Molybdenum powder continuous production device and continuous production method

Abstract

The embodiment of the present invention discloses a continuous production device and a continuous production method of molybdenum powder; the production device includes: a reaction furnace tube, the reaction furnace tube includes a low-temperature zone, a high-temperature zone and a cooling zone arranged in sequence along the length direction of the reaction furnace tube; a gas distribution pipe assembly is arranged inside the reaction furnace tube along the length direction of the reaction furnace tube; the gas distribution pipe assembly is respectively provided with air holes adapted to the low-temperature zone and the high-temperature zone, for respectively introducing reaction gas into the low-temperature zone and the high-temperature zone; a reaction crucible is arranged in the reaction furnace tube; the reaction crucible is adapted to be arranged with the gas distribution pipe assembly, and the reaction gas introduced from the gas distribution pipe enters the interior of the reaction crucible from the bottom of the reaction crucible; a guide assembly is arranged along the length direction of the reaction furnace tube; the reaction crucible is adapted to be arranged on the guide assembly to guide the reaction crucible to move along the length direction of the reaction furnace tube; a drive assembly is used to drive the reaction crucible to move on the guide assembly; an exhaust assembly is arranged to be connected to the bottom of the reaction furnace tube, for discharging reaction tail gas.

Description

Technical Field

[0001] The invention belongs to the technical field of metal powder materials, and particularly relates to a continuous production device and a continuous production method for molybdenum powder. Background Art

[0002] Currently, the process for producing molybdenum powder using hydrogen reduction of molybdenum oxide, both domestically and internationally, is primarily based on a reactor-type reduction process. Domestic molybdenum powder reduction furnaces primarily include single-tube, four-tube, eight-tube, thirteen-tube, and fifteen-tube reduction furnaces. Imported molybdenum powder reduction furnaces primarily include single-stage reduction rotary kilns (USA), large-diameter muffle furnaces (Germany), and two-stage reduction furnaces with eighteen tubes.

[0003] The two-stage push-boat hydrogen reduction process for preparing molybdenum powder is currently widely used in the industry. The process is mainly divided into four stages. In the first stage, MoO3 powder is reduced in a hydrogen atmosphere at 450-650℃ to obtain intermediate products MoO2 and Mo4O 11 The first stage is the reduction of the product from the first stage, followed by cooling to room temperature and deagglomeration and screening. In the third stage, the deagglomeration and screening intermediate product is further reduced at 850-1050°C to obtain molybdenum powder. The molybdenum powder is screened in the fourth stage. Throughout the production process, hydrogen flows over the molybdenum trioxide or molybdenum dioxide layer, diffuses downward, and chemically reacts with the material. The generated water vapor diffuses upward, away from the reaction interface, and eventually flows out of the reduction furnace together with the unreacted hydrogen.

[0004] In the process of preparing molybdenum powder by two-stage push-boat hydrogen reduction, the product of the first stage experiences over-temperature sintering and agglomeration, hardening, and compaction, which increases the resistance to the continuous downward diffusion of hydrogen, not only reducing the reduction efficiency, but also increasing the screen material and reducing the yield. Usually, the first stage reduction product needs to undergo a series of complex processes such as boat discharge, deagglomeration, and screening, and then the raw powder particle size must be readjusted before it is raised to a high temperature again before the second stage reduction can be carried out. Therefore, the production cycle is long, the efficiency is low, the energy consumption is high, the yield is low, and the particle size is difficult to control. Through the research of this team, it was found that the diffusion of hydrogen and the overflow of water vapor in the reduction process are in opposite directions, interfering and hindering each other, which is the fundamental reason for the slow reduction rate, poor molybdenum powder performance, and the molybdenum powder particle size and oxygen content also changing with the thickness gradient of the material layer. Summary of the Invention

[0005] In view of this, in one aspect, some embodiments disclose a continuous molybdenum powder production device, the production device comprising:

[0006] The reaction furnace tube includes a low temperature zone, a high temperature zone and a cooling zone arranged in sequence along its length;

[0007] The gas distribution pipe assembly is arranged inside the reactor tube along the length direction of the reactor tube; the parts of the gas distribution pipe assembly located in the low temperature zone and the high temperature zone are respectively provided with air holes adapted to the low temperature zone and the high temperature zone, for respectively introducing the reaction gas into the low temperature zone and the high temperature zone;

[0008] The reaction crucible is arranged in the reaction furnace tube and is used to place the reaction materials. The reaction crucible is adapted to be arranged with the gas distribution pipe assembly, and the reaction gas introduced from the gas distribution pipe assembly enters the interior of the reaction crucible from the bottom of the reaction crucible.

[0009] The guide assembly is arranged inside the reaction furnace tube along the length direction of the reaction furnace tube; the reaction crucible is adapted to be arranged on the guide assembly to guide the reaction crucible to move along the length direction of the reaction furnace tube;

[0010] A driving assembly, used for driving the reaction crucible to move on the guide assembly;

[0011] The exhaust assembly is connected to the bottom of the reaction furnace tube and is used to discharge the reaction tail gas.

[0012] Furthermore, in some embodiments of the molybdenum powder continuous production device disclosed, the reaction furnace tube also includes a material thinning area arranged between the low-temperature zone and the high-temperature zone.

[0013] In the molybdenum powder continuous production device disclosed in some embodiments, the air distribution pipe assembly and the guide assembly are configured as the same assembly.

