JP3516625B2 - Separation apparatus and separation method for impurities in metal - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a separation device and a separation method for impurities in a metal, and more particularly to a separation device for efficiently separating impurities in a sponge-like metal.

In this specification, "separation" means
Treatment of metals such as Mg and impurities such as chlorides such as MgCl ₂ remaining in sponge-like metals produced by reducing chlorides of metals such as titanium and zirconium with metals such as Mg at high temperature and under vacuum or reduced pressure Then, it means to volatilize and remove. "Metal" shall mean titanium or zirconium metal. Although MgCl ₂ is mainly recovered by the separation, metallic Mg may also be recovered together. In this specification, it may be simply referred to as MgCl ₂ at this time as well.

[0003]

2. Description of the Related Art For example, in the process for producing titanium sponge by the Kroll method, titanium tetrachloride and metallic magnesium are reacted at a high temperature to produce titanium sponge and MgCl ₂ , and further, a metal not reacted with MgCl ₂ is used. It consists of a separation step in which magnesium is separated and removed from titanium sponge by heating at high temperature while vacuuming.

In such a reduction and separation step of sponge-like metal, as a device used for separation, a reaction vessel and a condensation vessel are generally used, and the reaction vessel and the condensation vessel are arranged side by side to form a horizontal conduit. Many device configurations connected to each other are adopted.

[0005]

However, even in sponge-like metals such as titanium sponge that have undergone the above-described separation step, metals such as MgCl ₂ and Mg remain. Such a sponge-like metal is refined again into a sponge-like metal with less impurities by volatilizing and removing the above residue at high temperature and under vacuum or reduced pressure (hereinafter sometimes referred to as "re-separation"). You can
Conventionally, this re-separation has been performed by an apparatus configuration in which the reaction vessel and the condensation vessel used in the separation step are juxtaposed and connected to each other by a horizontal conduit.

MgCl ₂ recovered in the above re-separation
The residual amount of sponge-like metal such as is much less than the amount recovered in the separation step performed immediately after the generation of sponge-like metal, and is 1/10 or less. Since it is included, the separation time at the time of re-separation is also required to be twice as long as that in the separation step.
Therefore, using the same equipment used in the separation step for re-separation is very inefficient in terms of its separation capacity, and further diverts the original equipment for sponge-like metal production, Since it is occupied, the capacity in the separation step is lowered, and as a result, the spongy metal production capacity is lowered, which is a disadvantage.

An object of the present invention is to provide a facility capable of efficiently re-separating a sponge-like metal of a high melting point and high toughness metal in a single container, and further improving the production efficiency of the sponge-like metal. Thus, another object of the present invention is to provide a purifying separation facility for the recovered chloride (eg MgCl ₂ ).

[0008]

According to the first aspect of the present invention, there is provided a separation device attached to a container having a lid, which is connected to a jacket and a suction device for circulating a cooling medium. A cooler having a suction port and a receiver having an opening, the cooler being installed outside the container of the lid, and the receiver being installed inside the container of the lid. It is solved by making it connect with the container through the opening and connecting the cooler and the receiver with a connecting pipe.

As described above, according to the present invention, since the container having the opening is provided inside the container, solid or liquid MgCl ₂ evaporated by re-separation and condensed and deposited by the cooler is received. The structure is such that it will not be returned to the container.

Further, since the separation device of the present invention is attached to a container provided with a lid, it can be attached to the reaction container used for the reaction production of the sponge-like metal for re-separation, and the re-separation process is simplified. It is possible to do.

As described above, by using the device attached to the container and connecting the cooler and the receiver with the connecting pipe, the volumetric efficiency can be increased as compared with the conventional case.
It is possible to efficiently perform re-separation and to purify a sponge-like metal with higher purity. In addition, the original separation facility is released from the re-separation process, and it is possible to prevent a decrease in the processing capacity in the separation process, and as a result, it is possible to improve the production efficiency of the sponge-like metal. Here, the internal volume of the cooler in the separation apparatus of the present invention is usually 30% or less of the internal volume of the container, and preferably 1 to 10%. In the conventional separation device, the volume ratio of the container to the cooler is approximately 1: 1 and a very large cooling capacity is required, but in the present invention, since the cooler has such a small volume,
It became possible to cool efficiently and perform separation.

