High-purity vanadium continuous precipitation reaction device

Abstract

The invention discloses a high-purity vanadium continuous precipitation reaction device, which comprises: a feeding system, which comprises a liquid storage tank, an ammonium salt bin and a supply unit; the reaction system comprises a reaction kettle, a material reaction area, a material circulation area and a material deposition area are arranged in the reaction kettle from top to bottom, the liquid storage tank is connected to the material reaction area through a conveying pipeline, a conveying screw of the ammonium sulfate bin extends into the material circulation area, and two annular sealing rings are arranged on the periphery of the material reaction area; the discharging system comprises a discharging opening formed in the bottom of the reaction kettle; and the control system is in communication connection with the feeding system, the reaction system and the discharging system. The vanadium-containing qualified liquid is continuously conveyed into the reaction kettle by adopting the hyperbolic reaction kettle, compressed air and wood fiber particles are uniformly and stably sprayed into the middle section of the reaction kettle through the annular sealing ring, the crystallization efficiency is improved, continuous precipitation is realized, the production efficiency is high, and the requirement of industrial production can be met.

Description

Technical Field

[0001] This invention relates to the field of metallurgical technology, and in particular to a continuous precipitation reaction apparatus for high-purity vanadium. Background Technology

[0002] In the intermittent precipitation mode of ammonium metavanadate in the traditional vanadium extraction process, the vanadium precipitation process is limited by the inherent characteristics of the weakly alkaline reaction system, resulting in a series of problems that restrict the efficiency and stability of industrial production, including (1) the weakly alkaline system leads to limited reaction, long cycle and poor crystallization performance: under weakly alkaline conditions, the polymerization form of vanadate ions is complex and the ionic reactivity is low, resulting in a long induction period and slow reaction rate of precipitation reaction. In actual production, the single batch vanadium precipitation reaction cycle is usually as long as 12 to 24 hours, or even longer. (2) the intermittent reaction mode results in extremely poor equipment utilization and production continuity: after a single reactor completes the entire process from feeding, pH adjustment, reaction, crystallization and discharge, the next batch of production can be started, and the reactor cleaning and parameter recalibration are required between batches, which further prolongs the production interval.

[0003] Therefore, improvements to existing technologies are needed. Summary of the Invention

[0004] The main objective of this invention is to provide a high-purity vanadium continuous precipitation reaction device. The device uses a hyperbolic reactor to continuously transport qualified vanadium-containing liquid into the reactor. Compressed air and wood fiber particles are uniformly and stably injected into the middle section of the reactor through an annular sealing ring to improve crystallization efficiency. Simultaneously, continuous precipitation is achieved, resulting in high production efficiency and adaptability to the needs of industrial production.

[0005] According to one aspect of the present invention, a continuous precipitation reaction apparatus for high-purity vanadium is provided, comprising: The feeding system includes a storage tank for storing vanadium liquid, an ammonium salt silo, and a supply unit for providing a mixture containing compressed air and crystal nuclei. The reaction system includes a reaction vessel, inside which a material reaction zone, a material circulation zone, and a material sedimentation zone are formed from top to bottom. A storage tank is connected to the material reaction zone through a liquid inlet pipe. The conveying component of the ammonium salt silo extends into the material circulation zone. A first annular sealing ring is provided on the outer periphery of the material reaction zone, which is connected to the material reaction zone and the supply unit. A second annular sealing ring is provided on the outer periphery of the material circulation zone. The second annular sealing ring is connected to the material circulation zone and is connected to the liquid inlet pipe through a pumping pipe. A pumping pump is provided on the pumping pipe to pump liquid from the second annular sealing ring to the liquid inlet pipe. The discharge system includes discharge pipes that are connected to the material deposition area.

[0006] According to one embodiment of the present invention, a jet air channel is provided on the inner side of the first annular sealing ring, which faces the material reaction zone.

[0007] According to one embodiment of the present invention, the blowing direction of the blowing air passage is inclined upwards by 10° to 20° relative to the horizontal direction.

[0008] According to one embodiment of the present invention, the inner side of the second annular sealing ring is provided with a radial pipe communicating with the material circulation zone.

[0009] According to one embodiment of the present invention, the ammonium salt silo is used to store ammonium sulfate, and the crystal nuclei are wood fiber particles.

[0010] According to one embodiment of the present invention, a filter element is provided in the radial pipe and / or the pumping pipe.

