JPS6131167B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for reducing metal chlorides. Among the metal materials, titanium and zirconium, which are high melting point and high toughness metal materials, are mainly produced by reducing their chlorides with magnesium, and are first obtained in the form of metal sponges.

Currently, the production of sponges made of high-melting-point, high-toughness metals uses a reaction apparatus consisting of a sealed reaction chamber that can be heated and a condensation chamber that can be cooled and degassed above the reaction chamber. Magnesium and metal chloride are produced in the reaction chamber. (for example, titanium tetrachloride), the resulting liquid magnesium chloride and the sponge-like metal are separated, and then the magnesium chloride and unreacted magnesium are removed from the sponge-like metal under reduced pressure (vacuum separation). , by an operation in which magnesium chloride and magnesium are recovered by cooling in a condensing chamber.

Such an apparatus is disclosed, for example, in Japanese Patent Application Laid-Open No. 18717/1983, but the problem with this type of apparatus is how to communicate and shut off the lower reaction chamber and the upper condensation chamber. The above-mentioned device has a mechanism in which the passageway in the intermediate connection connecting the reaction chamber and the condensation chamber is blocked by a shielding lid, but this mechanism is complex and, in particular, high temperature magnesium vapor and magnesium chloride vapor are generated near the shielding lid. As it passes through, it is deformed by thermal strain,
The drawback is that it gradually becomes impossible to seal completely.

JP-A-52-49922 discloses a similar device,
A partial improvement of the above-mentioned drawbacks is disclosed. In this device, instead of the shielding lid, a metal plate made of an easily fusible metal, such as magnesium, aluminum, zinc, or antimony, is bolted to the intermediate connection, thereby blocking the passage through the intermediate connection during the reduction reaction. During vacuum separation, the connecting portion passage is opened by melting it away using a heating device provided at the connecting portion. Although this device eliminates the drawbacks of the previously cited devices, it is not satisfactory in terms of operation and economy, since a smooth, polished plate of easily meltable metal must be prepared and used anew each time. It's tough.

In both of the above-mentioned devices, the reaction chamber and condensation chamber are difficult to separate easily, so when taking out the reaction chamber from the heating chamber, the condensation chamber must be lifted and moved with a crane, etc. As equipment capacity continues to increase, inconveniences such as an increase in crane capacity, a significant rise in construction costs due to an increase in building height, and an increase in work space for disassembling and assembling equipment are increasing. .

The present invention provides an apparatus in which a reaction chamber and a condensation chamber for reducing chlorides of high-melting-point, high-toughness metals are connected and integrated at an intermediate connecting section, and a seal pot structure is used as means for blocking passages in the intermediate connecting section. By adopting the present invention, the aim is to overcome the drawbacks of devices of the prior art and to further improve the functionality of devices of this kind.

According to the present invention, for reducing a chloride of a high melting point high toughness metal with an active metal to obtain the metal,
A device consisting of a reaction chamber that can be heated, a condensation chamber for vacuum separation of the chloride produced, and an intermediate connecting part for communicating the two: A funnel-shaped body and its opening are installed in the intermediate connecting part. There is provided an apparatus characterized in that it is provided with a means for blocking a seal pot structure made of an easily melting and easily evaporating substance, which is comprised of a pot that receives a leg part, and a heating means for melting and vaporizing the easily melting and easily evaporating substance.

The term "seal pot" used herein has the same structural meaning as the conventional meaning (liquid-sealed tank), but is different from the conventional term in that it uses a room-temperature solid substance that melts easily and evaporates as a sealant. The meaning is somewhat different. The sealant used in the present invention can be metals such as magnesium, aluminum, zinc, antimony, magnesium chloride, sodium chloride, potassium chloride, and mixtures thereof, but it is said that perfect sealing properties can be expected. From this point of view, the above metals are preferable, and among them, high melting point and high toughness metals (titanium, zirconium, etc.)
The use of metallic magnesium is the most desirable since it does not contaminate the metal.

