CN213326724U - Device of hydrogen is used in hydrogenation of purification tantalum niobium metal - Google Patents

Device of hydrogen is used in hydrogenation of purification tantalum niobium metal Download PDF

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CN213326724U
CN213326724U CN202021995846.0U CN202021995846U CN213326724U CN 213326724 U CN213326724 U CN 213326724U CN 202021995846 U CN202021995846 U CN 202021995846U CN 213326724 U CN213326724 U CN 213326724U
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tank
hydrogen
purification tank
cooling
purification
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CN202021995846.0U
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李慧
郑培生
马海燕
陈学清
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Ningxia Orient Tantalum Industry Co Ltd
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Ningxia Orient Tantalum Industry Co Ltd
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Abstract

The application provides a device for purifying hydrogen for tantalum/niobium metal hydrogenation, which comprises a purification tank and a cooling tank, wherein a heating furnace wire is arranged around the outer wall of the purification tank; a plurality of sodium block adsorbers are arranged in the purification tank through a fixer, each sodium block adsorber comprises a sodium block and a crucible, the sodium block is placed in the crucible, and the crucible is arranged on the fixer; a hydrogen source air inlet is arranged on the purification tank, and a cooling hydrogen outlet is arranged at the top of the cooling tank; the purification tank comprises a tank body and a tank cover which are detachably arranged, and the tank cover is arranged on the top surface of the tank body; the cooling tank is connected with a cooling water tank body which is arranged on the upper edge of the purification tank. In the application, the sodium block is arranged in a crucible in the device, and molten sodium can react with oxygen and water in the hydrogen to generate sodium oxide or hydroxide and the hydrogen by heating a heating furnace wire around the outer wall of the purification tank to 100-300 ℃, so that the oxygen and water contained in the hydrogen are removed.