[0014] In some embodiments of the molybdenum powder continuous production device disclosed, the gas distribution pipe assembly includes:

[0015] An outer tube, wherein the upper wall of the outer tube is provided with air holes located in a high temperature zone and a low temperature zone;

[0016] The inner tubes are provided in plurality; the plurality of inner tubes are provided inside the outer tube; wherein one end of each inner tube is respectively provided to be connected to an air hole on the outer tube, and the other end of each inner tube is provided to be connected to an air source.

[0017] In some embodiments of the molybdenum powder continuous production device disclosed, the bottom of the reaction crucible is provided with a groove adapted to the outer tube, and a through hole is provided in the groove; when the groove of the reaction crucible is adapted to be installed on the outer tube, the position of the through hole corresponds to the air hole on the outer tube.

[0018] In the molybdenum powder continuous production device disclosed in some embodiments, the guide component is a guide rail, and the reaction crucible is provided with a structure adapted to the guide rail.

[0019] In some embodiments of the molybdenum powder continuous production device disclosed, a plurality of reaction crucibles are provided, and the plurality of crucibles are arranged in sequence and continuously, and are driven by a driving component to move intermittently and continuously to achieve continuous production of molybdenum powder.

[0020] In the molybdenum powder continuous production device disclosed in some embodiments, a material discharging assembly is provided inside the reaction furnace tube located in the material discharging area, and the material discharging assembly includes:

[0021] A fixing seat, arranged to be fixed on the upper wall of the reactor tube;

[0022] The material-dispersing plate is mounted on the fixed base via a retractable connector; the shape of the material-dispersing plate is adapted to the reaction crucible;

[0023] The driving component is used to drive the material separation plate to move.

[0024] In some embodiments of the molybdenum powder continuous production device disclosed, the exhaust assembly includes:

[0025] an exhaust pipe, arranged to communicate with the bottom of the reaction furnace tube;

[0026] The vacuum pump is connected to the exhaust pipe.

[0027] On the other hand, some embodiments disclose a method for continuously producing molybdenum powder, wherein the method comprises:

[0028] The reaction material is placed in the reaction crucible, and the driving assembly moves the reaction crucible along the guide assembly into the low-temperature zone of the reaction furnace tube; the gas distribution pipe assembly located in the low-temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the first stage reaction;

[0029] After the first stage reaction is completed, the driving assembly sends the reaction crucible along the guide assembly into the high temperature zone of the reaction furnace tube. The gas distribution pipe assembly located in the high temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the second stage reaction.

[0030] During the reaction process, the exhaust assembly discharges the tail gas from the bottom of the reaction furnace tube;

[0031] After the second stage reaction is completed, the driving component sends the reaction crucible into the cooling zone of the reaction furnace tube for cooling; molybdenum powder is collected;

[0032] The driving component intermittently and continuously delivers the reaction crucible into the reaction furnace tube to achieve continuous preparation of molybdenum powder.

[0033] The molybdenum powder continuous production device disclosed in the embodiment of the present invention is provided with a low-temperature zone, a high-temperature zone and a cooling zone in the reaction furnace tube, and the driving component is used to intermittently and continuously transport the reaction crucible into the reaction furnace tube to continuously carry out the first stage reaction and the second stage reaction, thereby realizing the continuous production of molybdenum powder; during the reaction process, the gas distribution pipe component inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to react with the solid material, so that the reaction gas and the water vapor generated by the reaction flow upward, which is conducive to the full contact between the reaction gas and the solid material, thereby improving the reaction efficiency, and effectively promoting the discharge of water vapor, which can effectively prevent the reaction material from hardening and agglomerating; discharging the reaction tail gas from the bottom of the reaction furnace tube is conducive to preferentially removing water vapor and reducing the water vapor partial pressure outside the crucible, which is not only conducive to promoting the reaction efficiency inside the powder, but also on the contrary, the water vapor outside the crucible reoxidizes the reduced powder. The molybdenum powder continuous production device can realize high-efficiency large-scale continuous production of molybdenum powder, and has good application prospects in the field of large-scale production and preparation of metal molybdenum powder. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 Example 1 Schematic diagram of the composition of a continuous production device for molybdenum powder;

[0035] Figure 2 Example 1 AA cross-sectional schematic diagram of a continuous molybdenum powder production device;

[0036] Figure 3 Example 1 Schematic diagram of the setting of the material discharging component of the continuous production device of molybdenum powder.

[0037] Reference numerals

[0038] 1. Reaction furnace tube 2. Reaction crucible

[0039] 3 Air pipe assembly 4 Exhaust assembly

[0040] 5 Drive assembly 6 Air source

[0041] 31 outer tube 32 inner tube

[0042] 7 Material layer of the material separation component 100 DETAILED DESCRIPTION

[0043] The term "embodiment" is used herein specifically to describe any embodiment as "exemplary," and should not be construed as superior or preferable to other embodiments. Performance indicators in the embodiments of the present invention were tested using conventional testing methods in the art, unless otherwise specified. It should be understood that the terms used in the embodiments of the present invention are intended solely to describe specific implementations and are not intended to limit the disclosure of the embodiments of the present invention.

[0044] Unless otherwise specified, the technical and scientific terms used herein have the same meanings as commonly understood by those skilled in the art to which the embodiments of the present invention pertain; any experimental methods and technical means not otherwise specified in the embodiments of the present invention refer to experimental methods and technical means commonly used by those skilled in the art.

