KR101839471B1 - Deoxidation apparatus for preparing titanium with low oxygen concentration - Google Patents

Abstract

The present invention relates to an improved titanium deoxidizing apparatus, which comprises: an inner container of which an upper portion is opened; and a separating cut disposed in the perpendicular direction to the axial direction of the inner container and having a first mesh of which an outer circumference surface is integrally fixed on an inner circumference surface of the inner container to allow the inner container to be divided into an upper portion wherein titanium is stored and a lower portion wherein a deoxidizing agent is stored. Therefore, the separating cut enables the deoxidizing agent evaporated by heat to come in contact with the titanium stored in the upper portion while passing through the first mesh, thereby deoxidizing the titanium. According to the present invention, the upper portion and the lower portion can be divided through the separating cut which is integrally formed in the inner container. Moreover, the titanium and the deoxidizing agent can be disposed in the portions, respectively, to enable the evaporated calcium steam and titanium powder to be effectively responded.

Description

[0001] The present invention relates to an improved titanium deoxidation apparatus,

The present invention relates to an improved titanium deoxidation apparatus, and more particularly to an improved titanium deoxidation apparatus capable of promoting the deoxidation of titanium by activating the contact of titanium with a deoxidizer.

Titanium (Ti) is a very lightweight, durable and corrosion-resistant material. For this reason, titanium is used in various fields such as aerospace, marine equipment, chemical industry, nuclear power, biomedical, and automobile.

Commercial titanium contains approximately 2,000 ppm to 10,000 ppm of oxygen. Therefore, much research has been conducted to produce titanium of higher purity.

Studies on the high purity of titanium have been mainly focused on the development of deoxidation processes by controlling gas impurities.

As a method of reducing oxygen in titanium through such a deoxidation process, a method of dissolving calcium (Ca) by using a halide-based flux such as calcium chloride (CaCl 2) and dissolving calcium oxide (CaO) A method has been proposed. However, the method using a halide-based flux has a problem that a complicated mechanical process such as crushing after deoxidation is required, and in the case where the raw material is a powder, there is a problem that it is difficult to recover a sound powder by applying the process.

In order to solve these problems, Jim Jae Won et al. Disclosed a Korean Patent No. 10-1135160 (deoxidation apparatus for producing a low-oxygen titanium powder, inventor, Jae Won et al. 4), and disclosed a deoxidation apparatus for producing a low-oxygen titanium powder have.

The disclosed deoxidation apparatus for producing titanium oxide powder has a structure in which one vessel is formed by joining the upper vessel 11 and the lower vessel 12 with the connecting material 13 and a sheave 20 is disposed at the lower end of the upper vessel 11 Deoxidizer (De) is disposed at the lower end of the lower vessel (12) to contact deoxidized deoxidizer and titanium (Ti), thereby deoxidizing the deoxidizer to increase the recovery of the powdery raw material.

However, Korean Patent No. 10-1135160 discloses a structure in which the upper container 11 and the lower container 12 are separated from each other in order to dispose the sheave 20 and a lower container It is troublesome to replace the disposable container 14 continuously.

In addition, when titanium is formed as powder, the evaporated deoxidizer formed in the lower vessel is prevented from being smoothly supplied to the upper portion of the titanium powder by blocking the sheath, thereby making it difficult to contact the deoxidizer with titanium.

(Korean Patent No. 10-1135160, April 03, 2012)

It is an object of the present invention to provide a method of manufacturing a high purity titanium by integrating a manufacturing vessel and a separating gut for manufacturing titanium with high purity to reduce the manufacturing cost of the vessel and promote contact between the deoxidizer and titanium to obtain high purity titanium Titanium deoxidation apparatus.

The objects of the present invention are not limited to the above-mentioned objects, and other objects not mentioned can be clearly understood by those skilled in the art from the following description.

According to an aspect of the present invention, there is provided an improved titanium deoxidation apparatus for deoxidizing titanium to produce hypoxic titanium according to an embodiment of the present invention. And a first mesh which is disposed in a direction perpendicular to the axial direction of the inner container and whose outer circumferential surface is integrally fixed to the inner circumferential surface of the inner container to divide the inner container into an upper region containing titanium and a lower region containing deoxidizer, And the deoxidizing agent evaporated by the second deoxidizing agent is passed through the first mesh and brought into contact with the titanium contained in the upper region so that titanium is deoxidized.