[0011] According to one embodiment of the present invention, a feed valve is provided on the inlet pipe and a discharge valve is provided on the outlet pipe. The high-purity vanadium continuous precipitation reaction device also includes a level gauge for measuring the liquid level height in the reactor and a control system. The control system is configured to control the feed rate of the feed valve to correspond to the discharge rate of the outlet valve when the level gauge detects that the liquid level height has reached a predetermined value.

[0012] According to one embodiment of the present invention, a pH meter is provided in the material reaction zone, and the high-purity vanadium continuous precipitation reaction device further includes a control system configured to control the conveying component to convey a predetermined amount of ammonium salt when the pH meter detects that the pH is lower than a predetermined value.

[0013] According to one embodiment of the present invention, a vanadium concentration measuring instrument is provided in the material circulation zone, and a discharge valve is provided on the discharge pipe. The high-purity vanadium continuous precipitation reaction device also includes a control system, which is configured to control the discharge valve to open when the vanadium concentration measuring instrument detects that the vanadium concentration is lower than a predetermined value.

[0014] According to one embodiment of the present invention, the two sides of the reactor have a hyperbolic shape.

[0015] In a high-purity vanadium continuous precipitation reaction apparatus according to an embodiment of the present invention, a hyperbolic reactor is used to continuously and uniformly transport the pretreated vanadium-containing qualified solution to the reaction zone inside the reactor. With the upper air channel design of the double-layer annular sealing ring, dried and filtered compressed air and uniformly sized wood fiber particles are precisely injected into the middle section of the reactor. The compressed air can break through the polymerization barrier of vanadate ions in the solution, while the wood fiber particles can act as crystallization nuclei to induce rapid nucleation and growth of vanadium crystals, greatly improving crystallization efficiency and crystal regularity. The entire process abandons the traditional intermittent operation mode and realizes the fully automated operation of continuous feeding, continuous reaction and continuous precipitation of vanadium-containing solution. It has significant advantages of high production efficiency, stable product quality and low energy consumption, and can fully adapt to the needs of large-scale and intensive industrial production. Attached Figure Description

[0016] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some implementation examples of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 A schematic diagram of a high-purity vanadium continuous precipitation reaction apparatus according to an exemplary embodiment of the present invention is shown.

[0018] The reference numerals in the figure are explained as follows: 1. Storage tank; 2. Ammonium salt silo; 3. Reactor; 4. Conveying screw; 5. First annular sealing ring; 6. Second annular sealing ring; 7. Supply unit. Detailed Implementation

[0019] The following detailed description of the embodiments is intended to exemplify the principles of the present invention, but should not be construed as limiting the scope of the invention. The present invention can be implemented in many different forms and is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

[0020] These embodiments are provided to make this disclosure thorough and complete, and to fully express the scope of the invention to those skilled in the art. It should be noted that, unless otherwise specifically stated, the relative arrangement of components and steps, material composition, numerical expressions, and values ​​set forth in these embodiments should be interpreted as merely exemplary and not as limiting.

[0021] It should be noted that, in the description of this invention, unless otherwise stated, "a plurality of" means two or more; the terms "upper," "lower," "left," "right," "inner," and "outer," etc., indicating orientation or positional relationships, are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0022] It should also be noted that, in the description of this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this invention depending on the specific circumstances. When a specific device is described as being located between a first device and a second device, an intermediary device may or may not be present between the specific device and the first or second device.

[0023] All terms used in this invention have the same meaning as understood by one of ordinary skill in the art to which this disclosure pertains, unless otherwise specifically defined. It should also be understood that terms defined in general dictionaries should be interpreted as having meanings consistent with their meanings in the context of the relevant art, and not as idealized or highly formalized, unless expressly defined herein.

[0024] Techniques, methods, and equipment known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and equipment should be considered part of the specification.

[0025] like Figure 1 As shown, a high-purity vanadium continuous precipitation reaction apparatus includes: a feeding system comprising a storage tank 1, an ammonium salt silo 2, and a supply unit 7 for providing a mixture containing compressed air and crystal nuclei; a reaction system comprising a reactor 3, wherein the reactor 3 forms a material reaction zone, a material circulation zone, and a material deposition zone from top to bottom; the storage tank 1 is connected to the material reaction zone via an inlet pipe (e.g., a 316L stainless steel pipe); the conveying component of the ammonium salt silo 2 extends into the material circulation zone; a first annular sealing ring 5 is provided on the outer periphery of the material reaction zone, communicating with the material reaction zone and the supply unit; a second annular sealing ring 6 is provided on the outer periphery of the material circulation zone, communicating with the material circulation zone and the inlet pipe via a pumping pipe; and a discharge system comprising a discharge pipe communicating with the material deposition zone.

