Neutralization kettle for gallium purification
By adopting a composite flow mode of three stirred leaves in the gallium purification neutralization kettle, the problem of uneven mixing of analytical qualified liquid and alkali liquid during the gallium purification process is solved, the reaction efficiency and product quality are improved, and the production cost is reduced.
Patent Information
- Application Number
- CN202411811300.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-10
- Publication Date
- 2025-03-07
AI Technical Summary
During the gallium purification process, the mixture of the analytical qualified liquid and the alkali liquid in the neutralization kettle is uneven, resulting in insufficient reaction and affecting the purity and yield of the gallium crystallization.
A neutralizing kettle for gallium purification was designed, and three different types of stirred leaves (first propulsion type, turbine type and second propulsion type stirred leaves) were combined to form a composite flow mode to ensure the full contact and mixing of the analytical qualified liquid and the alkali liquid in the neutralizing kettle.
Through the stirring design of the composite flow mode, the mixing uniformity of the analytical qualified liquid and the alkali liquid is improved, the efficiency of neutralization reaction is enhanced, the time of the gallium purification process is shortened, the components of the qualified liquid are stabilized, the purity and yield of the gallium crystals are improved, and the production cost is reduced.
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Figure CN119571058A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of gallium purification, and particularly relates to a neutralization kettle for gallium purification. Background Art
[0002] Gallium, as an important metal element, has a wide range of applications in the field of modern science and technology, and its purification process has attracted much attention. Currently, most gallium is purified from aluminum hydroxide solution. Specifically, the mother liquor formed after the aluminum hydroxide solution is filtered contains gallium. After the aluminum hydroxide and chelating resin are placed in the adsorption tower, the chelating resin will adsorb the gallium in the chelating resin; the mother liquor in the adsorption tower is discharged, and the concentrated sulfuric acid is diluted and discharged into the adsorption tower to react with the chelating resin containing gallium to obtain a qualified solution for analysis; the qualified solution for analysis is sent to the neutralization kettle, and then the diluted alkali solution is sent to the neutralization kettle for neutralization to obtain a qualified solution, which is discharged through the discharge hole at the bottom of the neutralization kettle. The qualified solution is subjected to centrifugal treatment, impurity removal, filter pressing, electrolysis and other processes to obtain gallium crystals.
[0003] When the qualified solution is neutralized in the neutralization kettle, the reaction solution (alkali solution and qualified solution) in the neutralization kettle is generally stirred by a stirrer. The alkali solution is generally added from the top of the neutralization kettle. Since the alkali solution first contacts the qualified solution at the top, the concentration of the reactants in the top area increases instantly, and the reaction rate is sharply accelerated. In contrast, it is difficult for the reactants in the bottom area to fully contact a sufficient amount of alkali solution for a long time, resulting in serious reaction lag and insufficient reaction. This reaction inhomogeneity will not only affect the efficiency of the neutralization reaction, prolong the time of the entire purification process, and increase production costs, but also may lead to unstable quality of the reaction product. The composition of the qualified solution after neutralization fluctuates greatly, which brings many adverse effects to subsequent processes such as centrifugation, impurity removal, filter pressing, and electrolysis, and ultimately affects the purity and yield of gallium crystals. Summary of the invention
[0004] The invention aims to provide a neutralization kettle for purifying gallium, so as to improve the uniformity of mixing the analyzed qualified solution with the alkaline solution.
[0005] A neutralization kettle for gallium purification in this scheme includes a kettle body, a motor is provided on the top of the kettle body, the output shaft of the motor is fixedly connected to a stirring shaft, a first feed hole is provided on the top of the kettle body, and a discharge hole is provided on the bottom; the stirring shaft is provided with a first propulsion stirring blade, a turbine stirring blade and a second propulsion stirring blade in sequence from top to bottom.
