JPH03140424A - Method and device for producing metal high in melting point and toughness - Google Patents

Abstract

PURPOSE:To completely absorb the thermal expansion of a duct with a simple structure and to accurately control the mass of the residue in a reduction vessel by allowing one between the reduction vessel and condensation vessel in parallel to each other with the duct to follow the thermal expansion of the duct and supporting the other through a weight sensor. CONSTITUTION:The reduction vessel 10 and a heating furnace 20 are supported through a load cell 16, the condensation vessel 30 is set in a cooling furnace 40 and supported on a rack along with the furnace 40 through an air spring 60. At this time, the vessel 30 and furnace 40 are positioned at the neutral point of the spring 60 when the duct 70 is thermally expanded. The vessel 30 and furnace 40 are drawn toward the vessel 10 in consideration of the expansion of the duct 70, and the upper ports of the vessels 10 and 30 are connected with the horizontal duct 70. When the unreacted active metal and chloride remaining in the spongy metal formed in the vessel 10 are recovered in the vessel 30 by vacuum separation, the weight change of the vessel 10 is detected by a sensor 16. The progress of recovery is estimated from the change.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an apparatus for producing high-melting-point, high-toughness metals such as Ti and Zr by reductive separation, and a method for producing high-melting-point, high-toughness metals using the apparatus. .

[Conventional technology]

High-melting-point, high-toughness metals such as Ti and Zr are produced by an industrial reduction method using the chloride of G.

In the production of high-melting-point, high-toughness metals using reduction methods, reduction vessels and condensation vessels have traditionally been used, and recently equipment configurations in which both are placed side by side and interconnected through horizontal conduits have been increasingly adopted. .

In such production equipment, after a high melting point and high toughness sponge metal is produced in a reduction vessel, the unreacted active metal and its chloride remaining in the sponge metal are vacuum separated, and the material is passed through a conduit. Collected in a condensation vessel. When the vacuum-separated substance is collected in a condensation vessel, the conduit is heated in order to prevent the vacuum-separated substance from solidifying within the conduit, but thermal expansion of the conduit due to the heating cannot be avoided. The extension of the conduit due to this thermal expansion is several hundred meters or more in large equipment, and the reduction vessel and iii? This is a major problem in devices that are connected to containers using horizontal conduits. Therefore, absorbing the thermal expansion of the conduit is an important issue in this type of equipment, and specific measures for this purpose include:
JP-A-59-80593 discloses a connection structure in which a conduit is divided in the middle and a gap is provided between the conduits.

[Problem to be solved by the invention]

However, in the above connection structure, thermal expansion of the conduit in a small device can be absorbed by the gap, but in a large device the thermal expansion can be absorbed by several centimeters.
The elongation of the conduit exceeding this amount is hardly absorbed. Therefore,
Stress is concentrated at the interconnections of the conduits and the connections between the conduits and the container, which can cause cracks to form at these connections. Furthermore, the gasket for sealing the gap requires cooling means. Since this cooling is performed in parallel with the heating of the conduit, it is technically difficult, leads to a complicated connection structure, and is hardly practical.

In addition, when recovering unreacted active metals and their chlorides remaining in the high-melting-point, high-toughness spongy metal generated in the reduction vessel into the condensation vessel, the product quality will deteriorate as the amount of residue in the reduction vessel increases. However, if the vacuum separation process is performed more than necessary, the amount of electricity used will increase and the economic efficiency will decrease. Therefore, it is necessary to accurately control the final amount of residual substances in the reduction container. However, conventionally, there has been no quantitative detection method for the amount of residual substances in the reduction container.

Therefore, the processing time for separation and recovery is statistically determined based on changes in the power consumption of the furnace and empirical time calculations, resulting in the problem that the amount of residual substances is not constant.

The present invention was developed in view of this situation, and it has a simple structure that can completely absorb the thermal expansion of the conduit, and also allows quantitative progress of the separation and recovery reaction when separating and recovering residual substances in the reduction vessel. It is an object of the present invention to provide an apparatus and method for producing a high-melting-point, high-toughness metal that can be estimated and separated and recovered in an appropriate time.

[Means to solve the problem]

The production apparatus of the present invention includes a reduction container for reducing a chloride of a high-melting-point, high-toughness metal to be produced with an active metal to produce a high-melting-point, high-toughness sponge-like metal, and a sponge-like metal produced in the reduction container. and a condensation container for recovering unreacted active metals and their chlorides remaining in the reactor by vacuum separation, and the condensation container is arranged side by side with the reduction container, and both are integrally connected by a conduit. In addition, one of the reduction vessel and the condensation vessel is supported so as to be able to follow the thermal expansion of the conduit, and the other is supported via a weight sensor.