[0026] In the high-purity vanadium continuous precipitation reaction apparatus according to an embodiment of the present invention, a hyperbolic reaction vessel 3 is used to continuously transport vanadium-containing qualified liquid into the reaction vessel 3. Compressed air and wood fiber particles are uniformly and stably sprayed into the middle section of the reaction vessel 3 through an annular sealing ring to improve crystallization efficiency and achieve continuous precipitation. This apparatus has high production efficiency and can meet the needs of industrial production.

[0027] The hyperbolic reaction in this application, based on numerical simulation, employs a two-layer annular sealing ring. The upper layer is always in a convection state, accelerating the rapid precipitation of vanadium and ammonium sulfate in the qualified liquid under the condition of lignocellulose nucleation in the reactor 3, ensuring the speed and stability of precipitation. Below the stable liquid surface layer, the already crystallized ammonium metavanadate continues to grow and accumulates in the lower part of the reactor 3. The discharge rate of ammonium metavanadate is controlled by a vanadium concentration detector.

[0028] In some specific embodiments, a jet air channel is provided on the inner side of the first annular sealing ring 5, which faces the material reaction zone.

[0029] Based on the above embodiments, the blowing direction of the blowing air channel is inclined upwards by 10° to 20° relative to the horizontal direction. The blowing air channel can extend radially, and its blowing nozzle has an upward blowing direction; or the blowing air channel can also extend upwards at an angle.

[0030] Preferably, the blowing direction of the blowing air passage is tilted upward at 15° relative to the horizontal direction.

[0031] In some specific embodiments, the inner side of the second annular sealing ring is provided with a radial pipe communicating with the material circulation area.

[0032] In some specific embodiments, the sprayed material in the spraying air channel is compressed air and lignocellulose particles, which are easily and evenly dispersed in the upper part of the hyperbolic reactor 3, facilitating the precipitation and crystallization of ammonium metavanadate. At the same time, the purified compressed air is not only used as a carrier gas, but also as a stirring gas to accelerate the rapid mass transfer of vanadium in the reaction solution.

[0033] Specifically, the ammonium salt silo is used to store ammonium sulfate, with the crystal nuclei being wood fiber particles.

[0034] Based on the above embodiments, for every 1 ton of ammonium metavanadate produced, the amount of lignocellulose particles added is 25~27 kg.

[0035] In some specific embodiments, a filter element is provided inside the radial pipe and / or the pumping pipe. Specifically, an annular filtration chamber is coaxially arranged inside the second annular sealing ring 6 to promptly filter the qualified liquid that has not yet fully reacted to the upper part for further reaction with ammonium sulfate. When the vanadium concentration is lower than a certain value, the bottom ammonium metavanadate is discharged in time, and fresh qualified liquid is promptly replenished at the upper feed inlet.

[0036] The inlet pipe is equipped with a feed valve, and the outlet pipe is equipped with a discharge valve. The high-purity vanadium continuous precipitation reaction device also includes a level gauge for measuring the liquid level in the reactor and a control system. The control system is configured such that when the level gauge detects that the liquid level has reached a predetermined value, it controls the feed rate of the feed valve to correspond to the discharge rate of the discharge valve.

[0037] Based on the above embodiments, a liquid level gauge is installed on the feed valve of the storage tank 1, which can monitor the changes in the liquid level in the tank in real time, accurately control the valve opening to realize automatic start and stop of feeding, avoid overflow due to excessive liquid level or empty tank due to excessive liquid level caused by manual operation, and ensure feeding stability; prevent equipment safety hazards and material waste caused by excessive liquid level, while reducing the frequency of manual inspection and reducing labor intensity; adapt to the needs of automated production lines, and realize the material conveying adjustment of the storage tank 1 and downstream equipment such as the reaction vessel 3.

[0038] During the reaction, the liquid level in reactor 3 is 3m.

[0039] Based on the above embodiments, a pH meter is installed inside the reactor 3, which can monitor the pH value changes of the weakly alkaline vanadium precipitation system in real time and accurately, avoiding the lag and error of manual sampling and testing, and timely feedback of data to coordinate the adjustment of acid and alkali dosage, stabilize the reaction environment, prevent the vanadate polymerization morphology from being too high or too low and crystallization difficulties from being difficult, improve the vanadium precipitation efficiency and product purity, ensure the consistency of pH parameters between batches, and reduce product quality fluctuations.