Furthermore, it is preferable that at least one baffle plate is arranged inside the cooler. By providing the baffle plate in this manner, the inside of the cooler has a labyrinth structure, the flow path of MgCl ₂ gas extends, and the contact area with the cooling part increases. For this reason, solid MgCl ₂ gas is easily deposited, and the efficiency of MgCl ₂ recovery can be increased.

Further, the inside of the cooler is divided into a plurality of rooms, and the respective rooms are communicated with each other by a connecting pipe projecting upward in the room, and a connecting pipe is provided above the connecting pipe through a space. It is also possible to form it so as to form a covering portion. In this way, by dividing the chamber into a plurality of chambers and providing the connecting pipe and the cover, the flow path is lengthened as in the case of the labyrinth structure, which facilitates the precipitation of MgCl.
It is possible to improve the collection efficiency of ₂ .

Further, it is preferable that the receiver is provided with a heat shield plate below the opening communicating with the container. As described above, since the heat shield plate is arranged below the opening communicating with the container in the receiver, the deposits are vaporized again by the heat shield plate. This can be prevented, and the efficiency of MgCl ₂ recovery can be increased.

According to a fifth aspect of the present invention, there is provided a separation device which is connected to a container, wherein a receiver having an opening located in the container and a pre-cooling device that communicates with the receiver. A cooling device having a jacket and a suction port for circulating the cooling medium, and a recovery container connected to the cooling device. A detachable suction device is connected to the recovery container for cooling and heating. It is solved by configuring so that it can be selectively performed.

When the recovery container is provided separately from the container as described above, and the recovery container is selectively cooled and heated, it is deposited on the recovery container by cooling, and the recovery container is heated in the deposited state. It is possible to melt the impurities in the collection container, discharge the impurities from the collection container, and collect the impurities.

At this time, a plurality of baffle plates having a shape in which impurities are deposited during cooling and the liquid impurities are melted and fallable during heating are arranged inside the recovery container. It is suitable if it is.

As described above, by providing the baffle plate having the special shape in the collection container, it is possible to prevent the precipitate deposited by cooling from coming out of the collection container during cooling, and the impurities are removed from the collection container during heating. It can be easily discharged.

According to a seventh aspect of the present invention, there is provided a cooler having a jacket and a suction port for circulating a cooling medium, and a receiver having an opening. A step of attaching the cooler to the outside of the container and the receiver to the inside of the container of the separation device in which the openings communicate with each other, and charging metal into the container to heat the container under reduced pressure or vacuum. And a step of causing impurities to be removed from the metal by the above method, and a step of condensing the impurities in a cooler of the separator and collecting the impurities in the receiver.

Further, according to the invention as set forth in claim 8, the above-mentioned problem is a step of charging a metal into a container and heating the container under reduced pressure or vacuum; and a receiver positioned in the container,
A step of pre-cooling impurities emitted from the metal through a cooler having a jacket and a suction port which communicate with the receiver and through which a cooling medium for pre-cooling flows, and cooling the pre-cooled impurities A first deposition step of depositing in a recovery container equipped with a jacket for circulating a cooling medium, a heating step of heating the recovery container in which the deposited impurities are present, and an impurity melted by the heating step. This is solved by a separation method including a second precipitation step of precipitation from the recovery container.

At this time, it is preferable that the recovery container is inverted when the first precipitation step is transferred to the heating step.

Further, in the first precipitation step, a recovery container is used in which a plurality of baffle plates are arranged so that impurities are not dropped but are turned into a heating step and liquid impurities can be dropped. In the first precipitation step, the impurities are precipitated as a solid, in the heating step, the solid precipitated in the first precipitation step is made into a liquid, and in the second precipitation step, the impurities turned into a liquid by the heating step. Is preferably configured to be recovered.

[0023]

As described above, according to the present invention, the re-separation of the sponge metal is attached to the container equipped with the lid,
By using a separator that connects a cooler and a receiver that has an opening with a heat shield plate at the bottom with a connecting pipe, it is possible to increase the volumetric efficiency compared to the conventional method, and efficiently. Re-separation can be performed to purify a sponge-like metal with higher purity. In addition, the original separation equipment is released from the re-separation process, the reduction of the processing capacity in the separation step can be prevented, and as a result, the production efficiency of the sponge-like metal can be improved. Furthermore, since the reaction container used for the reaction of the sponge-like metal can be used as it is as the above-mentioned container, the re-separation treatment can be easily performed.