In the production method of the present invention, when the unreacted active metal and its chloride remaining in the sponge-like metal generated in the reduction vessel are recovered into the condensation vessel by vacuum separation, the The feature is that the weight change of the container is detected and the progress of the separation and recovery reaction is estimated from the detected weight change.

[For production]

In the manufacturing apparatus of the present invention, one of the reducing vessels and the condensing vessel is entirely driven by the thermal expansion of the conduit, so even if both vessels are integrally connected by the conduit and worn out, the conduit expands thermally. is absorbed. Therefore, the entire conduit can be constructed in one piece, making it easy to heat the conduit, and eliminating the need for a packing and its cooling mechanism, thereby significantly simplifying the conduit and its ancillary mechanisms. In addition, the thermal expansion of a conduit is affected by the amount and temperature of the material recovered through the conduit, and exhibits complicated elongation, but when thermal expansion is absorbed by a container,
The container can accurately follow the complicated elongation of the conduit and reliably absorb the elongation.

Furthermore, since the other container is supported via a weight sensor, when the residual substance in the reduction container is separated and recovered, if the weight sensor detects a change in the weight of the container, the progress of the separation and recovery reaction can be monitored. Can be estimated quantitatively. That is, 1.
By measuring the change in the weight of the reduction container, the amount of the residual substance remaining in the reduction container can be measured, and by measuring the change in the weight of the condensation container, the amount of the residual substance recovered into the condensation container can be measured.

The manufacturing method of the present invention quantitatively estimates the progress of the separation and recovery reaction by detecting changes in the weight of the container supported by a weight sensor during separation and recovery. Allows collection processing time to be set.

In the manufacturing apparatus and method of the present invention, either the reduction vessel or the condensation vessel is movable to absorb thermal expansion, but in actual operation it is desirable that the condensation vessel side is movable. This is because, in the separation and recovery process, the weight of the contents in the condensation container is lighter than that in the condensation container, making it easier to move the container, and the heating state of the reduction container may change if it is moved.

As a specific means for making the container movable, it is desirable to directly or indirectly support the container with a fluid spring. When the container is supported by a fluid spring, the container moves with a slight external force, further relieving stress on the conduit, and even if the weight of the container changes as the recovery process progresses, the fluid pressure can be adjusted. This makes it easy to keep the container at a constant height.

Examples of the weight sensor include electrical means such as load cells and strain gauges, as well as mechanical means that directly measure changes in the weight of the container.

〔Example〕

Examples of the present invention will be described in detail below regarding the production of Ti.

FIG. 1 is a sectional view showing an example of a manufacturing apparatus embodying the present invention.

The reduction container 10 is housed in a heating furnace 20.

At the upper opening of the reduction container 10 is an inlet pipe 11 for Ticl, a.
is connected, and a by-product discharge pipe 11 is connected to the bottom. A load cell 16 as a weight sensor is interposed between the lower surface of the flange portion 15 that supports the reduction container IO in the heating furnace 20 and the upper surface of the heating furnace 20.

The condensation vessel 30 is housed in the cooling furnace 40 and has the same structure as the reduction vessel 10 and is used interchangeably. The cooling furnace 40 is supported in a floating state via an air spring 60 on a cylindrical pedestal 50 arranged in parallel with the heating furnace 20, and further includes a level gauge. air spring 6o
is an annular air bag connected to an air supply device (not shown). The air supply device adjusts the air pressure applied to the air spring 60 based on the output of the level meter to keep the height of the cooling furnace 40 constant.

The upper opening of the reduction vessel 10 and the upper opening of the condensation vessel 30 are connected by a horizontal conduit 70. The conduit 70 is removably connected to both openings, and its outer peripheral surface is covered with a heater 71. A valve 7 is provided between the conduit 70 and both openings.
It will be opened and closed at 2.73.

In order to produce Ti using such production equipment, a reduction vessel l
O is set in the heating furnace 20 via the load cell 16, and the condensing vessel 30 is set in the cooling furnace 40.
0 is supported on a pedestal 50 by an air spring 60. At this time, the condensing vessel 30 and the cooling furnace 40 are connected to the conduit 70.
is set to be located at the neutral point of the air spring 60 in a thermally expanded state. Then, the condensation vessel 30 and the cooling furnace 40 are drawn toward the reduction vessel 10 by an amount corresponding to the expansion of the conduit 70, and the reduction vessel 10 and the condensation vessel 30 are connected by the conduit 70.

Next, the heating furnace 20 is operated with the valves 72 and 73 closed to maintain molten Mg in the reduction vessel IO, and TiC1 is introduced from the introduction pipe 11.

