JPH0347929A - Method and apparatus for producing refractory metal with high toughness - Google Patents

Abstract

PURPOSE:To prevent the occurrence of crack and damage in a conduit and its connecting parts by a simplified structure by making a reduction vessel and a condensation vessel movable with the thermal expansion of a horizontal conduit in an apparatus in which the above vessels are placed side by side and integrated by means of the above conduit. CONSTITUTION:A reduction vessel 10 and a condensation vessel 30 are set in a heating furnace 20 and a cooling furnace 40, respectively, and the condensation vessel 30 is supported together with the cooling furnace 40 on a stand 50 by means of an air spring 60. At this time, the vessel 30 and the furnace 40 are set so that, in a state where a conduit 70 is thermally expanded, they are located at the neutral point of the spring 60. Subsequently, the vessel 30 and the furnace 40 are drawn toward the vessel 10 by the amount corresponding to the expansion of the conduit 70, and the vessel 10 is connected to the vessel 30 by means of the conduit 70. In the vessel 10, TiCl4, for example, is reduced by molten Mg to form Ti and MgCl2. Then, the furnace 20 is subjected to temp. rise and evacuation is performed through a tube 32 while heating the conduit 70 and cooling the vessel 30, by which unreacted substances contained in the sponsy Ti in the vessel 10 are evaporated and recovered into the vessel 30. In the above process, the conduit 70 is heated and expanded and, as a result, it is elongated in an axial direction. The vessel 30 is allowed to recede from the vessel 10 together with the furnace 40, by which the purpose can be accomplished.

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. .

(Prior Art) High melting point, high toughness metals such as Ti and Zr are industrially manufactured by a reduction method using their chlorides.

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, unreacted active metals and their chlorides remaining in the high-melting-point, high-toughness spongy metal produced in the reduction vessel are vacuum separated, and the substances are collected into the condensation vessel through a conduit. 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 elongation of the conduit due to this thermal expansion reaches several centimeters or more in large equipment, and is a major problem in equipment in which the reduction vessel and the condensation vessel are connected by a horizontal conduit. Therefore, absorbing the thermal expansion of the conduit is an important issue in this type of equipment, and a specific measure for this purpose is a connection structure in which the conduit is divided in the middle and a gap is provided between them. It is disclosed in Japanese Patent No. 59-80593.

[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 produced in the reduction vessel into the condensation vessel, the product quality will deteriorate as the amount of residual substances 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 has been made in view of this situation, and it is an object of the present invention to provide an apparatus for manufacturing a high-melting-point, high-toughness metal that has a simple structure and can completely absorb the thermal expansion of the conduit.

Another object of the present invention is to produce a high-melting-point, high-toughness metal that can quantitatively estimate the progress of the separation and recovery reaction and carry out the separation and recovery process in an appropriate amount of time when separation and recovery is performed using the above manufacturing equipment. The purpose is to provide a method.

[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, at least one of the reduction vessel and the condensation vessel is supported so as to be able to follow the thermal expansion of the conduit.

In the production method of the present invention, when recovering the unreacted active metal and its chloride remaining in the spongy metal generated in the reduction vessel into the condensation vessel by vacuum separation, The present invention is characterized in that a change in weight of at least one of the reduction vessel or the condensation vessel supported so as to be driven is detected, and the degree of progress of the separation and recovery reaction is estimated from the detected weight change.

[For production]

In the manufacturing apparatus of the present invention, at least one of the reduction vessel or the condensation vessel is entirely driven by the thermal expansion of the conduit, so even if both vessels are integrally connected by the conduit, the thermal expansion of the conduit is absorbed. be done.

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 a complicated elongation, but if the thermal expansion is absorbed by the container, the complicated elongation of the conduit will also cause the container to elongate. can be followed accurately and the elongation can be reliably absorbed.

In the production apparatus of the present invention, at least one of the reduction vessel and the condensation vessel is movable, but in actual operation, it is desirable that only the condensation vessel 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. Furthermore, by measuring the fluid pressure while keeping the container at a constant height by adjusting the fluid pressure, the amount of substances in the container can be detected quantitatively, and the progress of the separation and recovery process can be accurately estimated.

The manufacturing method of the present invention takes advantage of the fact that at least one of the reduction container or the condensation container is movable in the manufacturing apparatus, and detects the weight change of the movable fixed container during separation and collection. It quantitatively estimates the progress of the separation and recovery reaction, making it possible to set accurate recovery processing times.

〔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.

An inlet pipe 11 for T i Cf 24 is connected to the upper opening of the reduction container 10, and a discharge pipe 11 for byproducts is connected to the bottom.