Description

Device of hydrogen is used in hydrogenation of purification tantalum niobium metal
Technical Field
The application relates to the technical field of tantalum/niobium metal hydrogenation, in particular to a device for purifying hydrogen for tantalum/niobium metal hydrogenation.
Background
The tantalum/niobium metal hydrogenation process is widely applied to the tantalum-niobium metallurgical industry. The hydrogenation process has high requirements on the purity of hydrogen, and particularly has specific requirements on the content of oxygen and water in the hydrogen. When the oxygen and water content in the hydrogen is higher, dense metals such as tantalum/niobium sintered rods and smelting ingots can be subjected to oxidation reaction with the oxygen and water to generate a protective oxide film, the oxide film can prevent the hydrogen from permeating into the metal and reduce the hydrogen absorption amount, so that the hydrogenation effect of the final metal is influenced, and the tantalum/niobium ingot after hydrogenation can be in the form of blocky crystals, unobvious layering, insufficient intermediate hydrogenation and the like. Therefore, it is desirable to purify the tantalum/niobium metal hydride with hydrogen to have an oxygen content of 0.3ppm or less and a dew point of < -76 ℃.
At present, in the traditional technology, there are various devices for hydrogen purification, for example, a purification cylinder for continuously purifying hydrogen is produced, zirconium-based alloy powder is used for adsorbing and purifying impurities in hydrogen, the oxygen content of hydrogen purified by the scheme is less than 0.7ppm, and the requirement of hydrogen for tantalum/niobium metal hydrogenation on the oxygen content cannot be met; as another example, a method for purifying hydrogen by water electrolysis and a device for implementing the method are proposed in the related art, which have a complicated structure and insufficient oxygen removal capability and cannot meet the purity requirement of hydrogen for tantalum/niobium metal hydrogenation.
In view of the above, it is desirable to provide a hydrogen purification device which has a simple structure and is easy and convenient to operate, and can meet the requirement of hydrogen purity for hydrogenation of tantalum/niobium metal.
SUMMERY OF THE UTILITY MODEL
The application provides a device of hydrogen is used in hydrogenation of purification tantalum/niobium metal to the purification can satisfy hydrogen is used in the hydrogenation of tantalum/niobium metal, thereby satisfies the hydrogenation requirement of tantalum/niobium metal.
The technical scheme adopted by the application for solving the technical problems is as follows:
a device for purifying hydrogen for tantalum/niobium metal hydrogenation comprises a purification tank, a cooling tank and a heating furnace wire, wherein the heating furnace wire is arranged around the outer wall of the purification tank, and the cooling tank is arranged on the top surface of the purification tank and is communicated with the purification tank through a pipeline;
a plurality of sodium block adsorbers are arranged in the purification tank through a fixer, each sodium block adsorber comprises a sodium block and a crucible, the sodium block is placed in the crucible, and the crucible is arranged on the fixer;
a hydrogen source air inlet is formed in the purification tank, and a cooling hydrogen outlet is formed in the top of the cooling tank;
the purification tank comprises a tank body and a tank cover which are detachably arranged, and the tank cover is arranged on the top surface of the tank body;
the cooling tank is connected with a cooling water tank body, and the cooling water tank body is arranged on the upper edge of the purification tank.
Optionally, the hydrogen source air inlet is arranged at the bottom of the purification tank;
the fixer includes first baffle, second baffle, third baffle and fourth baffle, the one end of first baffle, second baffle, third baffle and fourth baffle all with purification jar inner wall is perpendicular, and follows purification jar radial direction forms the runner structure of buckling.
Optionally, the first partition plate, the second partition plate, the third partition plate and the fourth partition plate are respectively fixed on the inner wall of the purification tank through support rods.
Optionally, the hydrogen source inlet is arranged at the top of the purification tank, and sends a hydrogen source to the inner bottom of the purification tank through an L-shaped hydrogen drainage pipe, and a transverse part of the L-shaped hydrogen drainage pipe is provided with a plurality of openings;
the sodium block adsorber is characterized in that the fixator is of a layer-by-layer support structure and is fixed on the inner bottom surface of the purification tank through support legs, and the sodium block adsorber is placed on the support structure layer by layer.
Optionally, a circulating cooling water pipeline or a forced cooling cold well is arranged in the cooling tank.
Optionally, an oxygen and dew point online detector is arranged at the cooling hydrogen outlet.
Optionally, the hydrogen source air inlet is connected with a high-purity hydrogen source, and the high-purity hydrogen is hydrogen meeting the standard GB/T3634-2011.
The technical scheme provided by the application comprises the following beneficial technical effects:
the application provides a device for purifying hydrogen for tantalum/niobium metal hydrogenation, which comprises a purification tank and a cooling tank, wherein a heating furnace wire is arranged around the outer wall of the purification tank; a plurality of sodium block adsorbers are arranged in the purification tank through a fixer, each sodium block adsorber comprises a sodium block and a crucible, the sodium block is placed in the crucible, and the crucible is arranged on the fixer; a hydrogen source air inlet is arranged on the purification tank, and a cooling hydrogen outlet is arranged at the top of the cooling tank; the purification tank comprises a tank body and a tank cover which are detachably arranged, and the tank cover is arranged on the top surface of the tank body; the cooling tank is connected with a cooling water tank body which is arranged on the upper edge of the purification tank. In the device for purifying the hydrogen gas for tantalum/niobium metal hydrogenation, the sodium block is arranged in the crucible, the heating furnace wire around the outer wall of the purification tank is heated to 100-300 ℃, so that the sodium block is heated to be in a molten state, and the molten sodium can react with oxygen and water in the hydrogen gas to generate sodium oxide or hydroxide and the hydrogen gas, thereby removing the oxygen and water contained in the hydrogen gas. The device in the application has the advantages of simple integral structure and low maintenance cost, and can effectively remove the oxygen and water content in the hydrogen to obtain the hydrogen meeting the hydrogenation requirement of tantalum/niobium metal.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without any creative effort.
FIG. 1 is a schematic diagram of an apparatus for purifying hydrogen for hydrogenation of tantalum/niobium metal provided in the examples of the present application;
FIG. 2 is a schematic view of another embodiment of an apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation according to the present disclosure;
FIG. 3 is a schematic diagram of an embodiment of an apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation according to the present disclosure.
Description of reference numerals:
110-pipeline, 120-cooling tank, 130-cooling hydrogen outlet, 200-purification tank, 210-tank cover, 220-tank body, 231-first partition plate, 232-second partition plate, 233-third partition plate, 234-fourth partition plate, 240-crucible, 250-hydrogen source air inlet, 260-cooling water tank body, 270-sodium block, 280-heating furnace wire, 290-support structure, 251-L type hydrogen gas drainage tube and 300-hydrogenation furnace.
Detailed Description
In order to make the technical solutions in the present application better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application; it is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In order to meet the purity requirement of the hydrogenation process of tantalum/niobium metal on hydrogen, the embodiment of the application provides a device for purifying hydrogen for hydrogenation of tantalum/niobium metal, the hydrogen purified by the device can meet the hydrogenation requirement of tantalum/niobium metal, the oxygen content in the purified hydrogen is less than or equal to 0.3ppm, and the dew point is less than-76 ℃.
The device for purifying hydrogen for tantalum/niobium metal hydrogenation provided by the embodiment of the application comprises a purification tank 200 with a heating furnace wire 280 arranged around the outer wall, and a cooling tank 120 arranged on the top surface of the purification tank 200 and communicated with the purification tank 200 through a pipeline 110;
a plurality of sodium block adsorbers are arranged in the purification tank 200 through a holder, each sodium block adsorber comprises a sodium block 270 and a crucible 240, the sodium block 270 is placed in the crucible 240, and the crucible 240 is arranged on the holder;
a hydrogen source air inlet 250 is arranged on the purification tank 200, and a cooling hydrogen outlet 130 is arranged at the top of the cooling tank 120;
the purification tank 200 comprises a tank body 220 and a tank cover 210 which are detachably mounted, wherein the tank cover 210 is mounted on the top surface of the tank body 220;
the cooling tank 120 is connected with a cooling water tank 260, and the cooling water tank 260 is arranged on the upper edge of the purification tank 200.
In the embodiment of the application, the sodium block 270 is arranged in the crucible 240 in the device for purifying the hydrogen for tantalum/niobium metal hydrogenation, the heating furnace wire 280 around the outer wall of the purification tank 200 is heated to 100-300 ℃, so that the sodium block 270 is heated to be in a molten state, and the molten sodium can react with oxygen and water in the hydrogen to generate sodium oxide or hydroxide and the hydrogen, thereby removing the oxygen and water contained in the hydrogen. The device in the embodiment of the application has the advantages of simple integral structure and low maintenance cost, and can effectively remove the oxygen and water content in the hydrogen to obtain the hydrogen meeting the hydrogenation requirement of tantalum/niobium metal.
Specifically, the following two structures can be respectively set:
example 1
As shown in fig. 1, the apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation provided in this embodiment comprises a purification tank 200 having a heating wire 280 disposed around the outer wall thereof, and a cooling tank 120 disposed on the top surface of the purification tank 200 and communicating with the purification tank 200 via a pipe 110;
a plurality of sodium block adsorbers are arranged in the purification tank 200 through a holder, each sodium block adsorber comprises a sodium block 270 and a crucible 240, the sodium block 270 is placed in the crucible 240, and the crucible 240 is arranged on the holder;
a hydrogen source air inlet 250 is arranged on the purification tank 200, and a cooling hydrogen outlet 130 is arranged at the top of the cooling tank 120;
the purification tank 200 comprises a tank body 220 and a tank cover 210 which are detachably mounted, wherein the tank cover 210 is mounted on the top surface of the tank body 220;
