Reaction device and method for preparing high-purity molybdenum trioxide
By using the design of lifting columns and spoilers in the reaction device, the hierarchical and radial mixing of the reaction solution is achieved, and the problem of uneven mixing in traditional devices is solved, and the purity and yield of high-purity molybdenum trioxide is improved.
Patent Information
- Application Number
- CN202510307356.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-17
- Publication Date
- 2025-04-15
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
When preparing high-purity molybdenum trioxide, traditional reaction devices lack effective hierarchical and radial mixing of the reaction solution, resulting in incomplete or overreaction of local reactions, affecting product purity.
A reaction device including a reactor, a filter bag, a lifting column and a spoiler is designed to achieve hierarchical and radial mixing of the reaction solution through the upper and lower jitter of the lifting column and the radial thrust of the spoiler.
It effectively promotes uniform mixing of the reaction solution, breaks down the local concentration gradient, and improves product purity and yield.
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Figure CN119819241A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of chemical reaction technology, and more specifically, to a reaction device and method for preparing high-purity molybdenum trioxide. Background Art
[0002] Molybdenum trioxide is an inorganic compound, mainly used for the determination of protein, phenol, arsenic, lead, bismuth, etc. It can also be used as a reducing agent for phosphorus pentoxide, arsenic trioxide, hydrogen peroxide, phenol and alcohol, and can also be used to prepare molybdenum salts and molybdenum alloys.
[0003] High-purity molybdenum trioxide is prepared by an ammonium molybdate solution method, the impurity-removed ammonium molybdate solution is mixed with nitric acid for acid precipitation crystallization to produce molybdenum trioxide precipitate, and the molybdenum trioxide precipitate is separated from the solid and liquid and dried to obtain high-purity molybdenum trioxide;
[0004] During the above reaction process, the mixing uniformity of ammonium molybdate solution and nitric acid directly affects the purity and yield of high-purity molybdenum trioxide. The traditional reaction device can only perform a single circumferential mixing of the reaction solution, lacking the turbulence effect on different levels and radial directions of the reaction solution, resulting in incomplete or excessive local reaction, thereby affecting the purity of the final product. Summary of the invention
[0005] In order to overcome the above technical problems, the present invention proposes a reaction device and method for preparing high-purity molybdenum trioxide.
[0006] The purpose of the present invention can be achieved through the following technical solutions:
[0007] A reaction device for preparing high-purity molybdenum trioxide, comprising:
[0008] A reactor, the upper end of which is respectively provided with a first feed inlet and a second feed inlet, and a discharge sleeve is provided at the center of the lower end of the reactor;
[0009] The filter bag is arranged in the reactor, and comprises a mounting ring which can be raised and lowered and a bag body connected to the mounting ring;
[0010] A lifting column is detachably mounted in the discharge sleeve and is detachably connected to the center of the bag body;
[0011] A lifting drive component, which is arranged at the upper end of the reactor and is used to drive the lifting column to move up and down;
[0012] The spoiler is movably arranged on the lifting column and is located in the bag body.
[0013] As a further solution of the present invention: the lifting drive component includes a driving motor fixed to the top of the reactor, a rotating shaft connected to the output end of the driving motor, a rotating drum coaxially fixed with the rotating shaft, and a connecting frame fixed on the lifting column, the rotating drum is provided with a spiral reciprocating groove, and the connecting frame is provided with a pin adapted to the spiral reciprocating groove.
[0014] As a further solution of the present invention: the lifting column is provided with a plurality of axial slide bars slidably matched with the discharge sleeve; when the lifting column moves up and down, the axial slide bars slide axially relative to the discharge sleeve.
[0015] As a further solution of the present invention: the spoiler includes a limit plate fixed on the lifting column and a ring movably mounted on the lifting column, the ring is rotatably connected with a rocker, the end of the rocker away from the ring is rotatably mounted with a roller, and the rocker is also provided with a push plate; a return spring is provided between the limit plate and the ring, and the return spring is movably mounted on the lifting column.