[0045] As used herein, the terms "substantially" and "approximately" are used to describe small fluctuations. For example, they can refer to less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. Numerical data expressed or presented in range format herein are used for convenience and brevity only and should therefore be interpreted flexibly to include not only the values ​​explicitly listed as the limits of the range, but also all independent values ​​or subranges contained within the range. For example, a numerical range of "1-5%" should be interpreted to include not only the explicitly listed values ​​of 1% to 5%, but also the independent values ​​and subranges within the indicated range. Thus, included in this numerical range are independent values ​​such as 2%, 3.5%, and 4%, and subranges such as 1% to 3%, 2% to 4%, and 3% to 5%, etc. This principle also applies to ranges that only list a single value. Furthermore, this interpretation applies regardless of the width of the range or the characteristics described.

[0046] Throughout this document, including in the claims, transitional terms such as "comprises," "includes," "with," "having," "contains," "involving," and "accommodating" are understood to be open-ended, meaning "including but not limited to." Only the transitional terms "consisting of" and "composed of" are closed transitional terms.

[0047] In order to better illustrate the present invention, numerous specific details are provided in the following specific examples. It should be understood by those skilled in the art that the present invention can be practiced without certain specific details. In the examples, some methods, means, instruments, and equipment well known to those skilled in the art are not described in detail in order to highlight the main purpose of the present invention.

[0048] Under the premise of no conflict, the technical features disclosed in the embodiments of the present invention can be arbitrarily combined, and the resulting technical solutions belong to the contents disclosed in the embodiments of the present invention.

[0049] In some embodiments, the molybdenum powder continuous production apparatus comprises:

[0050] The reaction furnace tube includes a low-temperature zone, a high-temperature zone and a cooling zone arranged in sequence along its length; the reaction furnace tube is usually an integrated component, and the low-temperature zone, high-temperature zone and cooling zone required for the reaction are arranged in the same component, which is conducive to the continuous transportation of solid materials and continuous production; in the reaction furnace tube, the low-temperature zone, high-temperature zone and cooling zone are usually arranged in sequence according to the reaction needs to form different functional zones; different functional zones can be spaced at a certain distance to achieve a reasonable transition between the functional zones; usually the functional zones need to be set to a certain length so that the reaction crucible passing through each functional zone can stay for a suitable time to ensure that the set function is achieved. For example, when the material in the reaction crucible undergoes the first-stage reaction in the low-temperature zone, it needs to react at a set temperature for a set time to ensure that the first-stage reaction is completely carried out; when the material that completes the first-stage reaction enters the high-temperature zone, it needs to react at a set temperature for a set time to ensure that the second-stage reaction is completely carried out; after the reaction is completed, the product needs to be cooled in the cooling zone and needs to stay in the cooling zone for a sufficient time to reach a reasonable low temperature so that the product can be collected;

[0051] Typically, the reaction furnace tube is arranged in a reaction furnace body, and the reaction furnace body is used to heat the reaction furnace tube. Corresponding to the reaction furnace tube having a low temperature zone, a high temperature zone and a cooling zone arranged in sequence, the reaction furnace body also includes three zones, so that the temperature of the low temperature zone and the high temperature zone can be independently controlled so that different reaction zones can reach different reaction temperatures; at the same time, the cooling zone realizes the cooling of the material, and a forced cooling component can also be set, such as cooling with cold air or cold water;

[0052] The gas distribution pipe assembly is arranged inside the reaction furnace tube along the length direction of the reaction furnace tube; the parts of the gas distribution pipe assembly located in the low-temperature zone and the high-temperature zone are respectively provided with air holes adapted to the low-temperature zone and the high-temperature zone, which are used to respectively introduce reaction gas into the low-temperature zone and the high-temperature zone; the gas distribution pipe assembly for conveying reaction gas into the reaction furnace tube is usually arranged inside the reaction furnace tube, so that the reaction gas can be conveyed to different parts of the interior of the reaction furnace tube, and it can be ensured that the materials in the reaction crucibles reacting in the low-temperature zone and the high-temperature zone can fully contact the reaction gas; for this purpose, it is also necessary to provide a plurality of air holes on the gas distribution pipe assembly, and the air holes provided are respectively provided in the low-temperature zone and the high-temperature zone, and at the same time, the air holes provided in the low-temperature zone and the high-temperature zone should be reasonably arranged in positions so as to evenly convey the reaction gas to the materials in the reaction crucible, so that the reaction gas is fully and evenly contacted with the solid material, and the reaction is carried out evenly and efficiently;

[0053] The reaction crucible is arranged in the reaction furnace tube and is used to place the reaction materials. The reaction crucible is adapted to be arranged with the gas distribution pipe assembly, and the reaction gas introduced from the gas distribution pipe enters the reaction crucible from the bottom of the reaction crucible. The reaction crucible is a component for arranging solid materials and for the reaction between gas and solid materials. The materials are usually arranged outside the reaction furnace tube. The materials are arranged in the reaction crucible according to the set thickness and arrangement method, and then the reaction crucible is placed in the reaction furnace tube for further subsequent processes. The reaction crucible is usually adapted to be arranged with the gas distribution pipe assembly so that the reaction gas can be transported into the reaction crucible by using the gas distribution pipe assembly.