[0024]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described below with reference to the drawings. The members, arrangements, etc. described below do not limit the present invention and can be variously modified within the scope of the gist of the present invention.

1 to 9 show a separation apparatus according to the present invention, FIG. 1 is an explanatory view showing a schematic structure of the separation apparatus, FIG. 2 is an explanatory view of the structure of a cooler which constitutes the separation apparatus, and FIG. Of the cooling device of FIG. 4, FIG. 4 is a diagram of the structure of another cooling device, FIG. 5 is a diagram of the structure of a receiver constituting the separating device, and FIG. 6 is a schematic diagram of the separating device including a recovery container. FIG. 7 is an explanatory view showing a state in which the recovery container is inverted, FIGS. 8 and 9 are more specific perspective views of the separating device, and FIG. 8 is a configuration diagram showing a container equipped with the separating device. 9 is a schematic perspective view of the separation device of FIG. In the embodiments of each drawing, the same members are designated by the same reference numerals and described.

As shown in FIG. 1, the separating device S comprises a container 1
0, but in FIG. 1, the lid 11 of the container 10
It shows an example attached to. That is, the container 10 of this example is housed in a heating furnace (not shown). Container 10
A lid 11 is disposed above the. A separating device S is attached to the lid 11.

The separating apparatus S of this example comprises a cooler 30, a receiver 40, and a connecting pipe 50. The receiver 40 of the present example has an opening 41 of a hollow cylinder that projects to the outside of the receiver 40, and is communicated with the container 10 through this opening 41. The receiver 40 is installed inside the container 10 and attached to the lid 11 of the container 10.

The cooler 30 of this embodiment is provided with a jacket 31 on the outer periphery of the cooler 30, and a cooling medium is circulated in the jacket 31 to cool the cooler 30. Has been done. A suction port 32 is formed on the upper side of the cooler 30 (see FIG. 1), and the suction port 32 is connected to a suction device (for example, a vacuum pump) not shown.

As described above, the cooler 30 and the receiver 40 are connected by the connection pipe 50, and the connection pipe 50 connects the cooler 30 and the receiver 40.

Because of the above-mentioned configuration, the sponsor
Taking dititanium as an example, the container 10 is heated and the cooler 30 is used.
When the suction device (not shown) on the side is activated,
MgCl which is an impurity introduced_TwoSponge containing
When the tan is heated, MgCl _TwoIs vaporized into gas,
Received from the opening 41 of the receiver 40 located in the container 10.
Flows into the container 40 and further through the connecting portion 50 to the container 10
It is cooled by the cooler 30 located outside the. By this
And gaseous MgCl_TwoIs cooled, and it precipitates or becomes liquid.
And then deposits inside the receiver 40 through the connecting pipe 50.
It

FIG. 2 shows another embodiment of the cooler 30, and in this example, the inside of the cooler 30 becomes a maze.
The baffle plate 33 is formed in different steps. According to this example, the baffle plates 33 that are formed in the cooler 30 and have different steps
The impurities (eg MgCl ₂ ) also deposited on the upper surface of the
Are accumulated and can be collected in the cooler 30 in addition to the receiver 40.

3 and 4 show further different modes of the cooler 30, and in these examples, the inside of the cooler 30 is divided into a plurality of rooms. In the example of FIG. 3, the first room 35 is connected to the first room 3 by the connecting pipe 50.
It is configured to communicate with each other by a connecting pipe 36 projecting upward in the inside 5. Similarly, the second chamber 37 is configured to communicate with the first chamber 35 by a connecting pipe 38 projecting upward in the second chamber 37. A cover 61 is provided above the connecting pipes 36 and 38 so as to cover the connecting pipes 36 and 38 with a space therebetween. As shown in FIG. 3, the cover portion 61 is formed with a substrate 61a and a hanging portion 61b formed downward toward the outer periphery.

In the example shown in FIG. 3, the connection between the container 10 and the first room 35 and the connection between the first room 35 and the second room 37 have the same structure. The example of FIG. 4 illustrates an example in which the connection (communication) between the first room 35 and the second room 37 is different. That is,
As shown in FIG. 4, the first chamber 35 and the second chamber 37 communicate with each other by using two connecting pipes 39, and other configurations are the same as those in FIG.