[0016] As a further solution of the present invention: a transition chamber with an opening at the lower end is provided in the rotating drum, the upper end of the lifting column is movably embedded in the transition chamber, and a suction flow channel connected to the transition chamber is provided at the upper end of the lifting column; a plurality of suction holes are provided at the bottom of the suction flow channel, a plurality of spray holes are provided circumferentially at the upper end of the transition chamber, and an inverted cone-shaped guide plate adapted to the spray holes is provided at the top of the rotating drum; a first one-way valve is installed in the suction flow channel, and a second one-way valve is installed at the top of the transition chamber.
[0017] As a further solution of the present invention: the lower end of the lifting column is provided with a drainage channel connected to the outside, and the upper end of the drainage channel is provided with a plurality of drainage holes connected to the reactor; a connecting ring is provided at the center of the bag body, and a sealing connector adapted to the lifting column is provided on the connecting ring.
[0018] As a further solution of the present invention: the sealing connector includes a mounting cavity provided in the connecting ring and an airbag embedded in the mounting cavity, and a recessed portion adapted to the airbag is provided at the periphery of the drainage hole.
[0019] As a further solution of the present invention: a plurality of regulating cylinders are arranged circumferentially at the bottom of the reactor, the output ends of the regulating cylinders are fixedly connected to the connecting rings, and an air pipe is also connected between the regulating cylinders and the airbags.
[0020] As a further solution of the present invention: a casing is arranged outside the reactor, a water inlet pipe is arranged at the bottom of the casing, and a water outlet pipe is arranged at the top of the casing.
[0021] The present invention also discloses a method for preparing high-purity molybdenum trioxide using a reaction device, comprising the following steps:
[0022] S1, adding ammonium molybdate solution and nitric acid into the reactor from the first feed inlet and the second feed inlet respectively;
[0023] S2, driving the lifting column to move up and down by the lifting driving member, driving the bag body to shake up and down, achieving mixed flow of reaction solutions at different levels, and driving the spoiler to radially disturb the reaction solution;
[0024] S3, after the mixing is completed, the bag is lifted up so that the reaction solution is completely under the bag;
[0025] S4, after the acid precipitation crystallization is completed, the filter bag moves down, so that the bag body wraps and covers the lower layer of molybdenum trioxide precipitation, and the upper clear liquid is discharged;
[0026] S5. The molybdenum trioxide precipitate is fished out and dried to obtain a high-purity molybdenum trioxide product.
[0027] Beneficial effects of the present invention:
[0028] The present invention effectively promotes the mixing of the reaction solution in the vertical direction by shaking the bag body up and down, thereby enhancing the hierarchical fluidity of the solution. At the same time, the spoiler pushes the reaction solution at the center to the periphery, and then gathers the peripheral solution to the center, thereby forming effective radial mixing and realizing radial mixing of the reaction solution. This helps to break any local concentration gradient that may exist, ensures that the reactants are evenly distributed in the entire reactor, ensures that the reaction solutions in the entire reactor can be fully mixed, and effectively improves the purity of the product. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] The present invention will be further described below in conjunction with the accompanying drawings.
[0030] Figure 1 It is a three-dimensional schematic diagram of a reaction device for preparing high-purity molybdenum trioxide according to the present invention;
[0031] Figure 2 A cross-sectional view of a reaction device for preparing high-purity molybdenum trioxide according to the present invention;
[0032] Figure 3 It is a schematic structural diagram of a lifting drive member and a spoiler member in a reaction device for preparing high-purity molybdenum trioxide according to the present invention;
[0033] Figure 4 It is a schematic diagram of the structure of a filter bag and a lifting column in a reaction device for preparing high-purity molybdenum trioxide according to the present invention;
[0034] Figure 5 for Figure 4 Enlarged view of point A in the middle;
[0035] Figure 6 for Figure 4 Enlarged view of point B in the middle;
[0036] Figure 7 for Figure 4 Enlarged view of point C in the middle;
[0037] Figure 8 The figure is a side view of a reaction device for preparing high-purity molybdenum trioxide according to the present invention.