[0054] In some embodiments, a through hole is provided at the bottom of the reaction crucible, and the gas distribution pipe assembly transports the reaction gas to the through hole and into the reaction crucible; generally, the through holes provided at the bottom of the reaction crucible need to be set at a reasonable position and number so that when the reaction crucible is fed into the reaction furnace tube, they correspond to the gas holes of the corresponding gas distribution pipe assembly; when the reaction crucible is in the low temperature zone, the gas distribution pipe assembly in the low temperature zone transports the gas from its gas holes to the through hole of the reaction crucible; when the reaction crucible is in the high temperature zone, the gas distribution pipe assembly in the high temperature zone transports the gas from its gas holes to the through hole of the reaction crucible and into the reaction crucible;

[0055] A guide assembly is disposed inside the reaction furnace tube along the length of the reaction furnace tube; a reaction crucible is adapted to be disposed on the guide assembly to guide the movement of the reaction crucible along the length of the reaction furnace tube; the guide assembly is typically disposed inside the reaction furnace tube, covering a low-temperature zone, a high-temperature zone, and a cooling zone, so as to transport the reaction crucible to the low-temperature zone, the high-temperature zone, and the cooling zone; further, the reaction furnace tube includes a feed zone, and the guide assembly extends from the low-temperature zone to the feed zone of the reaction furnace tube, so as to place the reaction crucible on the guide assembly for material loading and placement in the reaction crucible; further, the guide assembly can extend from the cooling zone to the outside of the reaction furnace tube, so as to transport the reaction crucible away from the reaction furnace tube for product collection;

[0056] A drive assembly is used to drive the reaction crucible to move on the guide assembly. The drive assembly is usually arranged outside the reaction furnace tube. The drive assembly includes a fixed component, a power component, and a rod-shaped component. The rod-shaped component is driven by the power component to push the reaction crucible along the guide assembly, enter the reaction furnace tube, and move in the reaction furnace tube according to the set program.

[0057] The exhaust assembly is connected to the bottom of the reactor tube and is used to discharge the reaction exhaust gas. Usually, the reaction of preparing molybdenum powder will produce water vapor and some unreacted reaction gas, which need to be discharged from the reactor body in time to ensure the reaction is efficient and continuous. Usually, the exhaust assembly is connected to the bottom of the reactor tube and exhausts the exhaust gas from the bottom to the outside. Usually, among the exhaust gases containing water vapor, hydrogen, etc., water vapor has a lower distribution position than hydrogen due to its higher density and is mainly distributed in the lower part of the reactor tube. Setting an exhaust assembly connected to the bottom of the reactor tube is conducive to preferentially removing water vapor, improving the efficiency of removing water vapor, and preventing the occurrence of a hardening effect during the material reaction process.

[0058] In the molybdenum powder continuous production device disclosed in some embodiments, the reaction furnace tube also includes a material-dispersing zone arranged between the low-temperature zone and the high-temperature zone. In the first-stage reaction occurring in the low-temperature zone of the reaction furnace tube, the static material and its reaction products may be compacted to a certain extent, and may even cause unevenness in the gas channels inside the powder. The material-dispersing zone is provided after the low-temperature zone, and the products in the low-temperature zone can be loosened so that the first-stage materials that may be compacted have a suitable looseness, and the material layer has a suitable gap inside, which is sufficient to ensure that the material layer can fully contact with the reaction gas in the high-temperature zone, conduct an efficient and uniform reaction, and discharge the generated water vapor in time. The material-dispersing zone is also conducive to independently controlling the temperature of the low-temperature zone and the high-temperature zone to prevent mutual influence.

[0059] In some embodiments of the disclosed molybdenum powder continuous production apparatus, the gas distribution pipe assembly and the guide assembly are configured as a single component. Typically, the gas distribution pipe assembly and the guide assembly are configured as a single component, and the gas distribution pipe assembly can also serve as the guide assembly, thereby reducing the number of components in the reactor tube and simplifying the internal structure of the reactor tube.

[0060] In some embodiments of the molybdenum powder continuous production device disclosed, the gas distribution pipe assembly includes:

[0061] The outer tube has air holes located in the high temperature zone and the low temperature zone on its upper wall. A circular tubular component is usually used as the outer tube. The air holes are arranged at intervals on one side arc surface of the circular tubular component. When the outer tube is placed in the reaction furnace tube, the air holes are located at the top. The size of the air holes is adapted to the through holes on the reaction crucible, and the intervals between the air holes are consistent with the intervals between the through holes on the reaction crucible. The outer tube is usually provided with multiple air holes, which are reasonably distributed in the low temperature zone and the high temperature zone. In addition, the outer tube can usually be provided with multiple reaction crucibles, and the through holes on the multiple reaction crucibles respectively correspond to the air holes on the outer tube.

[0062] Multiple inner tubes are provided; the multiple inner tubes are arranged inside the outer tube; wherein one end of each inner tube is connected to a gas hole, and the other end of each inner tube is connected to a gas source. The inner tubes are usually arranged inside the outer tube and connected to the gas holes provided on the side wall of the outer tube. Each gas hole is connected to an inner tube, so that the reaction gas can be input into each gas hole through the inner tube and the ventilation status of each gas hole can be independently controlled. Typically, the other end of the inner tube is connected to the gas source, and each inner tube is provided with a gas control switch to control the flow and stop of gas in the inner tube.

[0063] In some embodiments of the molybdenum powder continuous production apparatus disclosed herein, the bottom of the reaction crucible is provided with a groove adapted to fit within the outer tube, and a through-hole is provided within the groove. When the reaction crucible is adapted to fit within the groove of the outer tube, the through-hole is positioned to correspond to the gas holes on the outer tube. Typically, the reaction crucible is adapted to fit within a gas distribution pipe assembly to allow reaction gas to enter the reaction crucible for reaction with solid materials.