[0006] The working principle of this scheme is: the qualified solution is discharged into the body of the neutralization kettle through the first feed hole, and then the alkali solution is discharged into the neutralization kettle at one time or in batches through the first feed hole. Start the motor, the motor drives the stirring shaft to rotate, and the first propulsion stirring blade, turbine stirring blade and second propulsion stirring blade on the stirring shaft rotate together with the stirring shaft. During the stirring process, since the first propulsion stirring blade is located at the upper part of the stirring shaft, it generates an axial flow, pushing the qualified solution and alkali solution near the top downward, preventing the reactants at the top from excessively gathering, and allowing the reactants at the top to move quickly to the middle and bottom. The turbine stirring blade is in the middle of the stirring shaft and mainly generates radial flow. It forms a strong shear force in the middle area of the kettle body, and quickly disperses and mixes the qualified solution and alkali solution coming down from the top in a radial direction, so that the reactants in the middle area can fully contact and avoid local uneven concentration. The second propulsion stirring blade is at the bottom of the stirring shaft, generating an axial flow, pushing the reactants at the bottom upward. It can effectively bring the reactants at the bottom to the middle and top, and pull the reactants at the middle and top downward, forming a complete up-and-down circulation flow pattern. The qualified solution after sufficient mixing and reaction with the alkali solution is discharged through the discharge hole at the bottom of the kettle body and enters the subsequent centrifugal treatment, impurity removal, filter pressing, electrolysis and other processes.
[0007] Beneficial effects of this solution: 1. Through the synergistic effect of three different types of stirring blades, an axial and radial composite flow is formed to ensure that the qualified solution and the alkali solution can fully contact and mix in all areas of the neutralization kettle, solving the problem of insufficient bottom reaction caused by the addition of alkali solution from the top of the traditional neutralization kettle, and improving the uniformity of the reaction. 2. The uniform mixing enables the reaction to proceed quickly and fully in the entire kettle, reducing the extension of the reaction time caused by uneven local reactions, thereby improving the efficiency of the neutralization reaction and shortening the time of the entire gallium purification process. 3. Due to the uniform reaction, the composition of the qualified solution after neutralization is more stable, reducing the fluctuation of the composition, providing a more stable quality raw material for subsequent centrifugal treatment, impurity removal, filter pressing, electrolysis and other processes, which is conducive to improving the purity and yield of gallium crystals. 4. Improve the reaction efficiency and stabilize the product quality, reduce the rework and waste caused by insufficient reaction or unqualified product quality, reduce the consumption of raw materials and energy, and thus reduce the production cost of gallium purification.
[0008] Furthermore, the second propulsion stirring blade is a spiral stirring blade. The spiral stirring blade has a better axial pushing ability in structure, and can more effectively transport the reactants at the bottom upward, ensuring that the reactants at the bottom can quickly participate in the entire mixing and reaction process. At the same time, during the neutralization reaction, some impurities or incompletely reacted particles may be deposited at the bottom. The rotation of the spiral stirring blade can prevent these substances from accumulating at the bottom.
[0009] Furthermore, a second feed hole is provided on the top of the kettle body. The alkali solution enters from the second feed hole on the top, and is discharged into the kettle body synchronously with the analytical qualified solution entering from the first feed hole, so that the reactants begin to disperse when entering the kettle body, thereby improving the initial mixing uniformity of the reactants in the kettle body.
[0010] Furthermore, an observation window is provided on the top of the kettle body, through which the operator can directly observe the reaction conditions in the kettle body, which helps to find abnormal conditions in time so as to take corresponding measures to make adjustments and ensure the normal progress of the reaction.
[0011] Furthermore, a sampling port is provided at the observation window, through which a sample of the reaction liquid in the kettle can be conveniently taken out for accurate pH value determination without affecting the normal progress of the reaction.