The microsieve may be formed of a second mesh having a size smaller than that of the first mesh when the titanium is in powder form.

Here, at least one of the ring slit portions protruding into the upper region and the lower region through the first mesh and the second mesh to form a deoxidizing gas flow path so that the deoxidizing agent evaporated by heating is increased to the upper region .

Here, the inner container may have a cap that seals the open top.

Here, the container may further include an outer container for receiving the inner container.

Here, the inner vessel may be formed of a stainless steel material to facilitate the cleaning of the deoxidizer.

The improved titanium deoxidation apparatus according to the present invention separates an upper region and a lower region through a separating gut formed integrally in an inner vessel and arranges titanium and a deoxidizer in each of them, so that the reaction between titanium and vaporized calcium vapor and titanium powder So that high purity titanium can be formed.

The effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned can be clearly understood by those skilled in the art from the following description.

1 is a view showing a conventional deoxidation apparatus.
2 is a diagram of an improved titanium deoxidation apparatus in accordance with an embodiment of the present invention.
3 is a diagram of an improved titanium deoxidation apparatus having a ring sleeve according to an embodiment of the present invention.
Figure 4 is a view of a detachable gusset according to one embodiment of the present invention.
5 is a diagram illustrating an improved titanium deoxidation apparatus according to another embodiment of the present invention.
6 is a detailed view showing a ring sleeve according to another embodiment of the present invention.
FIGS. 7A to 7C are graphs showing results of oxygen reduction experiments according to temperature of an improved titanium deoxidation apparatus according to an embodiment of the present invention. FIG.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. Note that, in the drawings, the same components are denoted by the same reference symbols as possible. Further, the detailed description of known functions and configurations that may obscure the gist of the present invention will be omitted. For the same reason, some of the components in the drawings are exaggerated, omitted, or schematically illustrated.

Also, throughout the specification, when an element is referred to as " including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise. Also, throughout the specification, the term " on " means located above or below a target portion, and does not necessarily mean that the target portion is located on the upper side with respect to the gravitational direction.

FIG. 2 is a view of an improved titanium deoxidation apparatus according to an embodiment of the present invention, and FIG. 3 is a view of an improved titanium deoxidation apparatus having a ring slit section according to an embodiment of the present invention, Fig. 2 is a view showing a detachable gusset according to an embodiment of the present invention.

2 through 4, an improved titanium deoxidizer according to an embodiment of the present invention includes an inner vessel 110, a separation gut 120, a microsieve 130, and a ring sleeve 140 .

The inner container 110 is formed by opening the upper portion and has a cap 113 for sealing the opened upper portion. The cap 113 is convex upward and may further include a pressing member 115 to closely contact the cap 113 along the upper circumferential surface of the inner container 110.

The inner container 110 is preferably made of stainless steel. The inner container 110 formed of stainless steel can be easily cleaned by the tap water to remove the deoxidizing agent even when the deoxidizer De described below is pressed against the bottom of the inner container 110 by heating, Can be continuously recycled, thereby reducing the maintenance cost.

The separating gut 120 is provided with the first mesh 121 and arranged in a direction perpendicular to the axial direction of the inner container 110. The outer circumferential surface of the separating gut 120 is integrally formed with the inner circumferential surface of the inner container 110 . Therefore, the separating gut 120 divides the inner vessel 110 into an upper region 111 containing titanium (Ti) and a lower region 112 containing a deoxidizer (Ca), and a deoxidizer Deoxidation of titanium (Ti) can be performed by contacting the titanium (Ti) contained in the upper region (111) while passing through the first mesh (121).

That is, the separating gut 120 is integrally bonded to the inner container 110 in which the upper region 111 and the lower region 112 are integrally formed, whereby the upper region 111 containing titanium Ti and the deacidifying agent De ), And promote the deoxidation of titanium. Here, deoxidizer (De) may be formed of calcium.

At this time, the size of the first mesh 121 is smaller than that of bulk titanium, and the shape of the first mesh 121 is formed in a zigzag shape so that bulk titanium (Ti) falls into the lower region 112 Can be effectively prevented.