[0064] In some embodiments, a groove is provided at the bottom of the reaction crucible, and the outer tube of the gas distribution pipe assembly can be adapted and provided in the groove. A through hole is provided in the groove as a gas channel between the reaction crucible and the gas distribution pipe assembly. On the one hand, the air holes on the outer tube are adapted to the through holes of the reaction crucible to allow the reaction gas to pass through. On the other hand, the outer tube provided in the groove does not hinder the movement of the reaction crucible in the reaction furnace tube, thereby realizing intermittent continuous movement of the reaction crucible, continuous feeding, and continuous production.

[0065] In some embodiments of the disclosed molybdenum powder continuous production apparatus, the guide assembly is a guide rail, and the reaction crucible is provided with a structure compatible with the guide rail. Typically, the guide rail is a linear component disposed within the reaction furnace tube, having longitudinal grooves or ridges disposed thereon. The reaction crucible is provided with longitudinal ridges or grooves that mate with these, allowing the reaction crucible to be positioned on the guide rail and guided along the length of the reaction furnace tube. Typically, a single guide rail or a plurality of guide rails can be provided, and correspondingly, the reaction crucible can be provided with one or more structures compatible with the guide rail.

[0066] In some embodiments, the guide assembly is a guide rail, and a structure adapted thereto is provided at the bottom of the reaction crucible. The guide rail is provided at the bottom of the reaction crucible, and the guide rail and the gas distribution pipe assembly are parallel to each other and located in the same horizontal plane.

[0067] In some embodiments, the guide assembly is two parallel guide rails, and a structure adapted to the guide rails is provided on each side of the reaction crucible. The guide rails are provided on both sides of the reaction crucible; the two guide rails are parallel to each other and located in the same horizontal plane.

[0068] In some embodiments of the molybdenum powder continuous production device disclosed, a plurality of reaction crucibles are provided, and the plurality of reaction crucibles are arranged in sequence and continuously, and intermittently and continuously moved under the drive of a driving component, thereby realizing continuous production of molybdenum powder. Generally, the intermittent continuous movement includes such a process that the driving component pushes the reaction crucible to move a set distance to reach a set position, the reaction crucible stays at the set position for a period of time, and then the driving component moves the reaction crucible again for a certain distance, and then stays for a period of time, so that intermittent movement of the reaction crucible can be realized; in order to realize continuous production, usually during the time when the driving component stops moving, a reaction crucible is added, materials are added therein, and then the added reaction crucible is moved synchronously with the reaction crucible that has been reacting in the reaction furnace tube; repeating this process can set a plurality of reaction crucibles that are adjacent to each other in sequence in the reaction furnace tube, and the plurality of reaction crucibles are intermittently moved in the reaction furnace tube at the same time, thereby realizing continuous movement of the reaction crucible, thereby realizing continuous production of molybdenum powder.

[0069] Some embodiments disclose a continuous production device for molybdenum powder, in which a plurality of reaction crucibles are provided, and the plurality of reaction crucibles are arranged in sequence and continuously, and are driven by a driving component to move continuously, thereby realizing continuous production of molybdenum powder. Generally, the continuous movement includes a process in which the driving component continuously pushes the reaction crucible to move at a certain speed, and the residence time in each temperature zone is the ratio of the temperature zone length to the movement speed. By independently setting the temperature of different temperature zones and setting the propulsion speed of the crucible, continuous reduction at different temperatures is respectively completed. When replacing the crucible, the cooling crucible at the rear end of the furnace body is first pulled out, leaving space for the crucible at the back to stay. This process does not affect the continuous movement of other crucibles in the furnace. After the driving component pushes the last crucible a distance of a crucible, the driving component first withdraws to the starting position in time, and then sends a new crucible into the reaction furnace tube. Finally, the driving component continues to push the new crucible into the reaction furnace tube at the same speed. Thereby, the continuous production of molybdenum powder is realized.

[0070] In some embodiments, the width of the reaction crucible is smaller than the width of the reaction furnace tube, and the length of the reaction crucible is smaller than the length of the low-temperature zone of the reaction furnace tube. For example, the length of the reaction crucible is half, one-third, one-quarter, or one-fifth of the length of the low-temperature zone of the reaction furnace tube. In this way, two, three, four, or five reaction crucibles can be arranged in the low-temperature zone of the reaction furnace tube. In actual production, the number of reaction crucibles may be greater. For example, the length of the reaction furnace tube, as well as the lengths of the low-temperature zone and the high-temperature zone of the reaction furnace tube, can be designed according to production needs, and the number of reaction crucibles can be further designed.

[0071] In some embodiments, the length of the reaction crucible is less than the length of the high-temperature zone in the reaction furnace tube. For example, the length of the reaction crucible is half, one-third, one-quarter, or one-fifth of the length of the high and low temperature zones in the reaction furnace tube. In this way, two, three, four, or five reaction crucibles can be set in the high-temperature zone of the reaction furnace tube.