As described above, the plurality of connecting pipes 39 (2 in FIG.
However, it is possible to enhance the precipitation effect and increase the precipitation amount. In the example of FIG. 4, the first room 35
Although an example in which the communication between the second chamber 37 and the second chamber 37 is performed by a plurality of connecting pipes 39 is illustrated, the receiver 4 not shown in FIGS.
It is also possible to configure the connecting portion between 0 and 0 by a plurality of connecting pipes.

FIG. 5 shows another example of the receiver 40. The receiver 40 shown in FIG.
The receptacle 40 is provided with a heat shield plate 43 at a position lower than the opening 42 communicating with the container 10. With this structure, impurities (for example, M
It is possible to collect and collect gCl ₂ ). Note that FIG. 5 shows the receiver 40 having a structure in which the heat shield plate 43 is disposed below to serve as a bottom plate, but the present invention is not limited to this, and the heat shield plate 43 is disposed inside the receiver 40. It may be configured.

6 and 7 show impurities (eg MgCl 2
₂ shows an example in which the recovery container 70 is used instead of the receiver 40. That is, as shown in FIG. 6, in the case of the present example, the portion of the cooler 30 is configured to perform pre-cooling, and further, the cooler 30 is connected to the recovery container 70 via the pipe 63. Has been done.

The tubular body 63 and the recovery container 70 of this example are connected by a removable connecting portion 67. Further, a suction device (not shown) is detachably connected to the recovery container 70 located on the opposite side of the pipe 63 connected to the cooler 30 by the connecting portion 68. A vacuum pump or the like is used as the suction device, and may be directly and removably connected to the vacuum pump, or may be connected to the vacuum pump via the pipe 64 so that the pipe 64 and the recovery container 70 can be attached and detached. It may be configured to be connected to.

Further, in this embodiment, a rotation mechanism (not shown) is connected to the recovery container 70 so that the recovery container 70 is inverted. Although not shown as a rotation mechanism,
A rotation shaft is formed at a predetermined position on the outer circumference of the collection container 70, and the rotation shaft is driven by a drive source such as a motor to generate the collection container 70.
Can be configured to be reversible. The control of the drive source and the like can be performed by a computer device including a CPU and the like.

A cooling device 72 and a heating furnace 74 are arranged at the outer peripheral position of the recovery container 70. The cooling device 72 of this example is air-cooled in this example, and cools the recovery container 70 with a blower fan. An electric heating furnace is used as the heating furnace 74. Of course, the cooling device 72 and the heating furnace 74 are not limited to these.

In this example, the cooling device 72 is arranged on the half circumference side of the outer circumference half position of the recovery container 70, and the heating furnace 74 is arranged on the other half circumference side. The heating furnace 74 and the heating furnace 74 are movable, and the collection container 7 is selectively used.
It is also possible to configure to be alternately located at the outer peripheral position of 0. As described above, in this example, cooling and heating can be selectively performed, and the structure is formed so as to be upside down.

Inside the recovery container 70, a cooling device 7 is provided.
Impurities (for example, MgCl ₂ ) that precipitate in the recovery container 70 do not fall when driving No. ₂ and are liquefied when inverted and heated in a heating furnace (for example, MgCl ₂ ). A plurality of baffle plates 80 having a shape capable of falling are arranged at predetermined intervals.

Specifically, as shown in FIG. 6, the baffle plate 80 has impurities (eg, MgC) deposited during cooling.
l ₂ ), so that the V-shaped receiving baffle 81,
It is formed by appropriately combining mountain-shaped baffle plates 82 formed in a mountain shape from the wall of the collection container 70 toward the center. A communication hole (communication hole) is provided at a predetermined position of the mountain-shaped baffle plate 82.
83 is formed. A plurality of communication holes 83 can be formed. Further, as shown in FIG. 7, the baffle plate 80
Has a shape such that it easily drops when heated, contrary to the state when cooled.

Next, the operation of the example shown in FIGS. 6 and 7 will be described. Impurities (eg, MgCl ₂ ) vaporized in the container 10 by suction by a suction device (vacuum pump) connected to the recovery container 70. Is introduced into the cooler 30 via the receiver 40 and precooled by the cooler 30.
At this time, the pre-cooling is performed by water cooling to a temperature equal to or higher than the melting point of impurities (for example, 800 ° C. or higher for MgCl ₂ ). Further, the cooling (air cooling) in the recovery container 70 is performed so as to be below the melting point of impurities (for example, MgCl ₂ ) (714 degrees Celsius). Then, the impurities (eg, MgCl ₂ ) pre-cooled by the cooler 30 are further cooled by the collection container 70 and are deposited on the baffle plate 80 arranged in the collection container 70. In the case of MgCl ₂ , this reaction is
l ₂ (gas) → MgCl ₂ (solid).

