5...Central tube, 7
... Branch tube, 8 ... Feeder, 9 ...
...Damper, 20...Reaction container, 30.
...Condensation vessel.

Claims (1)

[Scope of Claims] 1. An apparatus for producing metallic zirconium by reduction of zirconium halide, which has a reaction vessel, a condensation vessel, and an intermediate partition with a central cylinder communicating between the vessels,
A metal metal characterized in that a branch tube connected to the center tube is provided on a side of the intermediate partition, and a feeder for supplying zirconium halide and a damper for opening and closing the center tube are replaceably installed in the branch tube. Zirconium production equipment. 2. The metal zirconium manufacturing apparatus according to claim 1, wherein the damper is equipped with a heater.