[0072] In some embodiments, the lengths of the low-temperature zone and the high-temperature zone in the reaction furnace tube are set according to the reaction needs. If the reaction time in the low-temperature zone is required to be longer than the reaction time in the high-temperature zone, the length of the low-temperature zone can be set longer than the length of the high-temperature zone. If the reaction time in the low-temperature zone is required to be shorter than the reaction time in the high-temperature zone, the length of the low-temperature zone can be set less than the length of the high-temperature zone. Usually, the reaction crucible moves at the same speed in the reaction furnace tube under the push of the driving component. The residence time in the low-temperature zone of the reaction furnace tube is directly related to the length of the low-temperature zone and is proportional to the residence time in the high-temperature zone. The residence time in the cooling zone is proportional to the length of the cooling zone. The residence time in the material-dispersing zone is proportional to the length of the material-dispersing zone. Therefore, by adjusting the lengths of the high-temperature zone and the low-temperature zone, the residence time of the reaction crucible in the low-temperature zone and the high-temperature zone can be adjusted, that is, the reaction time of the reaction material in the low-temperature zone and the high-temperature zone can be adjusted.

[0073] In the molybdenum powder continuous production device disclosed in some embodiments, a material discharging assembly is provided within the material discharging area inside the reaction furnace tube, and the material discharging assembly includes:

[0074] A fixing seat, arranged to be fixed on the upper wall of the reactor tube;

[0075] The material-dispersing plate is mounted on the fixed base via a retractable connector; the shape of the material-dispersing plate is adapted to the reaction crucible; the material-dispersing plate is usually arranged parallel to the reaction crucible so that the material-dispersing plate is in uniform contact with the material layer in the reaction crucible, thereby loosening the reaction material;

[0076] The driving component is used to drive the material dispersing plate to move; usually, the driving component drives the material dispersing plate to move in the vertical direction of the reaction furnace tube. When it moves downward, it is close to the material layer, which can loosen the material layer. When it moves upward, it leaves the material layer and the reaction crucible to prevent it from interfering with the movement of the reaction crucible.

[0077] In some embodiments of the molybdenum powder continuous production device disclosed, the exhaust assembly includes:

[0078] An exhaust pipe is provided and communicated with the bottom of the reaction furnace tube; usually, multiple exhaust pipes are provided, each located at the bottom of the reaction furnace tube and distributed in various functional areas;

[0079] The vacuum pump is connected to the exhaust pipe. Usually, the vacuum pump is connected to the exhaust pipe to form a certain negative pressure in the exhaust pipe and the reaction furnace tube, which is conducive to the discharge of exhaust gas.

[0080] In some embodiments, a plurality of exhaust pipes are respectively arranged on both sides below the reaction furnace tube to form two rows of exhaust pipes. Each row of exhaust pipes is connected to a gas collecting pipe, and the two gas collecting pipes are connected to an exhaust pump.

[0081] Some embodiments disclose a method for continuously producing molybdenum powder, which uses a continuous molybdenum powder production device to produce molybdenum powder, comprising:

[0082] The reaction materials are placed in the reaction crucible, and the driving assembly sends the reaction crucible along the guide assembly into the low-temperature zone of the reaction furnace tube; the gas distribution pipe assembly located in the low-temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the first stage reaction; in the reaction of preparing molybdenum powder, the first stage reaction includes reducing MoO3 powder in a hydrogen atmosphere at 450-600℃ to obtain intermediate products MoO2 and Mo4O 11 and by-product water vapor;

[0083] After the first stage reaction is completed, the driving component sends the reaction crucible along the guide component into the high temperature zone of the reaction furnace tube. The gas distribution pipe component located in the high temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the second stage reaction. In the reaction of preparing molybdenum powder, the second stage reaction includes the intermediate products MoO2 and Mo4O 11 Continue reduction at 850-1050°C to finally obtain molybdenum powder;

[0084] During the reaction process, the exhaust assembly discharges the tail gas from the bottom of the reaction furnace tube;

[0085] After the second stage reaction is completed, the driving component sends the reaction crucible into the cooling zone of the reaction furnace tube for cooling; molybdenum powder is collected;

[0086] The driving component intermittently and continuously delivers the reaction crucible into the reaction furnace tube to achieve continuous preparation of molybdenum powder.

[0087] The technical details are further illustrated below with reference to embodiments.

[0088] Example 1

[0089] Figure 1 This is a schematic diagram of the composition of the molybdenum powder continuous production device disclosed in Example 1. Figure 2 for Figure 1 AA interface diagram of the disclosed molybdenum powder continuous production device; Figure 3 This is a schematic diagram of the setting of the material discharging component of the molybdenum powder continuous production device;

[0090] like Figure 1 、 23, the molybdenum powder continuous production device disclosed in Example 1 includes a horizontally arranged reaction furnace tube 1, the reaction furnace tube 1 is rectangular, and is sequentially arranged from left to right along its length direction as a low-temperature zone I, a material-dispersing zone II, a high-temperature zone III and a cooling zone IV; on the left side of the low-temperature zone, the reaction furnace tube is extended for a certain distance, and a feeding component is provided above the extended portion; the feeding component is used to add solid reaction materials into the reaction crucible 2; a plurality of air holes are provided at the bottom of the reaction furnace tube 1, which are respectively arranged in the low-temperature zone I and the high-temperature zone II, for inputting reaction gas into the low-temperature zone I and the high-temperature zone II; the rectangular reaction furnace tube 1 is a rectangular parallelepiped as a whole, and its cross-section is square, including upper and lower parallel side walls and two vertical parallel side walls, and the gas distribution pipe assembly is usually arranged and installed on the lower side wall of the reaction furnace tube;

[0091] The gas distribution pipe assembly 3 is arranged inside the reaction furnace tube 1 along the length direction of the reaction furnace tube. The reaction crucible 2 is arranged in the reaction furnace tube 1 for placing reaction materials. The gas distribution pipe assembly 3 includes a circular outer tube 31 and a plurality of inner tubes 32 arranged inside the outer tube 31. One end of each inner tube 32 is connected to each air hole at the bottom of the reaction furnace tube 1, and the other end of each inner tube is connected to the gas source 6.