[0040] Specifically, during the reaction process, the reaction vessel 3 is weakly alkaline, with a pH value ranging from 9 to 10.

[0041] Based on the above embodiments, a vanadium concentration meter is installed inside the reactor 3, which can monitor the changes in vanadium ion concentration in the reactor in real time, accurately control the vanadium precipitation reaction process, and avoid poor crystallization or substandard product purity due to concentration deviation; timely feedback of concentration data can be used to adjust the amount of ammonium salt fed and the stirring speed, optimize reaction conditions, and improve vanadium recovery rate; reduce the error and lag of manual sampling and testing, and reduce labor intensity; ensure stable concentration parameters between batches, and improve product quality consistency.

[0042] Specifically, the initial vanadium concentration was 35 g / L, and during the reaction, the vanadium concentration was 20-25 g / L.

[0043] Based on the above embodiments, the conveying screw 4 is a variable frequency conveying screw 4, which flexibly matches the feed / discharge rate of the reactor 3 to achieve quantitative and stable material conveying, avoid material overload or shortage, and dynamically adjust the speed according to the material characteristics to effectively prevent powder bridging and sticky material adhesion and blockage, thereby improving conveying efficiency.

[0044] The material inside reactor 3 is always in dynamic equilibrium. The inlet and outlet are precisely controlled by a pneumatic regulating valve. The pneumatic regulating valve is interlocked with the level gauge, and the bottom outlet is consistent with the top inlet.

[0045] In some embodiments, the two sides of the reactor 3 have a hyperbolic shape. The hyperbolic shape forms two annular rings. The first layer is used to spray compressed air and wood fiber particles, which serve as nuclei for AMV crystallization. After crystallization, they continuously aggregate, grow, and sink to the bottom. The second layer is used for continuous self-circulation of the upper stirring liquid, which accelerates the rapid mass transfer of V element in the qualified liquid. Through upper circulation, lower aggregation, and regular discharge of AMV at the bottom, the continuous precipitation reaction of AMV in this device is ensured.

[0046] In some embodiments, this application further includes a metering system, which is installed on the feeding system for real-time metering and displaying of the material weight, fault self-diagnosis, and automatic correction of lead time. The metering system includes a solid metering component and a liquid metering component. The solid metering component is a load cell, and the liquid metering component includes a flow sensor. The metering system in this application is typically used in conjunction with the feeding system and has the following functions: (1) Real-time weight display and error detection. The weight value of the material is displayed in real time; each weighing process is subject to error detection, judgment and alarm when the error exceeds the tolerance. After weighing, the material is conveyed to the reactor 3 by the conveying screw 4. The conveying pipe extends into the middle of the reactor 3 to facilitate timely dissolution of the material during the floating process and accelerate the precipitation reaction.

[0047] (2) Fault self-diagnosis. The weighing control terminal has a fault self-diagnosis function and displays it through codes. Each cycle detects the existing quantity and automatically corrects deviations to avoid errors caused by feeding deviations. The automatic advance correction function can dynamically adjust the material conveying volume to ensure the stability of the material ratio in the reaction system, greatly improve the consistency of product quality, help continuous production, and meet the needs of large-scale industries.

[0048] (3) Automatic advance correction function. This function overcomes the impact of changes in material accumulation and properties in the weighing hopper, so as to ensure packaging accuracy.

[0049] A metering system is installed at the discharge end of reactor 3 to determine whether the material discharged per unit time meets the design specifications based on material balance calculations, thus ensuring the continuous and stable operation of reactor 3.

[0050] In some specific embodiments, the control system is a PLC control system. Using a PLC control system enables full automation of the vanadium precipitation process, precisely controlling parameters for processes such as reactor feeding, stirring, blowing, and filtration, replacing frequent manual operations, reducing labor intensity and human error; it features real-time data acquisition and automatic fault diagnosis and alarm functions, enabling timely detection of equipment anomalies and triggering protection mechanisms to prevent production accidents; it supports parameter storage and batch traceability, ensuring product quality stability; and it can flexibly adapt to process upgrades and adjustments, significantly improving production efficiency and equipment reliability, meeting the needs of large-scale continuous production.

[0051] The control system of this application is installed in a remote control room, while the operation panel is installed separately on the front of the machine. The control panel is connected to the PLC control system in the electrical box of the packaging machine via a communication cable, which is more ergonomic and facilitates operation and use by the operator. The control panel mainly consists of a touch screen and an emergency stop button.