The precooling in the cooler 30 and the cooling of the recovery container 70 are performed within a range in which precipitation of impurities (eg, MgCl ₂ ) does not often occur in the precooling in the cooler 30, and the cooling device 72 is cooled in the recovery container 70. Impurities (eg MgC
The temperature range in which l ₂ ) precipitates is appropriately selected. At this time, impurities (eg, MgCl 2) deposited in the recovery container 70
_{Since 2} ) is heated again to 714 ° C. or higher in the heating furnace 74, it is necessary to take care not to lower the temperature too much by cooling the recovery container 70.

Then, as shown in FIG. 7, a recovery container 70
Invert. When the collection container 70 is inverted, the connection with the connecting pipe 63 is released and, at the same time, the connection with the suction device is released (the connecting portions 67 and 68 are released). Then, a rotation mechanism (not shown) is driven to reverse the collection container 70. At this time,
Some of the precipitated impurities (eg, MgCl ₂ ) fall as shown in FIG. 8, so the container Y is arranged. Then, the recovery container 70 is heated. This heating order to ensure the fluidization of the solid and become impurities (e.g. MgCl ₂₎
, And the heat so that the temperature higher than the melting point of the impurities (e.g., MgCl _2). As a result, the precipitated impurities (for example, MgCl ₂ ) located on the baffle plate 80 become liquid, fall inside the collection container 70, and can be collected inside the container Y. The reaction at this time is, for example, in the case of MgCl ₂ is MgCl ₂ (solid) → MgCl ₂ (liquid). Incidentally, which was further purified, it is possible Rukoto to be sold product sales in the anhydride.

In this example, the cooling and heating of the recovery container 70 is shown by arranging the cooling device 72 and the heating furnace 74 at half positions on the outer circumference of the recovery container 70. Liquefied from the portion heated by the heating furnace 74 first and dropped, but as the cooling device 72 and the heating furnace 74, the heating furnace 74 is arranged with the space 73 at the outer periphery of the recovery container 70 placed. At the time of cooling, without heating the heating furnace 74, air is sent between the recovery container 70 and the heating furnace 74 for cooling, and at the time of heating, the sending out of air is stopped,
The heating furnace 74 may be used for heating. As described above, heating and cooling can be appropriately selected on condition that the heating temperature and the cooling temperature are within the optimum range.

As a separating method, a separating device S as shown in FIGS. 1 to 5 is attached to the container 10. In other words, the cooler 30 having the jacket 31 and the suction port 32 for circulating the cooling medium and the receiver 40 having the openings 41 and 42 are provided, and the cooler 30 and the openings 41 and 42 are provided.
The step of attaching the cooler 30 to the outside of the container 10 and the receiver 40 to the inside of the container 10 is performed for the separating device S communicating with. Next, after metal (titanium sponge in the case of titanium) is charged into the container 10 to heat the container 10, the container 1
A step of starting decompression within 0 to volatilize and remove MgCl ₂ as an impurity from titanium sponge is performed. Further, the steps of causing the cooler 30 of the separation device S to agglomerate MgCl ₂ as an impurity and causing the receiver 40 to precipitate MgCl ₂ as an impurity are performed in parallel. Thereby, MgCl ₂ contained in titanium sponge can be separated again.

Further, as a separation method using the apparatus shown in FIGS. 6 and 7, when titanium is re-separated, first, titanium sponge containing impurities is charged into the container 10 and heated. After that, the step of reducing the pressure in the container 10 is performed. Next, a step of precooling MgCl ₂ as an impurity emitted from the titanium sponge through the receiver 40 having the opening 42 located in the container 10 is performed. In addition, the first precipitating impurities are cooled and deposited in the recovery container 70.
Is performed. Further, a heating step of heating the recovery container 70 containing the precipitated impurities is performed. Then, a collecting step as a second depositing step of depositing and collecting the impurities melted by the heating step is performed. At this time, the recovery container 70 is inverted when the first precipitation step is transferred to the heating step.

