JP5036488B2 - Titanium sponge extraction method and apparatus - Google Patents

Description

  The present invention relates to a method and apparatus for producing titanium sponge by magnesium reduction of titanium tetrachloride, and more particularly to a method and apparatus for efficiently extracting the produced titanium sponge from a container.

  Titanium metal production has been greatly increased not only in the aircraft industry but also in recent years with the expansion of global demand. Sponge titanium, which is a raw material for metallic titanium, is mass-produced by the crawl method, and this method is performed by dropping titanium tetrachloride onto a molten magnesium bath surface charged and held in a stainless steel reaction vessel. Sponge titanium is produced in the reaction vessel.

  Subsequently, by heating at a high temperature under reduced pressure to separate impurities such as magnesium chloride and metal magnesium remaining in the sponge titanium produced in the reaction vessel from the sponge titanium, a sponge titanium lump is obtained. It is done.

  After the impurities in the sponge titanium produced in the vessel are removed in the vacuum separation step, the product is cooled to room temperature, and then the concave member joined to the bottom of the reaction vessel is cut and separated, An opening is formed at the bottom. This schematic diagram is shown as the reaction vessel 10 in FIG. As shown in FIG. 3, an opening 12 is formed at the bottom of the reaction vessel 10 holding the sponge titanium 11.

  FIG. 3 also shows a conventional extraction device N for extracting the produced sponge titanium 11 from the reaction vessel 10. The extraction device N includes an extraction device main body 20, a support base 21, and a punch bar 22. In order to push out the sponge titanium lump 11 generated in the reaction vessel 10, first, a push-out rod 22 is inserted from the opening 12 provided at the bottom of the reaction vessel 10 and brought into contact with the bottom of the sponge titanium 11. After that, the top of the reaction vessel 10 is then extracted to the apparatus main body 20 by the fixing jig 24 to restrain the movement of the reaction vessel 10.

  Subsequently, the sponge titanium 11 is moved into the reaction vessel 10 by gradually moving the push-out rod 22 in contact with the bottom of the sponge titanium 11 upward with the help of a hydraulic cylinder built in the support base. The sponge titanium 11 can be extracted from the reaction vessel 10 by gradually moving upward while sliding relative to the reaction vessel 10.

  However, in order to enable the sliding extraction of the sponge titanium as described above, it is necessary to transmit sufficient stress to the punching bar 22, and as a result, a large size for driving the punching bar 22 is required. A hydraulic cylinder is required.

  When introducing the large hydraulic cylinder, it is necessary not only to have a sufficient installation space in the factory, but also to calculate the cost corresponding to the size of the hydraulic cylinder, and the construction period may be long. Expected.

  Such a situation is a disadvantageous condition for newly responding to the recent demand for sponge titanium by newly installing a titanium sponge manufacturing facility, which is space-saving, has a short construction period and is cost effective. There is a demand for an apparatus for extracting sponge titanium that does not apply and an extraction method using the apparatus.

  A specific example of the method of punching out sponge titanium is disclosed in JP-A-6-145825 (see, for example, Patent Document 1). This publication describes a method for efficiently extracting not only sponge titanium produced in a reaction vessel but also sponge titanium produced on the inner wall surface of the reaction vessel above the sponge titanium produced in the reaction vessel.

  However, there is no description regarding a method for extracting sponge titanium, which has a short construction period, is inexpensive in initial investment, and saves space with respect to a method capable of efficiently extracting sponge titanium as described above.

Thus, there is a need for a sponge titanium extraction method and an apparatus suitable for this that require a small initial investment, a short construction period, and space saving.
JP-A-6-145825

  The present invention relates to a method for extracting titanium sponge produced by the crawl method and an apparatus used therefor, and in particular, a method and apparatus capable of efficiently extracting the titanium sponge produced in the reaction vessel from the reaction vessel. The purpose is to provide.

  As a result of intensive investigations in view of such circumstances, when extracting the titanium sponge from the reaction vessel, a punch bar is brought into contact with the bottom of the sponge titanium lump, and the reaction vessel and the titanium sponge are brought into contact with each other by the weight of the reaction vessel. It has been found that titanium sponge can be efficiently extracted from the reaction vessel while sliding against each other, and the present invention has been completed.