[0038] In the figure:
[0039] 100, reactor; 110, first feed inlet; 120, second feed inlet; 130, discharge sleeve; 140, casing; 150, water inlet pipe; 160, water outlet pipe;
[0040] 200, filter bag; 210, mounting ring; 220, bag body; 230, regulating cylinder; 240, connecting ring; 241, mounting cavity; 250, air bag; 260, air pipe;
[0041] 300, lifting column; 310, axial slide bar; 320, suction channel; 330, first one-way valve; 340, suction hole; 350, drainage channel; 360, recessed portion; 370, drainage hole;
[0042] 400, lifting drive member; 410, rotating drum; 411, transition chamber; 412, second one-way valve; 413, liquid spray hole; 414, inverted cone guide plate; 420, spiral reciprocating groove; 430, connecting frame; 440, bayonet; 450, driving motor; 460, rotating shaft;
[0043] 500, spoiler; 510, limit plate; 520, collar; 530, rocker; 540, roller; 550, push plate; 560, return spring. DETAILED DESCRIPTION
[0044] The subject matter described herein will now be discussed with reference to example embodiments. It should be understood that the discussion of these embodiments is only to enable those skilled in the art to better understand and implement the subject matter described herein, and the functions and arrangements of the elements discussed may be changed without departing from the scope of protection of the contents of this specification. Each example may omit, replace or add various processes or components as needed. In addition, the features described relative to some examples may also be combined in other examples.
[0045] See also Figure 1 , Figure 2 and Figure 4The first aspect of the present invention discloses a reaction device for preparing high-purity molybdenum trioxide, comprising a reactor 100, a filter bag 200, a lifting column 300, a lifting drive member 400 and a spoiler 500. The upper end of the reactor 100 is respectively provided with a first feed port 110 and a second feed port 120, and the lower end of the reactor 100 is provided with a discharge sleeve 130 at the center; the filter bag 200 is arranged in the reactor 100, comprising a mounting ring 210 that can be lifted and lowered and a bag body 220 connected to the mounting ring 210; the lifting column 300 is lifted and lowered in the discharge sleeve 130, and the lifting column 300 is detachably connected to the bag body 220 at the center; the lifting drive member 400 is arranged at the upper end of the reactor 100, and is used to drive the lifting column 300 to move up and down; the spoiler 500 is movably arranged on the lifting column 300 and is located in the bag body 220;
[0046] Specifically, ammonium molybdate solution and nitric acid are added to the reactor 100 from the first feed port 110 and the second feed port 120 according to the reaction ratio; in the process of preparing high-purity molybdenum trioxide by reaction, the lifting column 300 is driven to move up and down reciprocatingly by the lifting drive 400, so that the center of the bag body 220 repeatedly rises and falls up and down, and under the action of the bag body 220 shaking up and down, the reaction solutions of different layers in the reactor 100 pass through the bag body 220 back and forth and mix, which effectively promotes the mixing of the reaction solutions in the vertical direction, enhances the hierarchical fluidity of the solution, and thus improves the mixing efficiency; in the process of the reciprocating lifting and lowering movement of the lifting column 300, the spoiler 500 is triggered at the same time to push the reaction solution at the center of the bag body 220 radially outward, so as to achieve radial mixing of the reaction solution, which helps to break any local concentration gradient that may exist and ensure that the reactants are evenly distributed in the entire reactor 100;
[0047] It is worth noting that traditional stirring mixing may have stirring dead corners, resulting in uneven mixing. Compared with traditional stirring mixing, the present invention realizes a more complex and efficient mixing mode through the up and down shaking of the bag body 220 and the radial push of the spoiler 500, effectively avoiding stirring dead corners, ensuring that the reaction solution in the entire reactor 100 can be fully mixed, reducing local overheating or overcooling during the reaction process, and making the heat distribution more uniform, which is crucial for controlling reaction conditions and improving product purity.