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 60
is an annular air pump 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 IO 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 with such a production device, the reduction vessel 1
0 is placed in the heating furnace 20, and the condensation container 30 is set in the cooling furnace 40, and the cooling furnace 40 is supported on a pedestal 50 by an air spring 60. At this time, condensation vessel 3
0 and the cooling furnace 40 are set so that the conduit 70 is located at the neutral point of the air spring 60 in a thermally expanded state. Then, the condensing vessel 30 and the cooling furnace 40 are connected to the conduit 70.
is drawn toward the reduction container 10 by an amount corresponding to the expansion of
The reduction vessel 10 and the condensation vessel 30 are connected by a conduit 70.

Next, the valve'? 2.73 Heating furnace 20 with closed
is operated to hold molten Mg in the reduction vessel 10, and TiCρ4 is introduced from the introduction pipe 11.

As a result, Ti and MgCp, 2
is generated. The generated MBCffi is discharged from the discharge pipe 1 as appropriate.
2 is discharged to the outside. And finally, unreacted M
A spongy Ti containing g and MgC1!2 is obtained.

When the reduction process is completed, after opening the valve '72.73, the heating furnace 20 is heated to 1000'C or more, and the conduit 7
0 to a temperature at which Mg and MgCL do not shrink.
Heat at 1. 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 T in the reduction container 10
Unreacted Mg and M g C1,Z contained in i are evaporated and collected in condensation vessel 30 via conduit 70 .

In this separation and recovery step, the conduit 70 is expanded by heating by the heater 71 and is stretched in the axial direction. However, with the expansion, the condensation vessel 30 and the reduction vessel l along with the cooling furnace 40
The condensation container 30 and the cooling furnace 40 return to the neutral point of the air spring 60 by separating from the air spring 60 and the amount of movement thereof being offset by the amount by which they were 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.

Also, Mg and MgCF! .

As the condensation container 30 is collected, the weight of the condensation container 30 increases, and the load applied to the air spring 60 increases, but the air pressure of the air spring 60 increases so that the height of the condensation container 30 is kept constant. , the reduction vessel 10 and the condensation vessel 30 are always kept at the same level. Therefore, conduit 7
Stress generation due to zero slope is also prevented.

The manufacturing method of the present invention detects the air pressure of the air spring 60 in such a separation and recovery step of Ti manufacturing. As described above, this air pressure increases as the weight of the condensation container 30 increases, so the weight of the condensation container 30 can be quantitatively detected by detecting the air pressure, and the Mg collected in the condensation container 30 can be detected quantitatively. The amount and the amount of MgCl2 are accurately determined. That is, by measuring the air pressure applied to the air spring 60, the amount of Mg and MgCl2 evaporated and recovered can be quantitatively detected. From this change in the amount of evaporation and recovery and the change in the amount of electricity used compared to the conventional one, the amount of unreacted Mg and MgCl contained in the spongy Ti in the reduction vessel 10! , the changes in the amounts of the two are clarified, and the optimal separation and recovery processing time can be determined. As a result, the amount of Mg remaining in the Ti sponge and the amount of Mg (12) are sufficiently reduced, wasteful processing time is reduced, and power consumption is reduced.

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.

2 Table 1 FIG. 1 is a sectional view of a manufacturing apparatus showing an embodiment of the present invention.

In the figure, 10: reduction vessel, 20: heating furnace, 30: condensation vessel, 40: cooling furnace, 50: pedestal, 60: air spring, 70: conduit.

〔Effect of the invention〕

The manufacturing apparatus of the present invention reliably absorbs the thermal expansion of the conduit, which becomes a problem when the reduction vessel and the condensation vessel are integrated side by side,
Prevent crack damage to conduits and their connecting parts to extend equipment life. In addition, the entire conduit can be integrated, and there is no need to interpose gaskets in the middle of the conduit, which simplifies the structure of the conduit, making it easier to heat the conduit, and preventing clogging of the conduit starting from the connection. Ru.

In addition to the above-mentioned effects, the manufacturing method of the present invention optimizes the separation and recovery time for residual substances, thereby achieving reductions in power consumption and improvement in product quality.

[Brief explanation of drawings]

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. 1. An apparatus for producing a high-melting-point high-toughness metal, characterized in that at least one of the container and the condensation container is supported so as to follow the thermal expansion of the conduit. (2) When the unreacted active metal and its chloride remaining in the spongy metal generated in the reduction vessel are recovered into the condensation vessel by vacuum separation, the metal can be moved along with the thermal expansion of the conduit. 1. A method for producing a high-melting-point tough metal, comprising: detecting a change in weight of at least one of a reduction vessel or a condensation vessel supported by the vessel, and estimating the degree of progress of a separation and recovery reaction from the detected weight change.