As a result, Ti and MgCN□ are generated within the reduction container 10. The generated Mg(l□) is appropriately discharged to the outside from the discharge pipe 12. Finally, spongy Ti containing unreacted Mg and MgClt is obtained.

When the reduction process is completed, after opening the valves 72 and 73, the temperature of the heating furnace 20 is raised to 1000°C or higher, and the conduit 70 is heated with the heater 71 to a temperature at which Mg and MgCl do not condense.
Heat it up. Furthermore, while cooling the condensing vessel 30 within the cooling furnace 40, the inside of the condensing vessel 30 is evacuated using the exhaust pipe 32. As a result, the spongy Ti in the reduction container IO
Unreacted Mg and MgCff1. evaporates,
It is collected via conduit 70 into condensation vessel 30 .

In this separation and recovery step, the conduit 70 is expanded by heating by the heater 71 and extends in the axial direction. However, as the condensation vessel 30 expands, the reduction vessel 10 along with the cooling furnace 40
The condensing vessel 30 and the cooling furnace 40 return to the neutral point of the air spring 60 by moving away from the air spring 60 and by canceling out the amount of movement that was drawn toward the heating furnace 20 in advance.

Therefore, no problematic stress occurs in the conduit 70 or the connection between the conduit 70 and the container.

Further, as Mg and MgCC are collected and collected in the condensation vessel 30, the weight of the condensation vessel 30 increases, and the load applied to the air spring 60 increases, but the height of the condensation vessel 30 is kept constant. Since the air pressure of the air spring 60 increases, the reduction vessel lO and the condensation vessel 30 are always kept at the same level. Therefore, stress generation due to the inclination of the conduit 70 is also prevented.

In the production method of the present invention, the change in weight of the reduction vessel IO is measured by the load cell 16 in such a separation and recovery step of Ti production. The weight of the reduction container 10 is determined by the amount of Mg escaping from the spongy Ti inside it and the amount of Mg
It decreases according to C12tT. Therefore, by measuring the weight change of the reduction container IO, Mg and MgCjl
! The amount of recovered nuclear power plant z is detected quantitatively. From this change in the amount of evaporation recovery and the change in the amount of electricity used compared to the conventional amount, the trends in the amount of unreacted Mgtt and Mg (12) contained in the spongy Ti in the reduction vessel IO were clarified, and the optimal separation was determined. The recovery processing time can be determined.As a result, the amount of Mg remaining in the Ti sponge and the amount of MgCl
The amount of processing is sufficiently reduced, and wasteful processing time is also reduced, leading to savings in power consumption.

Table 1 shows the amount of power used and the amount of residual substances in the Ti sponge for the conventional method and the method of the present invention. When the conventional power usage is set to 100, the power usage is reduced to 90 in the method of the present invention, and the variation in the chlorine content of the Ti sponge is also greatly reduced.

Table 1 It is between men.

In the figure, 1O: reduction container, 16: weight sensor, 20: heating furnace, 30: condensation container, 40: cooling furnace, 50: frame, 60
: Air spring, 70: Conduit.

Applicant: Osaka Titanium Manufacturing Co., Ltd. [Effects of the Invention] The manufacturing apparatus and method of the present invention reliably absorb thermal expansion of the conduit, which becomes a problem when a reduction vessel and a condensation vessel are placed side by side and integrated. This prevents cracks and damage to the connecting parts and extends the life of the device.

In addition, the entire conduit can be integrated, and there is no need to interpose gaskets in the middle of the conduit, so the structure of the conduit is simplified.
Its heating is facilitated and clogging of the conduit starting from the connection is prevented. Furthermore, the separation and collection time of residual substances is optimized, thereby achieving reductions in power consumption and improvement in product quality.

[Brief explanation of the drawing]

Claims (2)

[Claims] (1) A reduction vessel in which the chloride of the high-melting-point, high-toughness metal to be produced is reduced with an active metal to produce a high-melting-point, high-toughness sponge-like metal, and any residue remaining in the sponge-like metal produced in the reduction vessel. It is equipped with a condensation container for recovering reactive metals and their chlorides by vacuum separation, and the condensation container is arranged side by side with the reduction container, and both are integrally connected by a conduit. Either the vessel or the condensing vessel is
supported so as to be able to follow thermal expansion of the conduit;
A high melting point high toughness metal manufacturing apparatus characterized in that the other side is supported via a weight sensor. (2) When the unreacted active metal and its chloride remaining in the spongy metal generated in the reduction container are recovered into the condensation container by vacuum separation, the weight of the container supported via the weight sensor changes. is detected by the weight sensor, and the progress of the separation and recovery reaction is estimated from the detected weight change of the container.