[0048] In one embodiment, see Figure 3 The lifting drive member 400 includes a driving motor 450 fixed to the top of the reactor 100, a rotating shaft 460 connected to the output end of the driving motor 450, a rotating drum 410 coaxially fixed to the rotating shaft 460, and a connecting frame 430 fixed to the lifting column 300, wherein the rotating drum 410 is provided with a spiral reciprocating groove 420, and the connecting frame 430 is provided with a bayonet 440 adapted to the spiral reciprocating groove 420;
[0049] Specifically, the driving motor 450 drives the rotating shaft 460 and the rotating drum 410 to rotate synchronously. Since the lifting column 300 can only perform axial lifting and lowering motion relative to the discharge sleeve 130 in the vertical direction, but cannot perform circumferential rotation relative to the discharge sleeve 130, when the rotating drum 410 rotates circumferentially, the bayonet 440 adaptively moves along the spiral reciprocating groove 420, so that the height of the bayonet 440 changes, thereby driving the lifting column 300 to adjust the height. With the continuous rotation of the rotating drum 410, the lifting column 300 can be driven to perform reciprocating lifting and lowering motion, so as to achieve the up and down shaking effect of the bag body 220;
[0050] It is worth noting that by driving the motor 450 to drive the rotating shaft 460 and the rotating drum 410 to rotate synchronously, the lifting column 300 can be precisely controlled, which helps to adjust the up and down shaking amplitude and frequency of the bag body 220, thereby finely controlling the reaction conditions in the reactor 100; the latch 440 moves adaptively along the spiral reciprocating groove 420, so that the height of the lifting column 300 can be dynamically adjusted. This adaptive adjustment mechanism allows the position of the bag body 220 to be adjusted at different reaction stages or under different reactant characteristics to optimize the mixing effect; the reciprocating lifting motion of the lifting column 300 drives the bag body 220 to shake up and down. This dynamic mixing in the vertical direction helps to break the laminar flow in the reactor 100 and enhance turbulence, thereby increasing the contact area between the reactants and the reaction efficiency; compared with traditional agitators, the above-mentioned driving method is easy to disassemble and clean, which helps to maintain the cleanliness of the reactor 100 and reduce the risk of cross contamination.
[0051] Furthermore, considering that the lifting column 300 can only move up and down, but cannot rotate in the circumferential direction, for this reason, please refer to Figure 4 The lifting column 300 is provided with a plurality of axial slide bars 310 slidably matched with the discharge sleeve 130; when the lifting column 300 moves up and down, the axial slide bars 310 slide axially relative to the discharge sleeve 130; in addition, in order to prevent the reaction solution in the reactor 100 from leaking, the sealing between the lifting column 300 and the discharge sleeve 130 needs to be ensured.
[0052] For further information, see Figure 3 The spoiler 500 includes a limit plate 510 fixed on the lifting column 300 and a collar 520 movably sleeved on the lifting column 300, a swing rod 530 is rotatably connected to the collar 520, a roller 540 is rotatably mounted on one end of the swing rod 530 away from the collar 520, and a flow pushing plate 550 is also provided on the swing rod 530; a return spring 560 is provided between the limit plate 510 and the collar 520, and the return spring 560 is movably sleeved on the lifting column 300;
[0053] Specifically, in the initial state, due to the elastic force of the return spring 560, the collar 520 is pushed up, and the swing rod 530 is in the retracted and folded state. When the lifting column 300 rises and pushes the center of the bag body 220 upward, under the action of inertia, the collar 520 moves toward the lower limit plate 510 along the lifting column 300. Since the roller 540 is always in contact with the upper end surface of the bag body 220, the swing rod 530 is forced to swing outward and unfold, thereby driving each flow-pushing plate 550 to push the reaction solution at the center of the bag body 220 radially outward. 0 descends and drives the bag body 220 to reset, under the action of inertia and the elastic force of the reset spring 560, the collar 520 resets upward along the lifting column 300, thereby driving the swing rod 530 to radially contract, and then driving the flow-pushing plate 550 to radially gather the peripheral reaction solution toward the center of the reactor 100, and so on, to achieve radial turbulence of the reaction solution; during the radial flow-pushing process of the flow-pushing plate 550, the roller 540 also rolls back and forth on the bag body 220, which can crush the particles that have not been completely dissolved on the bag body 220, so as to break the particles and further dissolve them;
[0054] The design of the spoiler 500 realizes radial spoiler of the reaction solution through the cooperation of the rocker rod 530 and the flow-pushing plate 550. This reciprocating radial flow-pushing action effectively promotes the mixing of the reaction solution in the reactor 100 and improves the mixing uniformity. When the lifting column 300 rises, the flow-pushing plate 550 pushes the reaction solution to the periphery, and when it descends, it gathers the peripheral solution to the center. This dynamic process enhances the mixing of the solution and helps to improve the reaction rate and product quality. In addition, the roller 540 rolls back and forth on the bag body 220 to crush the particles that have not been completely dissolved, causing the particles to break and further dissolve, which helps to improve the dissolution efficiency of the reactants and reduce the impact of undissolved particles on the reaction efficiency.