  That is, the method for extracting sponge titanium according to the present invention is a method for extracting sponge titanium produced in the reaction vessel by magnesium reduction of titanium tetrachloride from the reaction vessel, and forming an opening at the bottom of the reaction vessel, A punching rod is inserted into the opening, the punching rod is brought into contact with the lower end portion of the sponge titanium in the reaction vessel, and the reaction vessel and the sponge titanium are slid against each other by the own weight of the reaction vessel. It is characterized by moving downward.

  In the method for extracting sponge titanium according to the present invention, the wire engaged with the crane is connected to the reaction vessel in which sponge titanium is generated, and the wire is relaxed in a state where the punch bar is in contact with the lower end of the sponge titanium. Thus, it is preferable to slide the reaction vessel downward.

  In addition, prior to extracting the titanium sponge, the titanium sponge formed on the inner wall surface of the container in the upper space of the titanium sponge formed in the reaction container is preferably removed.

  Further, before extracting the entire amount of sponge titanium from the reaction vessel by the above method, the extraction operation is stopped, the wire engaged with the reaction vessel is removed, and then the sponge titanium extracted outside the reaction vessel is removed. A preferred embodiment is to connect the parts using wires or tongs and to extract the entire amount of sponge titanium from the reaction vessel.

  An apparatus for extracting sponge titanium according to the present invention is an apparatus used in the above-described extraction method, and includes an extraction apparatus main body that holds a reaction vessel in which sponge titanium is generated, a support pedestal provided at the bottom of the extraction apparatus main body, It is characterized by being comprised from the punching rod which is supported by the support base and presses the bottom part of sponge titanium.

  In the sponge titanium extracting apparatus of the present invention, it is preferable that the length of the punch bar held by the support pedestal is changeable, and at the lower end of the punch bar. The groove is formed in multiple stages in the vertical direction, and it is preferable that the punch bar and the support base are fixed at an arbitrary position by engaging the pin with the groove.

  According to the present invention, by inserting a punch bar from the bottom of the reaction vessel holding the titanium sponge and pressing the bottom of the titanium sponge upward, the reaction vessel receiving a downward force due to the weight of the reaction vessel, The sponge titanium that receives upward force by the pulling rod slides against each other, and the sponge titanium can be pushed out of the reaction vessel, so there is no need to install a separate large hydraulic cylinder for punching. This makes it possible to punch out sponge titanium with a small space and low initial investment.

The best embodiment of the present invention will be described below with reference to the drawings.
FIG. 1 is a preferred apparatus configuration example of a titanium sponge extraction device used in the present invention, and shows a state where a reaction vessel holding sponge titanium is installed in this extraction device.

  First, in a process (not shown), the reaction vessel 10 is filled with molten magnesium, and titanium tetrachloride is dropped into the reaction vessel 10 to reduce the magnesium tetrachloride to produce titanium sponge 11. Subsequently, after most of the by-product magnesium chloride is removed, the reaction vessel 10 is placed in a high-temperature and reduced-pressure atmosphere to remove residual impurities such as magnesium chloride. Next, after the opening 12 is formed by cutting the protrusion formed on the bottom of the reaction vessel 10, the opening 12 is suspended by the wire 14 engaged with the crane 13 and transferred to the punching device M. FIG. 1A shows the state at this time.

  As shown in FIG. 1 (a), the punching device M pushes out the punching device main body 20, the support pedestal 21 installed at the bottom thereof, and the sponge titanium disposed on the pedestal 21 while standing upright. And a punching rod 22.

  From the opening 12 of the reaction vessel 10 transferred to the punching device M, the wire 14 is fed out so that the punching bar 22 of the punching device M comes into contact with the bottom surface of the rooster 15 arranged in close contact with the sponge titanium 11. Adjust the situation.

  Next, the contact state between the punch bar 22 and the rooster 15 is confirmed by the looseness of the wire 14 by the above operation, and then the wire 14 is gradually fed out, so that the reaction container 10 is caused by its own weight. The entire 10 can be lowered.

  Since the sponge titanium 11 generated in the reaction vessel 10 is fixed to the punch rod 22 through the rooster 15, the reaction vessel 10 slides relative to the sponge titanium 11 as the wire 14 is fed. However, the reaction vessel 10 stops descending when it resists the stress of the wire 14 again.

  Therefore, the feeding amount of the wire 14 in the present invention can be appropriately adjusted while watching the descending state of the reaction vessel 10.