[0012] Furthermore, a mixing component is provided in the kettle body, and the mixing component is located directly above the first propulsion stirring blade. The mixing component includes a mixing disk and a plurality of guide vanes. A connecting cylinder is rotatably connected at the center of the mixing disk. The stirring shaft connecting the cylinder and the mixing disk are fixedly connected to the connecting cylinder and are coaxial. The outer wall of the connecting cylinder is provided with connecting ears of the same number as the guide vanes, and the plurality of guide vanes are respectively hinged on the corresponding connecting ears, and a torsion spring is provided at the connection between the guide vane and the connecting ear; the guide vane is arc-shaped, and the inner wall of the guide vane is in contact with the outer wall of the connecting cylinder, and the outer wall of the guide vane is in contact with the outer wall of the connecting cylinder under the action of the torsion spring. The inner wall of the mixing disk is contacted with the lower part; a guide block is integrally formed on the inner wall of the mixing disk, and the side of the guide block facing the connecting tube is a progressive arc, and the width of the narrowest part of the guide block and the connecting tube is equal to or slightly greater than the thickness of the guide plate; the mixing disk is provided with a liquid inlet and a liquid outlet, and the liquid outlet is located at the guide block, the liquid inlet is located on the side of the guide block, and the liquid inlet and the liquid outlet are located on both sides of the narrowest part of the guide block and the connecting tube; the liquid inlet is connected to a collection pipe, and the first feed hole and the second feed hole are both connected to the collection pipe, and a flow control valve is provided in the first feed hole and the second feed hole. After the analyzed qualified liquid and alkali solution enter the mixing disk from the collection pipe through the liquid inlet hole, under the synergistic action of the guide plate and the guide block, the materials are divided between the two adjacent guide plates, that is, the flow pushed by the two adjacent guide plates is consistent each time, and then discharged from the liquid outlet, to ensure a more accurate mixing of the analyzed qualified liquid and the alkali solution.
[0013] Furthermore, the bottom of the mixing plate is provided with a plurality of blind holes, each of which is provided with a stirring mechanism. The stirring mechanism enables the qualified solution and alkali solution entering the mixing plate to be fully stirred and mixed, further improving the mixing uniformity of the materials in the entire neutralization kettle.
[0014] Furthermore, the stirring mechanism includes a stirring rod and a plurality of mixing blades fixedly connected to the top of the stirring rod, and the mixing blades and the stirring rod are both located in the blind hole; a cavity is provided in the bottom wall of the mixing plate, and a driving gear and a plurality of driven gears meshing therewith are provided in the cavity, and the plurality of stirring rods are respectively fixedly connected to the plurality of driven gears, and the driving gear is fixedly connected to the stirring shaft. Through the gear transmission structure, the rotation of the stirring shaft can drive the driving gear to rotate, and then drive the plurality of driven gears and the stirring rods and mixing blades connected thereto to rotate, thereby realizing synchronous stirring at multiple positions at the bottom of the mixing plate; and because the driving gear and the driven gear have different rotation directions, that is, the guide vane and the mixing blade have different rotation directions, the qualified solution and the alkali solution can be mixed evenly to a greater extent.
[0015] Furthermore, the radius of the driven gear is smaller than the radius of the driving gear, which helps to increase the rotation speed of the driven gear, that is, to increase the rotation speed of the mixing blade, thereby improving the stirring effect.
[0016] Furthermore, the liquid outlet is connected to a guide tube, and the liquid outlet end of the guide tube is close to the stirring shaft, which helps the material to enter from a place close to the stirring shaft, thereby improving the pushing effect of the first propulsion stirring blade on the material. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 This is a schematic structural diagram of a neutralization kettle for gallium purification according to Example 1 of the present invention;
[0018] Figure 2 for Figure 1 A longitudinal cross-sectional view of
[0019] Figure 3 A longitudinal partial cross-sectional view of a neutralization kettle for gallium purification in Example 2;
[0020] Figure 4 for Figure 3 A top view of the mixing assembly without the top cover;
[0021] Figure 5 for Figure 4 Longitudinal section view after connecting the stirring shaft. DETAILED DESCRIPTION
[0022] The following is further described in detail through specific implementation methods:
[0023] The figure marks in the drawings of the specification include: kettle body 1, motor 2, first propulsion stirring blade 3, stirring shaft 4, turbine stirring blade 5, spiral stirring blade 6, discharge hole 7, observation window 8, first feed hole 9, second feed hole 10, collecting pipe 11, mixing component 12, liquid outlet 121, mixing disk 122, liquid inlet 123, blind hole 124, mixing blade 125, guide plate 126, connecting tube 127, connecting ear 128, guide block 129, driving gear 130.