[0055] It is worth noting that the design of the spoiler 500 realizes radial spoiler of the reaction solution through the reciprocating motion of the swing rod 530 and the flow-pushing plate 550, so that when the bag body 220 shakes up and down, the flow-pushing plate 550 can push the reaction solution at the center to the periphery, and then gather the peripheral solution to the center, forming effective radial mixing. This synergistic effect significantly improves the stirring effect, speeds up the reaction speed between the reaction solutions, and improves the mixing efficiency.
[0056] The spoiler 500 can increase the turbulent kinetic energy level inside the reactor 100, thereby improving the macroscopic mixing effect inside the reactor 100. During the process of radially and repeatedly pushing the flow by the pushing plate 550, the roller 540 also rolls back and forth on the bag body 220, which can crush the particles on the bag body 220 that have not been completely dissolved, promote the particle breakage and further dissolution, thereby providing better mass transfer efficiency for the electrochemical reaction process.
[0057] To further improve the mixing effect, see Figure 5 and Figure 6 The rotating drum 410 is provided with a transition chamber 411 with an opening at the lower end, the upper end of the lifting column 300 is movably embedded in the transition chamber 411, and the upper end of the lifting column 300 is provided with a suction channel 320 connected with the transition chamber 411; a plurality of suction holes 340 are provided at the bottom of the suction channel 320, a plurality of liquid injection holes 413 are circumferentially provided at the upper end of the transition chamber 411, and an inverted cone-shaped guide plate 414 adapted to the liquid injection holes 413 is provided at the top of the rotating drum 410; a first one-way valve 330 is installed in the suction channel 320, and a second one-way valve 412 is installed at the top of the transition chamber 411;
[0058] Specifically, when the lifting column 300 descends relative to the rotating drum 410, the first one-way valve 330 is opened and the second one-way valve 412 is closed, so that the reaction solution at the center of the bag body 220 is sucked into the transition chamber 411 through the suction hole 340 and the suction channel 320; when the lifting column 300 rises relative to the rotating drum 410, the first one-way valve 330 is closed and the second one-way valve 412 is opened, so that the reaction solution in the transition chamber 411 is sprayed out from each spray hole 413, and the sprayed reaction solution is thrown out to the outside under the guidance of the inverted cone guide plate 414, so as to achieve the effect of sucking the reaction solution at the center of the bottom layer and spraying it to the periphery of the upper layer, further improving the mixing effect of the reaction solution inside the reactor 100;
[0059] By the up and down movement of the lifting column 300, in coordination with the operation of the suction channel 320 and the spray hole 413, the reaction solution is circulated from the center of the bottom layer to the periphery of the upper layer. This circulating flow helps to break the local concentration gradient inside the reactor 100 and enhance the mixing uniformity; by sucking and spraying the reaction solution, in coordination with the inverted cone guide plate 414, the sprayed reaction solution is evenly distributed around the reactor 100, which increases the turbulence of the solution, thereby improving the mass transfer efficiency and helping to increase the reaction rate.
[0060] In another embodiment, after the reaction solution is fully mixed, the lifting column 300 is lifted to the highest point by the lifting drive 400, so that the center of the bag body 220 maintains an upward bulging posture. At this time, the reaction solution in the reactor 100 is all below the bag body 220, and then the ammonium molybdate solution and nitric acid are waited to react to produce acid precipitation crystals to generate molybdenum trioxide precipitation. After the reaction is completed, in order to facilitate the acquisition of the lower layer of molybdenum trioxide precipitation, the upper clear liquid needs to be discharged. For this purpose, please refer to Figure 4 and Figure 7The lower end of the lifting column 300 is provided with a drainage channel 350 connected to the outside, and the upper end of the drainage channel 350 is provided with a plurality of drainage holes 370 connected to the reactor 100; a connecting ring 240 is provided at the center of the bag body 220, and a sealing connector adapted to the lifting column 300 is provided on the connecting ring 240;
[0061] Specifically, during the mixing process, the connecting ring 240 is fixedly connected to the lifting column 300 through the sealing connecting piece, so that the bag body 220 can be driven to shake up and down synchronously during the lifting process of the lifting column 300, so as to achieve the hierarchical turbulence effect on the reaction solution, and at the same time, the sealing connecting piece blocks the drainage hole 370 to prevent the reaction solution from being discharged from the drainage channel 350; after the reaction is completed and molybdenum trioxide precipitation is generated, the sealing connecting piece releases the connection function, so that the connecting ring 240 is no longer relatively fixed to the lifting column 300, and the entire filter bag 200 is moved downward until The bag body 220 contacts the uppermost layer of molybdenum trioxide precipitate and covers the surface of the molybdenum trioxide precipitate. At this time, the drainage hole 370 is connected, so that the upper clear liquid in the reactor 100 can be discharged through the drainage hole 370 and the drainage channel 350. As the liquid level of the upper clear liquid continues to drop, the lifting column 300 can be driven to drop synchronously by the lifting drive member 400, thereby gradually lowering the height of the drainage hole 370, so that the upper clear liquid is discharged layer by layer until the upper clear liquid is completely discharged, and then the molybdenum trioxide precipitate in the reactor 100 is fished out and dried to obtain a high-purity molybdenum trioxide product.