  By repeating the above-described operation, the sponge titanium 11 is relatively restrained from moving through the rooster 15, and the reaction vessel 10 is slid with the sponge titanium 11 as the wire 14 is unwound. As a result, the sponge titanium 11 can be extracted from the reaction vessel 10.

  In the present invention, the length of the punch bar 22 is set so that the flange 16 of the reaction vessel 10 contacts the flange 23 of the extraction device body 20 before the sponge titanium 11 is completely extracted from the reaction vessel 10. It is preferable to set.

  FIG. 1B schematically shows the situation where the sponge titanium 11 has been pushed out until the flange 16 of the reaction vessel 10 abuts against the flange 23 of the punching device main body 20 after performing the above-described punching. . In the present invention, the extraction height of the sponge titanium 11, that is, the length of the sponge titanium 11 exposed from the end of the reaction vessel 10 (symbol a in FIG. 1B) is the total length of the sponge titanium 11 (same as above). It is preferable to adjust the length of the punch bar 22 so as to be in the range of 50% to 100% of the sign b).

  In accordance with the above-described embodiment, the extraction operation is stopped before the entire amount of the titanium sponge 11 is extracted from the reaction vessel 10 and the wire 14 engaged with the flange 16 of the reaction vessel 10 is removed. As described above, the sponge titanium 11 is connected to a wire 17 provided in advance around the sponge titanium 11 extracted from the reaction vessel 10, and further, the wire 14 is engaged with the crane 13 and lifted upward. The entire amount can be extracted from the reaction vessel 10.

  In the present invention, there is a case where titanium sponge adheres and grows on the upper inner wall surface of the reaction vessel 10 where the titanium sponge 11 is generated. In this case, prior to the extraction of the titanium sponge by the above-described method. It is preferable that the titanium sponge grown on the upper inner wall surface of the reaction vessel 11 is removed in advance.

  According to the above-described invention of the present application, there is no need for a hydraulic cylinder in which the punch rod 22 is extended upward and the sponge titanium 11 can be pushed out from the reaction vessel 10 as in the prior art, and the initial investment cost is suppressed. Can do. In addition, there is an effect that electric power and maintenance cost for driving the hydraulic cylinder are not required, and the running cost can be reduced.

  Furthermore, there is no need for the pressure generating device for the hydraulic cylinder, there is no need to secure the space, and there is an effect that the extraction device can be installed in the field with a small space.

  Next, the configuration of the punching device M used in the present invention and preferred modes thereof will be described below. As shown in FIG. 1, the punching device M used in the present invention includes a punching device main body 20, a punching rod 22, and a support base 21 for supporting the punching rod.

  The punch bar 22 is preferably configured to support the weight of both the sponge titanium 11 and the reaction vessel 10 and the frictional force generated when the reaction vessel 10 slides.

  In the present invention, the punch bar 22 can be made of, for example, tool steel, and the diameter of the punch bar 22 at that time is preferably in the range of 400 mm to 800 mm. By configuring with the punch bar 22 having the above size, 6 to 15 t / batch of sponge titanium can be efficiently punched out.

  In the present invention, as described above, the punch bar 22 does not need to be moved upward as in the prior art, and it is only necessary to fix and arrange it on the support base 21. However, the length of the punch bar 22 is set so that the flange 16 of the reaction vessel 10 is removed from the punching device main body 20 before the sponge titanium 11 is completely pushed out of the reaction vessel 10 as shown in FIGS. Although it is preferable to be configured to be placed on the flange 23, the amount of sponge titanium 11 produced in the reaction vessel 10 varies somewhat.

  Therefore, it is preferable to devise a connection method between the support base 21 and the punch bar 22 so that the length of the punch bar 22 can be changed. Specifically, a plurality of grooves may be formed in the vertical direction on the surface of the punch bar 22, and the support base 21 and pins may be fixed to the grooves. By adopting such an apparatus configuration, the length of the punch bar 22 can be adjusted, and there is an effect that it is possible to cope with variations in the overall length of the sponge titanium 11 in the reaction vessel 10. It is.

  The support pedestal 21 is a structural member for supporting and fixing the punch bar 22 to the punching device body 20 and supports the weight of the sponge titanium 11 and the reaction vessel 10 and the stress generated when the reaction vessel 10 slides. It should be configured so that it can.