[0024] Embodiment 1 is basically as attached Figures 1-2 As shown: A neutralization kettle for gallium purification, comprising a kettle body 1, a motor 2 is installed on the top of the kettle body 1, an output shaft of the motor 2 is fixedly connected to a stirring shaft 4, the stirring shaft 4 extends into the kettle body 1 and is close to the inner bottom of the kettle body 1, and a first propulsion stirring blade 3, a turbine stirring blade 5 and a spiral stirring blade 6 are arranged on the stirring shaft 4 from top to bottom, the turbine stirring blade 5 is located in the middle of the kettle body 1, the spiral stirring blade 6 is close to the bottom of the kettle body 1, and the first propulsion stirring blade 3 is close to the inner top of the valve body; a first feed hole 9 and a second feed hole 10 passing through the top wall of the kettle body 1 are provided, and three observation windows 8 are also provided on the top wall of the kettle body 1, and a sampling port is provided at the observation window 8; a discharge hole 7 is provided at the bottom of the kettle body 1.
[0025] The specific implementation process is as follows: according to the ratio required for the reaction, the qualified solution and the alkali solution are discharged into the neutralization kettle synchronously through the first feed hole 9 and the second feed hole 10 respectively; or the qualified solution is discharged into the kettle body 1 first, and then the alkali solution is introduced from the first feed hole 9 and the second feed hole 10. The motor 2 is started while the alkali solution is introduced, and the output shaft of the motor 2 drives the stirring shaft 4 to rotate. The first propulsion stirring blade 3, the turbine stirring blade 5 and the spiral stirring blade 6 on the stirring shaft 4 rotate together with the stirring shaft 4, and the first propulsion stirring blade 3, the turbine stirring blade 5 and the spiral stirring blade 6 realize the mixing of the qualified solution and the alkali solution. After the qualified solution and the alkali solution react for a certain period of time, the operator can directly observe the reaction situation in the kettle body 1 through the observation window 8 on the top of the kettle body 1, and take corresponding measures to adjust according to the observed situation. At the same time, using the sampling port at the observation window 8, the reaction liquid sample in the kettle body 1 can be conveniently taken out for accurate pH value measurement without affecting the normal progress of the reaction. According to the pH value measurement result, the progress of the reaction and whether the ratio of the reactants is appropriate can be further judged. If the pH value is not within the expected range, the amount of alkali solution added can be adjusted in time to ensure the normal reaction. When the pH value reaches the appropriate range and stabilizes, the qualified liquid after sufficient mixing and reaction is discharged through the discharge hole 7 at the bottom of the kettle body 1 and enters the subsequent centrifugal treatment, impurity removal, filter pressing, electrolysis and other processes.