[0062] It should be noted that, in the process of discharging the supernatant, the bag body 220 can wrap and cover the molybdenum trioxide precipitate in the lower layer, thereby preventing the molybdenum trioxide precipitate from being discharged with the supernatant and causing the loss of the molybdenum trioxide precipitate, thereby improving the yield of the high-purity molybdenum trioxide product;
[0063] In addition, in actual applications, the pore size of the bag body 220 can be set according to actual needs to ensure that the reaction solution can pass through smoothly, but the molybdenum trioxide precipitate cannot pass through smoothly. In other words, the pore size of the bag body 220 is larger than the molecular size of the reaction solution, but smaller than the size of the molybdenum trioxide precipitate.
[0064] For further information, see Figure 7 The sealing connection member includes a mounting cavity 241 provided in the connecting ring 240 and an airbag 250 embedded in the mounting cavity 241, and a concave portion 360 adapted to the airbag 250 is provided on the periphery of the drainage hole 370;
[0065] Specifically, during the mixing process, the airbag 250 expands and embeds into the recessed portion 360, thereby achieving a fixed connection between the connecting ring 240 and the lifting column 300, and at the same time, the expanded airbag 250 blocks the drainage hole 370; during the discharge of the upper clear liquid, the airbag 250 shrinks back into the mounting cavity 241, thereby releasing the lock between the connecting ring 240 and the lifting column 300, and at the same time making the drainage hole 370 conductive.
[0066] Furthermore, considering that during the discharge of the upper clear liquid, the entire filter bag 200 needs to be moved downward so that the bag body 220 can cover and wrap the molybdenum trioxide precipitation in the lower layer. Figure 2 A plurality of regulating cylinders 230 are arranged circumferentially at the bottom of the reactor 100. The output end of the regulating cylinder 230 is fixedly connected to the connecting ring 240. An air pipe 260 is also connected between the regulating cylinder 230 and the air bag 250.
[0067] Specifically, during the mixing process, the output end of the regulating cylinder 230 is extended, so that the connecting ring 240 is pushed upward, so that the entire filter bag 200 is located in the middle of the reactor 100 and remains unchanged, ensuring that the bag body 220 does not interfere with the inner wall of the reactor 100 during the up and down shaking process; at the same time, the regulating cylinder 230 inflates the airbag 250 to expand the airbag 250, so as to automatically realize the fixed connection between the connecting ring 240 and the lifting column 300 and the blocking of the drainage hole 370;
[0068] During the process of discharging the upper clear liquid, the output end of the regulating cylinder 230 is retracted, thereby driving the entire filter bag 200 to move downward, so as to wrap and cover the molybdenum trioxide precipitate in the lower layer to prevent the molybdenum trioxide precipitate from being lost; at the same time, the regulating cylinder 230 evacuates the airbag 250 to shrink and deflate the airbag 250, so as to automatically realize the separation of the connecting ring 240 and the lifting column 300 and the conduction of the drainage hole 370.