In the device disclosed in JP-A-52-49922, after vacuum separation, it is no longer possible to shut off the intermediate connection without disassembling the device. Therefore, since the condensing chamber cannot be desorbed without allowing outside air to enter, each condensing chamber must be lifted in order to cool the reactor. Although the device of JP-A-47-18717 is theoretically capable of removing the condensing chamber, it has the drawbacks mentioned above. The device of the present invention overcomes both of these disadvantages.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the apparatus of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a longitudinal sectional view showing the mechanism of the device of the present invention. The reaction chamber is a reaction retort 10 serving as an outer container.
It consists of an inner container 20 supported by a support body 21 and housed therein.

The retort may have any shape, but in practice it is cylindrical, with the inner container being a cylinder slightly smaller than the retort, with at least one small hole in the bottom for draining molten magnesium chloride. There is an opening/closing means 14 such as a valve for discharging magnesium chloride at the bottom of the retort.
A conduit 13 is provided having a diameter. A flange 11 is formed at the upper end of this retort, and a collar 12 is further provided for suspending the retort in a heating furnace, which will be described later.

The intermediate connection 30 essentially consists of a cylindrical body 31 having a smaller diameter than the inner vessel 20 of the reaction chamber, from the upper part of which projects a wide flange 32 and from the lower end a collar 33, which extends into the latter. A circumferential wall 34 is formed that extends upward from the cylindrical body 31 and is lower than the cylindrical body 31. The flange 3
5 is sticking out. This flange 35 is configured to overlap with the flange 11 of the retort. The diameter of the collar 33 at the lower end of the intermediate joint is:
Slightly smaller than the inner diameter of the retort, retort 1
It is large enough to fit into the inside of the 0 and come into contact with its inner wall.

Further, the height of the inner container 20 of the retort is
The upper edge thereof should be in contact with the lower surface of the collar 33 at the lower end of the intermediate connecting portion. Thus, although the periphery of the lower end collar 33 and the inner wall of the retort are not in close contact with the lower end collar 33 and the upper edge of the retort inner container 20, the free passage of the reaction gas within the inner container is prevented. ing.

The flange 35 of the intermediate joint portion and the flange 11 of the retort are removably fixed with bolts, clamps, etc. with a gasket interposed therebetween. The gasket may be made of known heat resistant elastomers.

The condensing chamber consists of a cooling chamber 40 having a jacket structure and a shape similar to a retort, and a condensing cylinder 50 housed inside the cooling chamber 40. The cooling chamber 40 has an exhaust port 41 and an inlet 4 for introducing cooling liquid (water) into the jacket.
2. A discharge port 43 is provided, and the lower end is a flange 44 similar to a retort. The condensing cylinder 50 is a cylindrical container that is slightly smaller than the cooling chamber, and has at least one hole in the ceiling to allow gas to pass through. Its lower end is a flange 52 similar to the cooling chamber. Cooling chamber 40 and condensing cylinder 50
is fixed by sandwiching a gasket between the flanges 44 and 52, and these two are further overlapped on the flange 32 of the intermediate connecting portion 30 via the gasket,
It is removably fixed with bolts, etc. However, normally the cooling chamber 40 and the condensing cylinder 50 are treated as one unit as a condensing chamber. The gasket in this part may also be made of a known heat-resistant elastomer.

In the intermediate connecting portion 30, a low cylindrical container (pot) 36 is supported at the center of the cylindrical body 31 by a support rod 37 from the peripheral wall. A funnel-shaped body 38 is provided above the pot 36 so as to face the pot, the upper end of the conical part is closely fixed to the inner periphery of the intermediate connecting part, and the lower end of the tubular leg is closer to the upper edge of the peripheral wall of the pot. It's invading below. The structure of this seal pot is illustrated in more detail in FIGS. 2 and 3.

Usually, this intermediate connecting portion 30 is provided with a conduit 61 for introducing a chloride of a desired metal, an inert gas, etc., and a conduit 62 for exhaust. Although these conduits may be provided in the body of the retort 10, it may be more convenient to provide them at this intermediate connection.