the cooling tank 120 is connected with a cooling water tank 260, and the cooling water tank 260 is arranged on the upper edge of the purification tank 200.
The hydrogen source inlet 250 is disposed at the bottom of the purification tank 200;
the fixer comprises a first clapboard 231, a second clapboard 232, a third clapboard 233 and a fourth clapboard 234, wherein one end of the first clapboard 231, one end of the second clapboard 232, one end of the third clapboard 233 and one end of the fourth clapboard 234 are all vertical to the inner wall of the purification tank 200, and a bent flow passage structure is formed along the radial direction of the purification tank 200.
The first partition 231, the second partition 232, the third partition 233 and the fourth partition 234 are fixed to the inner wall of the purification tank 200 by support rods, respectively.
Example 2
As shown in fig. 2, the apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation provided in this embodiment comprises a purification tank 200 having a heating wire 280 disposed around the outer wall thereof, and a cooling tank 120 disposed on the top surface of the purification tank 200 and communicating with the purification tank 200 via a pipe 110;
a plurality of sodium block adsorbers are arranged in the purification tank 200 through a holder, each sodium block adsorber comprises a sodium block 270 and a crucible 240, the sodium block 270 is placed in the crucible 240, and the crucible 240 is arranged on the holder;
a hydrogen source air inlet 250 is arranged on the purification tank 200, and a cooling hydrogen outlet 130 is arranged at the top of the cooling tank 120;
the purification tank 200 comprises a tank body 220 and a tank cover 210 which are detachably mounted, wherein the tank cover 210 is mounted on the top surface of the tank body 220;
the cooling tank 120 is connected with a cooling water tank 260, and the cooling water tank 260 is arranged on the upper edge of the purification tank 200.
The hydrogen source inlet 250 is provided at the top of the purification tank 200 and feeds a hydrogen source to the inner bottom of the purification tank 200 through an L-shaped hydrogen guide tube 251, a lateral portion of the L-shaped hydrogen guide tube 251 being provided with a plurality of openings;
the fixer is a layer-by-layer bracket structure 290 and is fixed on the inner bottom surface of the purification tank 200 through supporting legs, and the sodium block adsorbers are placed on the bracket structure 290 layer by layer.
Optionally, in the above embodiment, a circulating cooling water pipeline or a forced cooling cold well is disposed in the cooling tank 120, so as to achieve the purpose of reducing the temperature of the purified hydrogen; an oxygen and dew point online detector is arranged at the cooling hydrogen outlet 130; the hydrogen source air inlet 250 is connected with a high-purity hydrogen source, and the high-purity hydrogen is hydrogen meeting the standard GB/T3634-2011.
As shown in fig. 3, a specific implementation of the apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation provided in application example 1 is schematically illustrated, wherein the tank body 220 of the purification tank 200, the tank cover 210 of the purification tank 200, the first partition 231, the second partition 232, the third partition 233 and the fourth partition 234 in the tank, the cooling tank 120, the pipeline 110 connecting the purification tank 200 and the cooling tank 120, the hydrogen source inlet 250, the cooling hydrogen outlet 130, and the crucible 240 are made of stainless steel, the purified high purity sodium block 270 is placed in the crucible 240, a sealing gasket is disposed between the tank body 220 of the purification tank 200 and the tank cover 210 and fastened by rivets, the cooling hydrogen outlet 130 is connected to the hydrogenation furnace 300 through a pipeline by a valve, and the hydrogen source inlet 250 is connected to the high purity hydrogen gas tank or the pipeline hydrogen through a pipeline. Before use, the purification tank 200 is evacuated and replaced, air in the purification tank 200 is pumped out and argon is filled in to protect the high-purity sodium block 270 from being oxidized by air, then the circulating water in the cooling water tank 260 arranged at the upper edge of the purification tank 200 is opened, and the purification tank 200 is heated such that the temperature within the purification tank 200 is maintained between 100 ℃ and 300 ℃, preferably 100 ℃ and 200 ℃, then the gas inlet valve arranged between the gas inlet 250 of the hydrogen source of the purification tank 200 and the high-purity bottled hydrogen or pipeline hydrogen is opened to enable the hydrogen to enter the tank 220 of the purification tank 200, after the hydrogen gas passes through the sodium metal blocks 270 on the crucibles 240 which are alternately and symmetrically placed to remove the lower content of oxygen and water contained in the hydrogen gas, the hydrogen gas is input into the cooling tank 120 through the pipeline 110 connecting the purification tank 200 and the cooling tank 120, cooled to room temperature, and then input into the hydrogenation furnace 300 through the pipeline to participate in the hydrogenation of the tantalum/niobium metal. The hydrogen of the high-purity bottled hydrogen or the pipeline hydrogen meets the standard GB/T3634-2011, the oxygen content is 0.5-1ppm, and experiments prove that the oxygen content of the hydrogen purified by the device is less than or equal to 0.3ppm and the dew point is less than-76 ℃.
It is noted that relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
It will be understood that the present application is not limited to what has been described above and shown in the accompanying drawings, and that various modifications and changes can be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.