[0069] It is worth noting that, during the mixing process, the lifting column 300 drives the bag body 220 to shake up and down to achieve a hierarchical turbulence effect, and at the same time, the sealing connector blocks the drainage hole 370 to ensure that the reaction solution will not be lost during the mixing process; after the reaction is completed, the locking effect of the sealing connector is released, so that the connecting ring 240 and the lifting column 300 are no longer fixed, the entire filter bag 200 moves downward, and the drainage hole 370 is connected to achieve smooth discharge of the upper clear liquid. This process simplifies the traditional complex separation steps and improves the operating efficiency. The bag body 220 can cover and wrap the molybdenum trioxide precipitate in the lower layer during the discharge of the upper clear liquid, thereby avoiding the loss of the precipitate with the clear liquid and improving the yield of the molybdenum trioxide product;
[0070] The airbag 250 in the sealing connector expands to block the drainage hole 370 during the mixing process, and contracts to release the blockage when discharging the clear liquid. This automated sealing and unlocking mechanism reduces manual intervention and improves the safety and convenience of operation; the adjusting cylinder 230 lifts up the connecting ring 240 during the mixing process to keep the position of the filter bag 200 stable, and at the same time inflates the airbag 250 to achieve automatic fixation and sealing. When discharging the clear liquid, the adjusting cylinder 230 drives the filter bag 200 to move downward, and at the same time, air is pumped to shrink the airbag 250 to achieve automatic unlocking and conduction of the drainage hole 370. During the whole process, the linkage between the adjusting cylinder 230 and the airbag 250 reduces manual operation, reduces the complexity of operation, and improves the efficiency and safety of operation.
[0071] In addition, a casing 140 is disposed outside the reactor 100, a water inlet pipe 150 is disposed at the bottom of the casing 140, and a water outlet pipe 160 is disposed at the top of the casing 140;
[0072] Specifically, during the reaction process, hot water is introduced from the water inlet pipe 150 at the lower end to heat the reaction solution in the reactor 100, and the hot water that absorbs heat flows out from the water outlet pipe 160 at the upper end, thereby achieving uniform heating of the reaction solution in the reactor 100, which helps to maintain the uniformity of the internal temperature of the reactor 100 and avoid local overheating or overcooling, thereby ensuring the uniform progress of the chemical reaction.
[0073] See also Figure 8 The second aspect of the present invention discloses a method for preparing high-purity molybdenum trioxide using a reaction device, comprising the following steps:
[0074] S1, adding ammonium molybdate solution and nitric acid into the reactor 100 from the first feed port 110 and the second feed port 120 respectively;
[0075] S2, the lifting column 300 is driven to move up and down by the lifting driving member 400, so as to drive the bag body 220 to shake up and down, so as to achieve mixed flow of reaction solutions at different levels, and at the same time drive the spoiler 500 to radially spoil the reaction solution;
[0076] S3, after the mixing is completed, the bag body 220 is lifted up so that the reaction solution is completely under the bag body 220;
[0077] S4, after the acid precipitation crystallization is completed, the filter bag 200 moves downward, so that the bag body 220 wraps and covers the lower layer of molybdenum trioxide precipitation, and the upper clear liquid is discharged;
[0078] S5. The molybdenum trioxide precipitate is fished out and dried to obtain a high-purity molybdenum trioxide product.
[0079] The specific implementation methods of this embodiment are described above, but this embodiment is not limited to the above-mentioned specific implementation methods. The above-mentioned specific implementation methods are merely illustrative and not restrictive. Ordinary technicians in this field can also make many forms inspired by this embodiment, all of which are within the protection of this embodiment.
Claims
1. A reaction device for preparing high-purity molybdenum trioxide, characterized in that: include: A reaction kettle (100), wherein a first feed inlet (110) and a second feed inlet (120) are respectively arranged at the upper end thereof, and a discharge sleeve (130) is arranged at the center of the lower end of the reaction kettle (100); A filter bag (200) is arranged in the reaction kettle (100), comprising a mounting ring (210) that can be raised and lowered and a bag body (220) connected to the mounting ring (210); A lifting column (300) is liftably sleeved in the discharge sleeve (130), and the lifting column (300) is detachably connected to the center of the bag body (220); A lifting drive member (400), which is arranged at the upper end of the reaction kettle (100) and is used to drive the lifting column (300) to move upward and downward; The spoiler (500) is movably arranged on the lifting column (300) and is located in the bag body (220).