These conduits have a valve not far from the intermediate connection so that they can be removed from the parent pipe outside the valve. In FIG. 1, the right conduit is divided into a branch pipe for introducing metal chloride and a branch pipe for introducing inert gas, etc., each of which is provided with a valve.

A conduit 39 is provided above the funnel-shaped portion 38 of the intermediate coupling portion 30 for introducing a melt 80 of sealing material into the pot. A heating means, conveniently an electric resistance heating means 70, is provided on the outside of the intermediate connecting portion 30 and the outer periphery of the sealing material introducing conduit 39.

The reaction chamber, inner container, cooling chamber, condensing tube, and intermediate connection part can all be made of mild steel or stainless steel. However, in the case of titanium production, the inner container is made of mild steel because the produced titanium sticks to the container and the container becomes disposable.

Retort 10 is housed in a suitable heating device 90. A suitable heating device is of the electrical resistance type. This heating device has an opening for the magnesium chloride discharge pipe of the retort 10. This heating device can be appropriately designed by a person skilled in the art, so it will not be described in detail.

It is convenient for the heating means of the intermediate connection to consist of a plurality of semi-cylindrical (if necessary one-third cylindrical) units applied from both sides. The shape of the intermediate connection part should be made simple.
That is, the retort collar 12 is omitted and the flange 1
1 can be lowered to the position of the collar 12, and the intermediate connection part can be simply on a reel. However, in this case a means of cooling the interposed gasket would be required. It is also desirable to provide a heat insulating plate spaced below the seal pot and supported by suitable support means to prevent heat from the reaction chamber from directly reaching the seal pot.

In the apparatus of the present invention, the inner container of the reaction chamber is necessary only when the spongy metal produced tends to adhere and accumulate on the side wall of the reaction chamber, as in the case of titanium. This tendency is not necessary in the manufacture of metals as is the case.

The method of operating this device is as follows. After charging the internal container 20 of the retort with the magnesium mass, the flanges 11 and 35 are fixed, the intermediate connections are connected, and then the condensation chamber (40+50) is fixed and the whole device is assembled. The condensation chamber is fixed after the reaction chamber (including the intermediate connection) has been installed in the heating device 90. After assembling the device, the conduit 41 is evacuated and a leakage test is performed.

After confirming airtightness, exhaust air from the exhaust pipe 41,
Inert gas is filled into the entire apparatus through conduit 61 to a pressure slightly higher than atmospheric pressure. Next, a melt 80 of the sealing material is introduced into the pot 36 through the conduit 39 and solidified. Next, the heating furnace 90 is operated to heat the retort to melt the previously charged magnesium, and then metal chloride is introduced from the conduit 61 to carry out the reaction to obtain a sponge-like metal, and the produced magnesium chloride is It is discharged from the conduit 13.

Next, after closing the opening/closing means 14 of the conduit 13, electricity is applied to the heating device 70 of the intermediate connection part 30 to heat the sealing pot, melting the sealing material therein, and then degassing the conduit 41 to release the sealing material. evaporate.
However, since the condensing chamber is cooled by the cooling liquid in the cooling chamber, substantially all of the vapor of the sealing material solidifies on the inner surface of the condensing tube 50. In this state, the reaction chamber and the condensation chamber are in communication. Therefore, if the reaction chamber is continued to be heated in this state, both the magnesium chloride incorporated in the sponge-like metal and unreacted magnesium will be vaporized, separated from the metal, and collected in the condensing column 50.

When the vacuum separation process is completed, the pressure inside the apparatus is restored with argon, and the molten sealing material is again introduced into the pot 36 through the conduit 39 and solidified. At this time, in order to prevent contamination of the sealing material of the formed metal by vapor, it is preferable to carry out the process while flowing a small amount of argon through the conduit 61. After blocking the reaction chamber and the condensation chamber in this way, it is desorbed from the condensation chamber and the intermediate connection part.
Only the reaction chamber (including the intermediate connecting part) is taken out from the heating furnace and cooled, and after cooling, the produced metal sponge is taken out. Thus, one batch operation is completed.