Further, in the first precipitation step, the impurities are precipitated as solids, in the heating step the solids precipitated in the precipitation step are made into liquids, and in the precipitation step the impurities do not fall, but they are inverted and become liquid by the heating step. A plurality of baffle plates 80 having a shape capable of dropping impurities are disposed so that the impurities that have become liquid in the heating process are collected.

[0050]

EXAMPLE An example of the apparatus shown in FIGS. 8 and 9 is shown as an example. FIG. 8 shows a state in which the separator S shown in FIG. 9 is attached, the container 10 is arranged in the heating furnace 20, and the heating furnace 20 has a heater 21 incorporated therein.
The inside of the heating furnace 20 is connected to a pressure reducing device (vacuum device) via a pipe line 22 so that the pressure can be reduced. Also heating furnace 20
A measuring instrument is appropriately arranged at a predetermined position, and the temperature inside the furnace is measured, and the temperature inside the furnace is controlled based on the measured temperature. In case of re-separation, near the receiver (container 1
The heater 21 located on the upper side (0) is not energized. This makes it possible to soften the heating of the receiver part. The container 10 may be a known one.

The separating apparatus S of this example, as shown in FIG.
It is composed of a cooler 30, a receiver 40, and a connecting pipe 50. The cooler 30 has a substantially truncated cone shape,
A pipe line 32 connected to a vacuum pump is arranged on the upper side portion. A valve 32a is provided in the conduit 32.

A jacket 31 is provided on the outer periphery of the cooler 30.
Is provided, and a top plate jacket 31a is provided on the upper surface of the cooler 30, and a peripheral wall jacket 31b is provided on the outer circumference. Cooling water (not shown) circulates in these jackets 31. A baffle plate 33 is provided inside the cooler 30 to increase the contact area between the MgCl ₂ gas and the cooling part.

The receiver 40 is formed in the shape of a hollow circular tarai, and a plurality of heat shield plates 43 (three in this example) are arranged on the lower part of the tarai. And the heat shield plate 43
At an upper position, an opening 42 (in the case of titanium sponge, MgC) is formed in the side body of the receiver 40 as a gas flow port.
L ₂ gas) is formed in plural. Incidentally, according to the method of the present invention, it can be applied to the removal of impurities in metallic zirconium.

A hollow circular tarai-shaped projection 12 is formed on the lower portion of the lid 11 of the container 10 so as to be fitted with the receptacle 40. The tarai-shaped projection is provided on the receptacle 40. Are configured to join. Also the lid 1
A cooling jacket 31c is disposed on the upper part of the unit 1 and is configured to cool.

Therefore, as shown in FIG. 8, in the case of titanium, sponge titanium for re-separation is put into the container 10 and heated under vacuum to gasify MgCl ₂ to obtain the above-mentioned distribution. It enters into the receiver 40 through the opening 42 as a mouth, is cooled by the cooler 30, and is deposited or condensed. As a result, titanium sponge becomes
gCl ₂ can be separated and collected.

According to the configuration of this example, the separating device S is the container 1
Since it is configured to be connected via the lid 11 of 0, the disassembling of the separating device S is easy, and since the inside and outside of the lid 11 of the container 10 are used, they are located outside. The cooling device has excellent cooling efficiency.

(Specific Example) The following raw materials, separation device,
Re-separation was performed depending on the separation conditions. Titanium sponge was used as the sponge metal of the high melting point and high toughness metal. The container is made of SUS316 and has an internal volume of 12 m ³ , and the cooler is made of material SS.
(Mild steel) with an internal volume of 0.5 m ³ with a baffle inside, and the receiver is SS (mild steel) with an internal volume of 0.2 m ³ and an opening on the side (Gas distribution hole)
I used that.

The raw materials, separation conditions, etc. were as set forth in Table 1.

[Table 1]

The products obtained were as shown in Table 2 below.

[Table 2] The "other" at the recovery position is a portion such as between the receiver and the lid.

Table 3 below shows a comparison with the conventional example in terms of volumetric efficiency.

[Table 3] From the above results, it was found that the volumetric efficiency of the re-separation according to the present invention is about 10 times higher than that of the conventional method.

[Brief description of drawings]

FIG. 1 is an explanatory diagram showing a schematic configuration of a separation device of the present invention.

FIG. 2 is an explanatory diagram of a configuration of a cooler.

FIG. 3 is a diagram illustrating the configuration of another cooler.