[0092] The gas distribution pipe assembly 3 is provided with two groups. The outer tubes 31 of each group of gas distribution pipe assemblies 3 are parallel to each other and are arranged in the bottom center area of ​​the reaction furnace tube 1. The two outer tubes 32 serve as the moving track of the reaction crucible 2.

[0093] The bottom of the reaction crucible 2 is provided with a semicircular groove, which is adapted to the outer shape of the outer tube 31. Multiple reaction crucibles 2 are sequentially adapted and arranged on the outer tube 32.

[0094] A driving assembly 5 is provided on the outside of the right end of the reaction furnace tube 1. The driving assembly 5 includes a fixed base and a driving component. The driving component is used to push the reaction crucible 2 to move toward the left side of the reaction furnace tube 1. The driving component can be a hydraulic rod.

[0095] The gas source 6 is provided at the left end of the reaction furnace tube 1 and is connected to the multiple inner tubes 32 through multiple gas pipelines; each gas pipeline is provided with a switch valve component for controlling the opening and closing of the gas flow in the inner tube;

[0096] The material discharging area is provided with a material discharging assembly; the material discharging assembly 7 is arranged above the reaction furnace tube, wherein the material discharging assembly includes a fixing component, which is adapted and fixed to the upper part of the reaction furnace tube 1, and a material discharging component is movably connected to the fixing component, and the material discharging component includes a material discharging plate arranged at its lower end, and the material discharging plate is provided with material discharging nails; after the reaction crucible enters the material discharging area, the reaction crucible 2 is located below the material discharging plate of the material discharging assembly 7, and the material discharging plate has a shape consistent with the opening above the reaction crucible 2, so that the material discharging plate moves downward into the reaction crucible and effectively contacts the material layer 100 therein, and the material in the material layer 100 is loosened by using the material discharging nails provided on the material discharging plate;

[0097] The exhaust assembly 4 is arranged to be in communication with the bottom of the reaction furnace tube 1 and is used to discharge the reaction tail gas.

[0098] Using the molybdenum powder continuous production device disclosed in Example 1, the method for producing molybdenum powder includes:

[0099] The feed component is used to add the reaction material into the reaction crucible and evenly distribute the raw materials at the bottom of the reaction crucible to form a material layer; the drive component sends the reaction crucible along the guide component into the low-temperature zone of the reaction furnace tube; the gas distribution pipe component located in the low-temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the first stage reaction;

[0100] After the first stage reaction is completed, the driving assembly sends the reaction crucible along the guide assembly into the high temperature zone of the reaction furnace tube. The gas distribution pipe assembly located in the high temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the second stage reaction.

[0101] During the reaction process, the exhaust assembly discharges the tail gas from the bottom of the reaction furnace tube;

[0102] After the second stage reaction is completed, the driving component sends the reaction crucible into the cooling zone of the reaction furnace tube for cooling; molybdenum powder is collected;

[0103] A plurality of reaction crucibles are arranged in the reaction furnace tube, and the plurality of reaction crucibles are arranged in sequence and continuously. Under the intermittent push of the driving component, the reaction crucibles gradually enter the reaction furnace tube to participate in the reaction process. Usually, when the reaction crucible enters the low-temperature zone of the reaction furnace tube for the first stage reaction, the driving component returns to its original position, the subsequent reaction crucible is placed on the guide component, and the reaction material is added to the reaction crucible again by using the feeding component, and the reaction crucible filled with the raw materials is pushed into the low-temperature zone of the reaction furnace tube for the first stage reaction. The sequential method can realize continuous feeding. After a certain period of time, the reaction crucible that has completed the first stage reaction in the low-temperature zone enters the material-discharging zone under the push of the next driving component, and carries out material discharging in the material-discharging zone. Then, it enters the high-temperature zone under the push of the next driving component for the second stage reaction. The reaction crucible stays in the high-temperature zone for a sufficient time, and after completing the second stage reaction, it enters the cooling zone under the push of the driving component for cooling. The residence time of the reaction crucibles arranged continuously in this way in the high-temperature zone and the low-temperature zone is directly related to the length of the high-temperature zone and the low-temperature zone, the intermittent stop time of the drive component, and the length of the reaction crucible; the relative lengths of the low-temperature zone and the high-temperature zone are usually set according to the relative time of the first-stage reaction and the second-stage reaction, and further, the intermittent stop time of the drive component is determined according to the total time of the first-stage reaction or the total time of the second-stage reaction.

[0104] The driving component intermittently and continuously sends multiple reaction crucibles into the reaction furnace tube in sequence. The reaction crucibles stay in the low-temperature zone, material discharging zone, high-temperature zone and cooling zone for a sufficient time according to the set process to respectively realize the first-stage reaction, material discharging operation, second-stage reaction and cooling, and finally collect the cooled products to realize the continuous preparation of molybdenum powder.