  The punching device main body 20 may be configured with a size and a material capable of supporting the above-described components, and may be configured with general structural steel. Alternatively, instead of the punching device main body 20, a pit may be configured, and the punching device M may be configured therein. By setting it as such a structure, there exists an effect that workability | operativity at the time of extracting the sponge titanium 11 from the reaction container 10 can be improved.

  As described above, by using the sponge titanium punching method and apparatus according to the present invention, it is possible to efficiently push the sponge titanium in a space-saving manner while keeping initial investment and running cost low. It plays.

  Using the sponge titanium punching device shown in FIG. 1, 9 t of sponge titanium 10 was extracted from the reaction vessel. This operation was performed 5 batches. The average time required for extracting the 5 batches is shown in Table 1 as an example. Moreover, the sponge titanium 10 was extracted from the reaction vessel 11 under the same conditions as in the example except that the conventional sponge titanium punching device shown in FIG. 3 was used, and is shown in Table 1 as a comparative example.

  Table 1 summarizes the examples and comparative examples from the viewpoint of the extraction time of sponge titanium, equipment cost, and space, with Comparative Example 100. The extraction time when using the extraction apparatus according to the present invention shown in FIG. 1 was not significantly different from that when using the conventional apparatus. However, in terms of equipment cost and installation space, it has been confirmed that there has been a significant improvement over the prior art. As a result, it was also confirmed that the construction period of the equipment can be greatly shortened compared to the conventional method.

  This contributes to cost reduction in the production of titanium metal, which is in increasing demand in recent years.

It is a schematic diagram sectional drawing which shows the sponge titanium extraction apparatus of this invention, Comprising: (a) shows the state before extraction, (b) shows the state after extraction. It is a schematic diagram sectional drawing which shows the sponge titanium extraction method in the sponge titanium extraction apparatus of this invention. It is a schematic cross section of the conventional sponge titanium extraction apparatus.

Explanation of symbols

M Sponge Titanium Extraction Device N Conventional Sponge Titanium Extraction Device 10 Reaction Vessel 11 Sponge Titanium 12 Opening 13 Crane 14 Wire 15 Rooster 16 Flange 17 Wire 20 Extraction Device Body 21 Support Base 22 Punch Bar 23 Flange 24 Fixing Jig

Claims (8)

A method of extracting titanium sponge produced in a reaction vessel by magnesium reduction of titanium tetrachloride from the reaction vessel,
An opening is formed at the bottom of the reaction vessel, a punching rod is inserted into the opening, the punching rod is brought into contact with the lower end of the sponge titanium in the reaction vessel, and due to the weight of the reaction vessel, A method for extracting titanium sponge, wherein the reaction container is moved downward while sliding the reaction container and the titanium sponge.   The wire engaged with the crane is connected to the reaction vessel in which the sponge titanium is generated, and the reaction vessel is moved downward by relaxing the wire in a state where the punch bar is in contact with the lower end of the sponge titanium. The method for extracting titanium sponge according to claim 1, wherein:   The sponge according to claim 1 or 2, wherein the sponge titanium formed on the inner wall surface of the container in the upper space of the sponge titanium formed in the reaction vessel is removed prior to the extraction of the sponge titanium. Titanium extraction method.   Before extracting the entire amount of the sponge titanium from the reaction vessel by the above method, stop the extraction operation, and use the wire or tongue on the portion of the sponge titanium extracted outside the reaction vessel, the total amount of the titanium sponge The method for extracting titanium sponge according to any one of claims 1 to 3, wherein the is extracted from the reaction vessel.   The method for extracting sponge titanium according to any one of claims 1 to 4, wherein the titanium sponge lump extracted from the reaction vessel is crushed and sized to obtain product sponge titanium. An apparatus for extracting titanium sponge used in the method for extracting sponge titanium according to claim 1,
The above-mentioned sponge titanium extraction device includes an extraction device main body that holds a reaction vessel in which sponge titanium has been generated, a support pedestal provided at the bottom of the extraction device main body, and a push that supports the bottom of the titanium sponge supported by the support pedestal. An apparatus for extracting titanium sponge, characterized in that it comprises a extracting rod.   The apparatus for extracting titanium sponge according to claim 6, wherein the length of the punch bar held on the support base is changeable.   Grooves are formed in multiple stages in the vertical direction at the lower end of the punch bar, and the punch bar and the support base are fixed at any position by engaging a pin with the groove. An apparatus for extracting titanium sponge according to claim 7.

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