FIG. 4 is a configuration explanatory view of still another cooler.

FIG. 5 is an explanatory diagram of a configuration of a receiver.

FIG. 6 is a schematic configuration diagram of a separation device including a recovery container.

FIG. 7 is an explanatory diagram showing a state in which the recovery container is inverted.

FIG. 8 is a configuration diagram showing a container provided with a separating device.

9 is a schematic perspective view of the separation device of FIG.

[Explanation of symbols]

10 containers 11 lid 30 cooler 31 jacket 32 Suction port 33 baffle 35 First Room 36,38,39 Connection pipe 37 Second Room 40 receiver 41,42 opening 43 Heat shield 50 connecting pipe 61 Cover 61a substrate 61b hanging part 63, 64 tube 67,68 Connection part 70 Collection container 72 Cooling device 74 heating furnace 80 baffle 81 Baffle board 82 Mountain-shaped baffle 83 Communication hole (communication hole) S separation device

─────────────────────────────────────────────────── ─── Continuation of front page (56) Reference JP-A-57-79134 (JP, A) JP-A-61-217539 (JP, A) JP-A-63-176440 (JP, A) JP-A-5- 43956 (JP, A) Japanese Patent Publication 31-9953 (JP, B1) (58) Fields investigated (Int.Cl. ⁷ , DB name) C22B 1/00-61/00

Claims (10)

(57) [Claims] 1. A separator attached to a container having a lid, comprising a jacket for circulating a cooling medium and a cooler having a suction port connected to a suction device, and a receiver having an opening. The cooler is installed outside the container of the lid, the receiver is installed inside the container of the lid, and communicates with the container through the opening, and the cooler is provided. A device for separating impurities in a metal, characterized in that the receiver is connected by a connecting pipe. 2. The device for separating impurities in a metal according to claim 1, wherein at least one baffle plate is provided inside the cooler. 3. The inside of the cooler is divided into a plurality of rooms, each room is connected by a connecting pipe projecting upward in the room, and is connected above the connecting pipe via a space. The device for separating impurities in a metal according to claim 1 or 2, wherein a cover portion that covers the tube is formed. 4. The separation of impurities in the metal according to claim 1, wherein the receiver is provided with a heat shield plate below an opening communicating with the container. apparatus. 5. A separation device connected to a container, the receiver having an opening located in the container, a jacket for communicating with the receiver and a cooling medium for circulating a cooling medium for precooling, and a suction port. And a collection container connected to the cooling device, and a removable suction device is connected to the collection container, so that cooling and heating can be selectively performed. Characteristic device for separating impurities in metals. 6. A plurality of baffle plates each having a shape in which impurities are deposited during cooling, and liquid impurities are melted and fallable during heating are disposed inside the recovery container. The device for separating impurities in a metal according to claim 5. 7. A cooler of a separation device, comprising: a cooler having a jacket and a suction port for circulating a cooling medium; and a receiver having an opening, wherein the cooler and the opening communicate with each other. To the outside of the container, respectively to attach the receiver to the inside of the container, the step of introducing metal into the container and heating the container under reduced pressure or vacuum to remove impurities from the metal, A step of condensing the impurities in a cooler of the apparatus and collecting the impurities in the receiver. 8. A step of charging a metal into a container and heating the container under reduced pressure or a vacuum, a receiver positioned in the container, and communicating with the receiver,
Precooling impurities emitted from the metal through a cooler having a jacket and a suction port through which a cooling medium for precooling flows, and cooling the precooled impurities to flow the cooling medium A first precipitation step of depositing in a recovery container equipped with a jacket, a heating step of heating the recovery container in which the precipitated impurities are present, and a second step of depositing impurities melted by the heating step from the recovery container. 2. A method for separating impurities in a metal, comprising the step of depositing 2. 9. The method for separating impurities in a metal according to claim 8, wherein the recovery container is inverted when the process proceeds from the first precipitation process to the heating process. 10. A recovery container is provided in which a plurality of baffle plates are arranged so that impurities are not dropped in the first precipitation step but are turned into a heating step to drop impurities that are liquid. In the first precipitation step, the impurities are precipitated as a solid, in the heating step, the solid precipitated in the first precipitation step is made into a liquid, and in the second precipitation step, the impurities turned into a liquid by the heating step. The method for separating impurities in a metal according to claim 9, characterized in that