[0105] The molybdenum powder continuous production device disclosed in the embodiment of the present invention is provided with a low-temperature zone, a high-temperature zone and a cooling zone in the reaction furnace tube, and uses a driving component to intermittently and continuously transport the reaction crucible into the reaction furnace tube to continuously carry out the first stage reaction and the second stage reaction, thereby realizing the continuous production of molybdenum powder; during the reaction process, the gas distribution pipe component inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to react with the solid material, so that the reaction gas and the water vapor generated by the reaction flow upward, which is conducive to the full contact between the reaction gas and the solid material, thereby improving the reaction efficiency, and effectively promoting the discharge of water vapor, which can effectively prevent the reaction material from hardening and agglomerating; discharging the reaction tail gas from the bottom of the reaction furnace tube is conducive to preferentially removing water vapor, which is conducive to promoting the reaction. The molybdenum powder continuous production device can realize high-efficiency large-scale continuous production of molybdenum powder in the same device, and has good application prospects in the field of large-scale production and preparation of metal molybdenum powder.

[0106] The technical solutions and technical details disclosed in the embodiments of the present invention are merely illustrative of the inventive concept of the present invention and do not constitute a limitation on the technical solutions of the embodiments of the present invention. Any conventional changes, replacements or combinations of the technical details disclosed in the embodiments of the present invention have the same inventive concept as the present invention and are within the scope of protection of the claims of the present invention.

Claims

1. A continuous molybdenum powder production device, characterized in that: include: A reaction furnace tube, wherein the reaction furnace tube comprises a low temperature zone, a high temperature zone and a cooling zone arranged in sequence along its length; a gas distribution pipe assembly disposed inside the reaction furnace tube along the length of the reaction furnace tube; portions of the gas distribution pipe assembly located in the low-temperature zone and the high-temperature zone are respectively provided with air holes adapted to the low-temperature zone and the high-temperature zone, for respectively introducing reaction gas into the low-temperature zone and the high-temperature zone; A reaction crucible is provided in the reaction furnace tube for placing reaction materials; the reaction crucible is adapted to be provided with the gas distribution pipe assembly, and the reaction gas introduced from the gas distribution pipe assembly enters the interior of the reaction crucible from the bottom of the reaction crucible; A guide assembly is arranged inside the reaction furnace tube along the length direction of the reaction furnace tube; the reaction crucible is adapted to be arranged on the guide assembly to guide the reaction crucible to move along the length direction of the reaction furnace tube; The air distribution pipe assembly and the guide assembly are configured as the same assembly, and the air distribution pipe assembly includes: an outer tube, wherein the upper wall of the outer tube is provided with air holes located in the high temperature zone and the low temperature zone; The inner tubes are provided in a plurality; the plurality of inner tubes are provided inside the outer tube; wherein one end of each inner tube is respectively provided to communicate with an air hole on the outer tube, and the other end of each inner tube is provided to communicate with an air source; The bottom of the reaction crucible is provided with a groove adapted to the outer tube, and a through hole is provided in the groove; when the groove of the reaction crucible is adapted to be installed with the outer tube, the position of the through hole corresponds to the air hole on the outer tube; a driving assembly, configured to drive the reaction crucible to move on the guide assembly; The exhaust assembly is arranged to be in communication with the bottom of the reaction furnace tube and is used for discharging reaction tail gas.

2. The molybdenum powder continuous production device according to claim 1, wherein The reaction furnace tube further includes a material thinning zone arranged between the low-temperature zone and the high-temperature zone.

3. The molybdenum powder continuous production device according to claim 1, wherein The guide assembly is a guide rail, and the reaction crucible is provided with a structure adapted to the guide rail.

4. The molybdenum powder continuous production device according to claim 1, wherein The reaction crucible is provided in plurality, and the plurality of crucibles are arranged in sequence and continuously, and are driven by the driving component to move intermittently and continuously, thereby realizing continuous production of molybdenum powder.

5. The molybdenum powder continuous production device according to claim 2, wherein A material discharging assembly is provided inside the reaction furnace tube located in the material discharging area, and the material discharging assembly includes: A fixing seat, arranged to be fixed on the upper wall of the reactor tube; A material-dispersing plate is mounted on the fixing seat via a retractable connector; the shape of the material-dispersing plate is adapted to the reaction crucible; The driving component is used to drive the material-separating plate to move.

6. The molybdenum powder continuous production device according to claim 1 or 2, wherein The exhaust assembly comprises: an exhaust pipe, arranged to communicate with the bottom of the reaction furnace tube; An air pump is arranged to be connected to the exhaust pipe.

7. A method for continuous production of molybdenum powder, characterized in that: The molybdenum powder continuous production device according to any one of claims 1 to 6 is used to produce molybdenum powder, comprising: The reaction material is placed in the reaction crucible, and the driving assembly moves the reaction crucible along the guide assembly into the low-temperature zone of the reaction furnace tube; the gas distribution pipe assembly located in the low-temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the first stage reaction; After the first stage reaction is completed, the driving assembly sends the reaction crucible along the guide assembly into the high temperature zone of the reaction furnace tube. The gas distribution pipe assembly located in the high temperature zone inputs the reaction gas from the bottom of the reaction crucible into the reaction crucible to carry out the second stage reaction. During the reaction process, the exhaust assembly discharges the tail gas from the bottom of the reaction furnace tube; After the second stage reaction is completed, the driving component sends the reaction crucible into the cooling zone of the reaction furnace tube for cooling; molybdenum powder is collected; The driving component intermittently and continuously delivers the reaction crucible into the reaction furnace tube to achieve continuous preparation of molybdenum powder.

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