[0026] Embodiment 2 is basically as attached Figures 3 to 5As shown, the difference between it and embodiment 1 is that: a mixing assembly 12 is provided in the kettle body 1, and the mixing assembly 12 is located directly above the first propulsion stirring blade 3. The mixing assembly 12 includes a mixing disk 122 and three guide plates 126. A connecting cylinder 127 is rotatably connected at the center of the mixing disk 122. The stirring shaft 4 is connected to the connecting cylinder 127 and the mixing disk 122. The stirring shaft 4 is fixedly connected to the connecting cylinder 127 and is coaxial. Three connecting ears 126 are integrally formed on the outer wall of the connecting cylinder 127. 8. Three connecting ears 128 are evenly distributed on the outer wall of the connecting tube 127. Three guide plates 126 are respectively hinged on the corresponding connecting ears 128. A torsion spring is provided at the connection between the guide plate 126 and the connecting ear 128. Specifically, a notch is provided on the outer wall of the connecting ear 128. A protrusion is integrally formed at one end of the guide plate 126. The protrusion is fixedly connected with a hinge rod. The guide plate 126 is hinged at the notch of the connecting ear 128 through the hinge rod. A torsion spring is provided at the connection between the hinge rod and the connecting ear 128. The flow piece 126 is arc-shaped, and the inner wall of the flow guide piece 126 is in contact with the outer wall of the connecting tube 127. The outer wall of the flow guide piece 126 contacts the inner wall of the mixing plate 122 under the action of the torsion spring; a flow guide block 129 is integrally formed on the inner wall of the mixing plate 122, and the side of the flow guide block 129 facing the connecting tube 127 is a progressive arc, and the narrowest width of the flow guide block 129 and the connecting tube 127 is equal to or slightly greater than the thickness of the flow guide piece 126 (greater than the thickness of the flow guide piece 126 by 0.1 to 0.5 mm); The mixing plate 122 is provided with a liquid inlet hole 123 and a liquid outlet hole 121, the liquid outlet hole 121 is located at the guide block 129, the liquid inlet hole 123 is located on the side of the guide block 129, and the liquid inlet hole 123 and the liquid outlet hole 121 are located on both sides of the narrowest part of the guide block 129 and the connecting tube 127; the liquid inlet hole 123 is connected to the collecting pipe 11, the first feed hole 9 and the second feed hole 10 are both connected to the collecting pipe 11, and the first feed hole 9 and the second feed hole 10 are both provided with flow control valves;
[0027] Five blind holes 124 are provided at the bottom of the mixing disk 122, and a stirring mechanism is provided in each of the blind holes 124. The stirring mechanism includes a stirring rod and four mixing blades 125 fixedly connected to the top of the stirring rod, and the mixing blades 125 and the stirring rod are both located in the blind hole 124; a cavity is provided in the bottom wall of the mixing disk 122, and a driving gear 130 and five driven gears meshing therewith are provided in the cavity, the five stirring rods are fixedly connected to the five driven gears respectively, the driving gear 130 is fixedly connected to the stirring shaft 4, and the radius of the driven gear is smaller than the radius of the driving gear 130.
[0028] Specific implementation method: According to the ratio required by the reaction, the qualified solution and the alkali solution enter the collecting pipe 11 through the first feed hole 9 and the second feed hole 10 respectively, and under the control of the flow control valve, the two flow into the mixing plate 122 at the set flow rate. The qualified solution and the alkali solution entering the mixing plate 122 enter from the liquid inlet 123. During this process, the stirring shaft 4 rotates to drive the connecting cylinder 127 to rotate, and the connecting ear 128 on the outer wall of the connecting cylinder 127 drives the guide plate 126 to rotate. Because the guide plate 126 is hinged with the connecting ear 128 and has a torsion spring, under the impact of the material and the action of the torsion spring, the guide plate 126 will open and close regularly to achieve the division and mixing of the material. At the same time, the driving gear 130 rotates with the stirring shaft 44, and the driving gear 130 drives the five driven gears to rotate, thereby causing the stirring rod connected to the driven gear and the mixing blade 125 on the top of the stirring rod to rotate in the blind hole 124; since the driving gear 130 and the driven gear rotate in different directions, that is, the guide blade 126 and the mixing blade 125 rotate in different directions, the qualified solution and the alkali solution are mixed evenly in the mixing pan 122 to a greater extent. The subsequent operations are consistent with those in Example 1 and will not be repeated here.
[0029] The only difference between Example 3 and Example 2 is that the liquid outlet hole 121 is connected with a flow guide tube, and the liquid outlet end of the flow guide tube is close to the stirring shaft 4 .