2. A reaction device for preparing high-purity molybdenum trioxide according to claim 1, characterized in that: The lifting drive member (400) comprises a driving motor (450) fixed to the top of the reaction kettle (100), a rotating shaft (460) connected to the output end of the driving motor (450), a rotating drum (410) fixed coaxially with the rotating shaft (460), and a connecting frame (430) fixed to the lifting column (300), wherein the rotating drum (410) is provided with a spiral reciprocating groove (420), and the connecting frame (430) is provided with a latch (440) adapted to the spiral reciprocating groove (420).
3. A reaction device for preparing high-purity molybdenum trioxide according to claim 1, characterized in that: The lifting column (300) is provided with a plurality of axial slide bars (310) slidably matched with the discharge sleeve (130); when the lifting column (300) moves up and down, the axial slide bars (310) slide axially relative to the discharge sleeve (130).
4. A reaction device for preparing high-purity molybdenum trioxide according to claim 2, characterized in that: The spoiler (500) comprises a limit plate (510) fixed on the lifting column (300) and a collar (520) movably sleeved on the lifting column (300); a swing rod (530) is rotatably connected to the collar (520); a roller (540) is rotatably mounted on one end of the swing rod (530) away from the collar (520); and a flow pushing plate (550) is also provided on the swing rod (530); a return spring (560) is provided between the limit plate (510) and the collar (520); and the return spring (560) is movably sleeved on the lifting column (300).
5. A reaction device for preparing high-purity molybdenum trioxide according to claim 2, characterized in that: A transition chamber (411) with an opening at the lower end is provided in the rotating cylinder (410); the upper end of the lifting column (300) is movably embedded in the transition chamber (411); a suction channel (320) communicating with the transition chamber (411) is provided at the upper end of the lifting column (300); a plurality of suction holes (340) are provided at the bottom of the suction channel (320); a plurality of liquid spray holes (413) are provided in the circumferential direction at the upper end of the transition chamber (411); an inverted cone-shaped guide plate (414) adapted to the liquid spray holes (413) is provided at the top of the rotating cylinder (410); a first one-way valve (330) is installed in the suction channel (320); and a second one-way valve (412) is installed at the top of the transition chamber (411).
6. A reaction device for preparing high-purity molybdenum trioxide according to claim 5, characterized in that: The lower end of the lifting column (300) is provided with a drainage channel (350) connected to the outside, and the upper end of the drainage channel (350) is provided with a plurality of drainage holes (370) connected to the inside of the reaction kettle (100); a connecting ring (240) is provided at the center of the bag body (220), and a sealing connecting piece adapted to the lifting column (300) is provided on the connecting ring (240).
7. A reaction device for preparing high-purity molybdenum trioxide according to claim 6, characterized in that: The sealing connection member comprises a mounting cavity (241) provided in the connecting ring (240) and an airbag (250) embedded in the mounting cavity (241); a recessed portion (360) adapted to the airbag (250) is provided on the periphery of the drainage hole (370).
8. A reaction device for preparing high-purity molybdenum trioxide according to claim 7, characterized in that: A plurality of regulating cylinders (230) are arranged circumferentially at the bottom of the reaction kettle (100); the output ends of the regulating cylinders (230) are fixedly connected to the connecting ring (240); and an air pipe (260) is also connected between the regulating cylinders (230) and the airbag (250).
9. A reaction device for preparing high-purity molybdenum trioxide according to claim 1, characterized in that: A casing (140) is disposed outside the reaction kettle (100), a water inlet pipe (150) is disposed at the bottom of the casing (140), and a water outlet pipe (160) is disposed at the top of the casing (140).
10. A method for preparing high-purity molybdenum trioxide using the reaction device according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1, adding ammonium molybdate solution and nitric acid into a reaction kettle (100) from a first feed port (110) and a second feed port (120), respectively; S2, driving the lifting column (300) to move up and down by means of the lifting driving member (400), driving the bag body (220) to shake up and down, thereby achieving mixed flow of reaction solutions at different levels, and driving the spoiler (500) to radially spoil the reaction solution; S3, after the mixing is completed, the bag body (220) is lifted up so that the reaction solution is completely under the bag body (220); S4, after the acid precipitation crystallization is completed, the filter bag (200) moves downward, so that the bag body (220) wraps and covers the molybdenum trioxide precipitate in the lower layer, and the upper clear liquid is discharged; S5. The molybdenum trioxide precipitate is fished out and dried to obtain a high-purity molybdenum trioxide product.
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