Claims (7)

1. An apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation, comprising a purification tank (200) having a heating wire (280) disposed around the outer wall thereof, and a cooling tank (120) disposed on the top surface of the purification tank (200) and communicating with the purification tank (200) through a pipe (110);
a plurality of sodium block adsorbers are arranged in the purification tank (200) through a fixer, each sodium block adsorber comprises a sodium block (270) and a crucible (240), the sodium block (270) is placed in the crucible (240), and the crucible (240) is arranged on the fixer;
a hydrogen source air inlet (250) is arranged on the purification tank (200), and a cooling hydrogen outlet (130) is arranged at the top of the cooling tank (120);
the purification tank (200) comprises a tank body (220) and a tank cover (210), wherein the tank cover (210) is arranged on the top surface of the tank body (220);
the cooling tank (120) is connected with a cooling water tank body (260), and the cooling water tank body (260) is arranged on the upper edge of the purification tank (200).
2. The apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation according to claim 1, wherein the hydrogen source inlet (250) is disposed at the bottom of the purification tank (200);
the fixer comprises a first partition plate (231), a second partition plate (232), a third partition plate (233) and a fourth partition plate (234), wherein one end of each of the first partition plate (231), the second partition plate (232), the third partition plate (233) and the fourth partition plate (234) is perpendicular to the inner wall of the purification tank (200), and a bent flow passage structure is formed in the radial direction of the purification tank (200).
3. The apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation according to claim 2, wherein the first partition plate (231), the second partition plate (232), the third partition plate (233) and the fourth partition plate (234) are fixed to the inner wall of the purification tank (200) by support rods, respectively.
4. The apparatus for purifying hydrogen for tantalum/niobium metal hydrogenation according to claim 1, wherein the hydrogen source gas inlet (250) is provided at the top of the purification tank (200) and feeds a hydrogen source to the inner bottom of the purification tank (200) through an L-shaped hydrogen guide tube (251), the L-shaped hydrogen guide tube (251) having a lateral portion provided with a plurality of openings;
the fixer is a layer-by-layer bracket structure (290) and is fixed on the inner bottom surface of the purification tank (200) through supporting legs, and the sodium block adsorbers are placed on the bracket structure (290) layer by layer.
5. The apparatus for purifying hydrogen gas for tantalum/niobium metal hydrogenation according to claim 1, wherein the cooling tank (120) is provided with a circulating cooling water pipe or a forced cooling cold well.
6. The apparatus for purifying hydrogen gas for tantalum/niobium metal hydrogenation according to claim 1, wherein an oxygen and dew point on-line detector is disposed at the cooling hydrogen outlet (130).
7. The apparatus for purifying hydrogen gas for tantalum/niobium metal hydrogenation according to claim 1, wherein the hydrogen gas source inlet (250) is connected to a high purity hydrogen gas source, and the high purity hydrogen gas is hydrogen gas according to the standard GB/T3634-2011.
CN202021995846.0U 2020-09-14 2020-09-14 Device of hydrogen is used in hydrogenation of purification tantalum niobium metal Active CN213326724U (en)

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Application Number Priority Date Filing Date Title
CN202021995846.0U CN213326724U (en) 2020-09-14 2020-09-14 Device of hydrogen is used in hydrogenation of purification tantalum niobium metal

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