[0030] The above is only an embodiment of the present invention, and the common knowledge such as the known specific structure and characteristics in the scheme is not described in detail here. It should be pointed out that for those skilled in the art, several deformations and improvements can be made without departing from the structure of the present invention, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.
Claims
1. A neutralization kettle for gallium purification, comprising a kettle body, a motor is arranged on the top of the kettle body, a stirring shaft is fixedly connected to the output shaft of the motor, a first feed hole is arranged on the top of the kettle body, and a discharge hole is arranged on the bottom; characterized in that: The stirring shaft is provided with a first propulsion stirring blade, a turbine stirring blade and a second propulsion stirring blade in sequence from top to bottom.
2. A neutralization kettle for gallium purification according to claim 1, characterized in that: The second propulsion stirring blade is a spiral stirring blade.
3. A neutralization kettle for gallium purification according to claim 2, characterized in that: The top of the kettle body is also provided with a second feed hole.
4. A neutralization kettle for gallium purification according to claim 3, characterized in that: An observation window is also provided on the top of the kettle body.
5. A neutralization kettle for gallium purification according to claim 4, characterized in that: A sampling port is arranged at the observation window.
6. A neutralization kettle for purifying gallium according to any one of claims 3 to 5, characterized in that: The kettle body is provided with a mixing component, which is located directly above the first propulsion stirring blade. The mixing component includes a mixing disk and a plurality of guide vanes. A connecting cylinder is rotatably connected at the center of the mixing disk. The stirring shaft connecting the cylinder and the mixing disk are fixedly connected to the connecting cylinder and are coaxial. The outer wall of the connecting cylinder is provided with connecting ears of the same number as the guide vanes. The plurality of guide vanes are respectively hinged on the corresponding connecting ears, and a torsion spring is provided at the connection between the guide vane and the connecting ear. The guide vane is arc-shaped, and the inner wall of the guide vane is in contact with the outer wall of the connecting cylinder. The outer wall of the guide vane is in contact with the outer wall of the connecting cylinder under the action of the torsion spring. In contact with the inner wall of the mixing disk; a guide block is integrally formed on the inner wall of the mixing disk, and the side of the guide block facing the connecting tube is a progressive arc, and the width of the narrowest part of the guide block and the connecting tube is equal to or slightly greater than the thickness of the guide plate; a liquid inlet hole and a liquid outlet hole are provided on the mixing disk, the liquid outlet hole is located at the guide block, the liquid inlet hole is located on the side of the guide block, and the liquid inlet hole and the liquid outlet hole are located on both sides of the narrowest part of the guide block and the connecting tube; the liquid inlet hole is connected to a collecting pipe, the first feed hole and the second feed hole are both connected to the collecting pipe, and flow control valves are provided in the first feed hole and the second feed hole.
7. A neutralization kettle for gallium purification according to claim 6, characterized in that: The bottom of the mixing plate is provided with a plurality of blind holes, and stirring mechanisms are arranged in the blind holes.
8. A neutralization kettle for gallium purification according to claim 7, characterized in that: The stirring mechanism includes a stirring rod and a plurality of mixing blades fixedly connected to the top of the stirring rod, and the mixing blades and the stirring rod are both located in the blind hole; a cavity is provided in the bottom wall of the mixing disk, and a driving gear and a plurality of driven gears meshing with the driving gear are provided in the cavity, and the plurality of stirring rods are respectively fixedly connected to the plurality of driven gears, and the driving gear is fixedly connected to the stirring shaft.
9. A neutralization kettle for gallium purification according to claim 8, characterized in that: The radius of the driven gear is smaller than the radius of the driving gear.
10. A neutralization kettle for gallium purification according to claim 9, characterized in that: The liquid outlet is connected with a flow guide pipe, and the liquid outlet end of the flow guide pipe is close to the stirring shaft.