For the next batch operation, after charging the magnesium lump into the inner container of the reaction chamber, the passage of the intermediate connection part has already been blocked, so assemble the apparatus as it is, and open the conduit 62 to drain the air inside the reaction chamber. Inert gas is sent from 61 for substitution. In this way, the next batch operation can be performed.

EXAMPLE An example of a device assembled by the inventors in accordance with the present invention is as follows.

The reaction chamber and condensation chamber both have an outer diameter of 700 mm and a height
It was 1760mm bell-shaped, and the cylindrical body at the intermediate joint had a length (height) of 370mm and an inner diameter of 185mm.

The reaction chamber and the intermediate joint (including the seal pot part) are made of chromium-containing steel.The reaction chamber and the intermediate joint part to be heated have a wall thickness of 25 mm, and the seal pot part is made of 5 mm thick material. 125
mm, and the height was 40 mm. The cooling chamber and condensing tube of the condensing chamber were made of 10 mm thick mild steel.

The inner vessel of the reaction chamber was made of mild steel.

Working Example 1 Titanium was produced according to the procedure described above. First, 350 kg of solid magnesium was charged into the inner container of the reaction chamber, and argon was introduced into the apparatus as an inert gas so that the internal pressure inside the apparatus was higher than atmospheric pressure. Next, metal magnesium is used as a sealing material to block the passage in the intermediate connection, and the retort is heated to 800-850°C to melt the charged magnesium, and about 1025 kg of titanium tetrachloride is heated to the temperature inside the retort. The reaction was carried out by dropwise introduction so as not to increase too much. After the reaction is complete, the produced magnesium chloride is discharged from the retort, and then the magnesium in the seal pot is melted and evaporated while flowing argon. The reaction chamber is then heated to 1000°C and vacuum separation is carried out for about 30 minutes.
Vacuum separation was completed over a period of time.

The seal pot was again filled with magnesium and solidified, the condensation chamber was removed, and the reaction chamber (including the intermediate connecting part) was taken out from the heating device, cooled, and opened to obtain about 250 kg of titanium sponge.

Working Example 2 Zirconium was produced according to the procedure described above. The inner vessel of the reaction chamber was not used.

Approximately 50 kg of magnesium was charged into the retort.
As the sealing material, metal magnesium was used as described above. Heat the retort to 800-850℃, approx.
Kg of zirconium tetrachloride was introduced into the retort.
The passage in the intermediate connection was opened in the same manner as above, and then the retort was heated to 900-950°C and the vacuum separation process was continued for about 20 hours to complete the vacuum separation. After that, the same process as in the case of titanium was carried out to obtain about 80 kg of sponge zirconium.

The present invention provides a system for reducing chlorides of high melting point, high toughness metals that is more convenient to use than known systems. To date, this equipment is useful for the production of titanium and zirconium, but a similar metal production process has been developed that involves reduction of chloride with active metals (sodium, calcium, etc. in addition to magnesium). It will be recognized by those skilled in the art that this device could be applied in any case.

[Brief explanation of the drawing]

FIG. 1 is a longitudinal sectional view showing the concept of the apparatus of the present invention. FIGS. 2 and 3 are a sectional view and a plan view showing an enlarged seal pot portion of the device of the present invention.
(Figure 3 is a plan view of the section cut at the position of member 39 in Figure 2.) In these figures, 10+20...reaction chamber,
40+50... Condensing chamber, 30... Intermediate connection part, 3
6+37+38...Seal pot.

Claims (1)

[Claims] 1. A reaction chamber that can be heated to obtain the metal by reducing the chloride of a high-melting-point, high-toughness metal with an active metal, and a condensation chamber for vacuum-separating the produced chloride, and both of these. In a device comprising an intermediate connecting part for communicating: a means for blocking a seal pot structure with an easily melting and evaporating substance consisting of a funnel-shaped body and a pot receiving the open leg of the intermediate connecting part; An apparatus characterized by being provided with heating means for melting and vaporizing an evaporated substance.