A microsieve 130 may further be disposed on the upper side of the separable gut 120. The detachable gut 120 may serve to support the microsieve 130. The microsieve 130 is formed of a second mesh smaller than the first mesh 121. Therefore, when the titanium is powder, it is possible to prevent the powdered titanium from falling down through the second mesh.

At this time, the microsieve 130 may be formed to have a size of 80 to 140 mesh, and the size of the powdered titanium is larger than that of the microsphere 130.

As described above, the separate gut 120 and the microsieve 130 can appropriately deoxidize titanium by selectively combining them according to the size of titanium.

At least one of the ring sliver portion 140 and the ring-shaped sliver portion 140 may be formed in the first mesh 121 and the second mesh of the microsieve 130 so that the supply of the deoxidizer De evaporated by heating is increased from the lower side to the upper region 111 And protrudes toward the upper region 111 and the lower region 112 to guide smooth movement of the deoxidized gas. Therefore, titanium (Ti) can be activated by contact with deoxidized gas, thereby facilitating deoxidation.

At this time, the ring sleeves 140 are arranged in a plurality of radial directions at the center of the inner container 110 formed in a cylindrical shape, and may be disposed at intervals of 60 degrees about the radial direction. The ring sleeve 140a and the ring sleeve 140b disposed in the radial direction are arranged at intervals of 30 degrees from each other so as to supply deoxidized gas so that the contact with the titanium disposed on the separable gut 120 is uniform and smooth. Thereby facilitating the deoxidation of titanium and forming high purity titanium.

As described above, the ring sleeve 140 according to the embodiment of the present invention is formed in the lower region 112 by communicating the upper region 111 and the lower region 112 through the first mesh 121 and the second mesh, The deoxidizing gas is smoothly transferred to the upper region 111 to increase the contact between the deoxidized gas and the titanium, so that the reaction between the calcium vapor and the titanium powder can be efficiently performed to form a high purity titanium.

Meanwhile, it is possible to further include an outer container 150 that receives the inner container 110. The outer vessel 150 serves to prevent the deoxidized steam that may be finely discharged from the inner vessel 110 from flowing out to the outside and may include an outer vessel cap 160 that hermetically closes the outer vessel 150 have.

FIG. 5 is a view of an improved titanium deoxidation apparatus according to another embodiment of the present invention, and FIG. 6 is a detailed view showing a ring sleeve according to another embodiment of the present invention.

Referring to FIGS. 5 and 6, an improved titanium deoxidation apparatus according to another embodiment of the present invention will be described in more detail. Hereinafter, the cap 113 and the ring sleeve 140 will be described in detail, and redundant descriptions are the same as those described above, and therefore, a detailed description thereof will be omitted.

The inner container 110 is provided with an adapter 116 protruding from the upper end toward the inner radius so as to have a smaller inner diameter to provide a tight seal with the cap 113. The adapter 116 is formed with a groove 116a from the upper side to the lower side.

The cap 113 has a protrusion 113a corresponding to the groove 116a and the protrusion 113a is fitted in the groove 116a so that the inner container 110 and the cap 113 are engaged with each other, It is possible to prevent the deoxidation gas in the fuel cell 110 from flowing out to the outside as much as possible. At this time, a silicon coating (not shown) is formed on the inner circumferential surface of the groove 116a, so that the adhesion between the protrusion 113a and the groove 116a can be further increased when the protrusion 113a is fitted.

Accordingly, since the cap 113 is fixed to the inner vessel 110, the cap 113 can be prevented from being separated by the internal pressure and tightly adhered to prevent leakage of vaporized calcium deoxidant, thereby effectively deoxidizing titanium .

The ring sleeve 140 can be formed by the venturi tube 141 and the branch tube 142 in the radial direction at the discharge end.

The ring sleeve 140 having the venturi pipe 141 can induce a deoxidizing gas smoothly upward without a separate suction device. At this time, the branch pipes 142 are disposed at intervals of 60 degrees along the circumferential direction, and the branch pipes 142 are disposed on the upper side of the loaded titanium.

Accordingly, the branch tube 142 disposed in the radial direction around the ring sleeve 140 uniformly supplies deoxidized gas evaporated around the ring sleeve 140, thereby promoting deoxidation of titanium, thereby forming high-purity titanium .