[0052] This invention replaces the traditional intermittent ammonium metavanadate (AMV) precipitation method. The AMV precipitation process is weakly alkaline, requiring the continuous addition of ammonium sulfate to maintain a consistently weakly alkaline pH. To ensure rapid crystal aggregation during precipitation, this invention employs a hyperbolic reactor 3 with two annular sealing rings. The first ring is used to spray compressed air and wood fiber particles, serving as nuclei for AMV crystallization. After crystallization, these nuclei continuously aggregate, grow, and sink to the bottom. The second ring allows for continuous self-circulation of the upper stirring liquid, accelerating vanadium mass transfer in the qualified liquid. Through upper circulation and lower aggregation, with regular discharge of AMV from the bottom, continuous precipitation of AMV is ensured. This equipment integration achieves deep fusion of information technology and industrialization, enhancing operational reliability and efficiency to meet the requirements of continuous industrial production.

[0053] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the invention (including the claims) is limited to these examples. Within the framework of the invention, technical features of the above embodiments or different embodiments can be combined, and many other variations of different aspects of the invention exist, which are not provided in the details for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the invention should be included within the protection scope of the invention.

Claims

1. A high purity vanadium continuous precipitation reaction apparatus, characterized by, The application relates to a high-purity vanadium continuous precipitation reaction device. The device comprises: a feeding system, which comprises a liquid storage tank for storing vanadium liquid, an ammonium salt bin and a supply unit for providing a mixture containing compressed air and crystal nucleus; a reaction system, which comprises a reaction kettle, the inside of the reaction kettle is formed with a material reaction zone, a material circulation zone and a material deposition zone from top to bottom, the liquid storage tank is connected to the material reaction zone through a liquid inlet pipeline, a conveying part of the ammonium salt bin extends into the material circulation zone, the outer periphery of the material reaction zone is provided with a first annular sealing ring which is in communication with the material reaction zone and the supply unit, the outer periphery of the material circulation zone is provided with a second annular sealing ring which is in communication with the material circulation zone and is connected to the liquid inlet pipeline through a pumping pipeline, and a pumping pump for pumping liquid from the second annular sealing ring to the liquid inlet pipeline is arranged on the pumping pipeline; and a discharging system, which comprises a discharging pipeline which is in communication with the material deposition zone. The first annular sealing ring is provided with a blowing air channel towards the material reaction zone. The blowing direction of the blowing air channel is inclined upwards by 10-20 degrees relative to the horizontal direction.

2. The high purity vanadium continuous precipitation reaction apparatus according to claim 1, characterized by, The inner side of the second annular sealing ring is provided with a radial pipeline which is in communication with the material circulation zone.

3. The high purity vanadium continuous precipitation reaction apparatus according to claim 2, characterized by, The ammonium salt bin is used for storing ammonium sulfate, and the crystal nucleus is a wood fiber particle.

4. The high purity vanadium continuous precipitation reaction apparatus according to claim 1, characterized by, The radial pipeline and / or the pumping pipeline is provided with a filtering part.

5. The high purity vanadium continuous precipitation reaction apparatus according to claim 4, characterized by, The liquid inlet pipeline is provided with a feeding valve, and the discharging pipeline is provided with a discharging valve.

6. The high purity vanadium continuous precipitation reaction apparatus according to claim 4, characterized by, The reaction kettle is provided with a liquid level meter for measuring the liquid level in the reaction kettle, and a control system is arranged, which is configured to control the feeding amount of the feeding valve and the discharging amount of the discharging valve when the liquid level meter detects that the liquid level reaches a predetermined value.

7. The high purity vanadium continuous precipitation reaction apparatus according to claim 1, characterized by, The material reaction zone is provided with a pH meter, and the high-purity vanadium continuous precipitation reaction device further comprises a control system, which is configured to control the conveying part to convey a predetermined amount of ammonium salt when the pH meter detects that the pH is lower than a predetermined value.

8. The high purity vanadium continuous precipitation reaction apparatus according to claim 1, characterized by, The material circulation zone is provided with a vanadium concentration meter, and the discharging pipeline is provided with a discharging valve, and the high-purity vanadium continuous precipitation reaction device further comprises a control system, which is configured to control the discharging valve to be opened when the vanadium concentration meter detects that the vanadium concentration is lower than a predetermined value.

9. The high purity vanadium continuous precipitation reaction apparatus according to claim 1, characterized by, The profile of the reaction kettle on both sides is in a hyperbolic shape.

10. The high purity vanadium continuous precipitation reaction apparatus according to claim 1, characterized by, ​

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