Accordingly, the branch pipe 142 smoothes the supply of the deoxidized gas around the ring sleeve 140, thereby more smoothly bringing the contact between the deoxidized gas and the titanium. At this time, since the titanium is located below the upper side of the ring sleeve 140, deoxidized gas discharged from the branch pipe 142 can induce smooth contact with titanium.

powder Titanium  Experiment

The deoxidation performance was compared through the oxygen content of titanium after deoxidation for the improved titanium deoxidation apparatus (example) and the conventional deoxidation apparatus (comparative example) according to the embodiment of the present invention. In this case, the embodiment is based on FIG. 3, and the comparative example can be understood as a deoxidizer registered in Korean Patent No. 10-1135160.

First, titanium powder and calcium (deoxidizing agent) were charged in each of Examples and Comparative Examples as shown in Table 1, respectively.

Table 1 shows the results of the experiments for the comparative examples and the examples in which the materials charged in Table 1 were subjected to deoxidation of titanium powder at a temperature of 1000 캜.

In the example, 59.8% of the oxygen was reduced from 2,000 ppm to 805 ppm in the raw materials (see FIG. 7A). In the comparative example, the oxygen content was changed from 2,200 ppm to 825 ppm to 62.5% The oxygen reduction ratio of the comparative example and the example was almost the same.

Thus, the oxygen reduction value in the example is reduced in the case where the amount of calcium charged is reduced by 50% as compared with that in the comparative example, and titanium deoxidation according to the embodiment is characterized in that the deoxidation effect can be maintained while the amount of calcium charged is greatly reduced .

bulk Titanium  Experiment

The deoxidation performance was confirmed by the titanium oxygen content after deoxidation for the improved titanium deoxidation apparatus (example) according to the embodiment of the present invention. In the conventional art (Korean Patent No. 10-1135160), since it is difficult to supply a deoxidizing agent smoothly to the bulk titanium, it has been difficult to carry out the deoxidation through the noncontact type of the bulk titanium.

In the following, titanium and calcium (deoxidizing agent) were charged in bulk form of pure titanium and Ti-6Al-V alloy according to the present invention on the basis of Table 3, respectively, and deoxidation performance was evaluated.

As shown in Table 4, it was confirmed that oxygen depletion of pure titanium and Ti-6Al-V alloy was 30.3% and 51.5%, respectively, when deoxidized at 1000 ° C compared to raw materials 7b and 7c).

As described above, the deoxidation apparatus according to the embodiment of the present invention can also deoxidize titanium through the noncontact system with respect to bulk titanium, thereby forming high purity titanium.

It should be noted that the embodiments of the present invention disclosed in the present specification and drawings are only illustrative of the present invention in order to facilitate description of the present invention and to facilitate understanding of the present invention and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that other modifications based on the technical idea of the present invention are possible in addition to the embodiments disclosed herein.

100: deoxidizer 110: inner vessel
111: upper region 112: lower region
113: cap 114: pressure member
120: separating gut 121: 1st mesh
130: microsieve 140: ring sleeve
150: outer container 160: outer container cap

Claims (6)

1. A deoxidation apparatus for producing titanium by deoxidizing titanium,
An inner container having an open top; And
A first mesh disposed in a direction perpendicular to an axial direction of the inner vessel and having an outer circumferential surface integrally fixed to an inner circumferential surface of the inner vessel to divide the inner vessel into an upper region containing titanium and a lower region containing deoxygenating agent Wherein the deoxidizing agent evaporated by heating is brought into contact with the titanium contained in the upper region while passing through the first mesh so that deoxidation of the titanium is performed; And
Further comprising a microsieve disposed on the separating gut and formed of a second mesh smaller than the first mesh. delete The method according to claim 1,
Wherein at least one of the first and second meshes penetrates through the first mesh and the second mesh so that the supply of the deoxidizer evaporated by heating is increased to the upper region, thereby forming a deoxidizing gas flow path; Wherein the titanium deoxidation apparatus further comprises: The method according to claim 1,
Wherein the inner container comprises:
And a cap to seal the open top. 5. The method of claim 4,
And an outer container for receiving the inner vessel. The method according to claim 1,
Wherein the inner container comprises:
Wherein the deoxidizing agent is formed of a stainless steel material to facilitate washing of the deoxidizer.

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