Coprecipitation reaction device and method for high-selectivity oxygen carrier containing high-purity selenium additive

Abstract

The invention relates to the technical field of oxygen carrier production, in particular to a coprecipitation reaction device and method for a high-selectivity oxygen carrier containing a high-purity selenium additive, the device comprises a rack, and a driving device is installed on the rear wall in the rack; the tank body is internally connected with the rack, and the upper end of the tank body is rotationally connected with a rotating shaft The plurality of large stirring blades are uniformly mounted at the outer end of the rotating shaft; the piston is in sliding connection with the interior of the tank body and rotationally connected to the outer end of the rotating shaft; the movable plate is in sliding connection with the interior of the tank body and is in sliding connection with the outer end of the rotating shaft; the outer rubber cylinder is mounted between the piston and the movable plate; the inner rubber cylinder is arranged between the piston and the movable plate; according to the design, the stock solution in the tank body is isolated, so that the probability of interference and the like on the coprecipitation reaction is effectively reduced, the stirring operation is buffered, the probability of obstruction and the like on stirring in the coprecipitation reaction is effectively reduced, and the coprecipitation reaction effect and the quality of the high-selectivity oxygen carrier are effectively ensured.

Description

Technical Field

[0001] The invention discloses a highly selective oxygen carrier coprecipitation reaction device and method containing a high-purity selenium additive, and belongs to the technical field of oxygen carrier production. Background Art

[0002] A highly selective oxygen carrier is a key material that has the ability to efficiently adsorb, bind and release oxygen under specific conditions. Its preparation often uses a co-precipitation reaction method. Usually, the preparation process of this material covers the following key steps: First, accurately weigh the metal salt raw materials, precipitants and additives, among which high-purity selenium additives can be used as additives. Next, the stock solution formed by mixing these raw materials is placed in a reaction vessel for sufficient stirring and heating. Under specific stirring rate and temperature conditions, the stock solution undergoes a co-precipitation reaction to generate a highly selective oxygen carrier precursor precipitate. Subsequently, the precipitate is subjected to subsequent treatments such as washing, drying and calcination in turn to finally obtain a highly selective oxygen carrier.

[0003] At present, the preparation process mostly relies on a reactor to provide a reaction space for the stock solution. In actual operation, a certain gap will be reserved above the stock solution in the reactor to ensure that the stock solution can be stably turbulent during the stirring operation during the reaction. However, during the stirring process, the high-purity selenium additive is in contact with the air, which makes the high-purity selenium additive easy to oxidize. The oxidation product is very likely to interfere with the co-precipitation reaction of the stock solution, reducing the reaction efficiency and product quality. To solve this problem, some processes choose to fill the gap in the reactor with inert gas. Although it can effectively reduce the oxidation phenomenon of high-purity selenium additives, it has caused new problems during the stirring and heating process: on the one hand, the inert gas is easy to form bubbles in the generated precipitate, affecting the structure and properties of the precipitate; on the other hand, the inert gas recovery is difficult, resulting in a serious waste of resources. The combined effect of these factors greatly affects the effect of the co-precipitation reaction and the final quality of the highly selective oxygen carrier. Summary of the invention

[0004] In view of the problems in the prior art, the present invention provides a highly selective oxygen carrier co-precipitation reaction device and method containing a high-purity selenium additive.

[0005] The technical solution adopted by the present invention to solve its technical problem is: A highly selective oxygen carrier coprecipitation reaction device containing a high-purity selenium additive comprises: A frame, wherein a driving device is installed on a rear wall inside the frame; A rotating shaft connected to an output shaft of a driving device; A tank body is connected to the frame, the upper end of the tank body is rotatably connected to a rotating shaft, and the rotating shaft extends into the tank body; Large stirring blades, with multiple large stirring blades provided. The multiple large stirring blades are evenly installed on the outer end of the rotating shaft, and the large stirring blades are located inside the tank; A piston, which is slidably connected inside the tank. The piston is rotatably connected to the outer end of the rotating shaft; A movable plate, which is slidably connected inside the tank. The movable plate is slidably connected to the outer end of the rotating shaft, and the movable plate is located below the piston; An outer rubber cylinder, which is in contact with the inner wall of the tank. The outer rubber cylinder is installed between the piston and the movable plate; An inner rubber cylinder, which is arranged between the piston and the movable plate, and the inner rubber cylinder is located outside the rotating shaft and inside the outer rubber cylinder; A first auxiliary part, which is connected to the upper end of the tank. The first auxiliary part is installed on the outer end of the rotating shaft. The lower end of the first auxiliary part passes through the tank, the piston and the movable plate, and the first auxiliary part is located above the large stirring blades; A second auxiliary part, which is connected to the lower end of the rotating shaft. The second auxiliary part is rotatably connected to the inner bottom end of the tank.

[0006] Further, the first auxiliary part includes a first gear. The first gear is arranged on the outer end of the rotating shaft, and the first gear is located at the upper end of the tank. A plurality of second gears are evenly meshed with the outer end of the first gear. Connection components are arranged in the middle of the lower ends of the plurality of second gears. The lower ends of the plurality of connection components pass through the tank, the piston and the movable plate. A plurality of small stirring blades are evenly installed on the outer ends of the plurality of connection components, and the small stirring blades are located below the movable plate. An annular plate is installed on the inner wall of the tank, and the annular plate is in contact with the lower end of the movable plate. The small stirring blades are located inside the annular plate.

[0007] Further, the connection component includes a connection shaft and a cylinder. The connection shaft is installed in the middle of the lower end of the second gear, and the lower end of the connection shaft passes through the tank. The connection shaft is rotatably connected to the tank. A block is installed at the lower end of the connection shaft, and the cross-section of the block is rectangular. The cylinder is rotatably connected to the lower end of the movable plate, and the upper end of the cylinder penetrates through the movable plate and the piston. The cylinder is slidably connected to the piston, and the cylinder is located between the outer rubber cylinder and the inner rubber cylinder. A groove is formed by downward depression on the upper end surface of the cylinder, and the cylinder is located above the large stirring blades. The block is slidably connected to the upper end of the groove, and the block extends into the groove. A plurality of small stirring blades are evenly installed on the outer end of the cylinder.

[0008] Further, the second auxiliary part includes a tapered column. The tapered column is installed at the lower end of the rotating shaft, and the tapered column is arranged with a narrow upper part and a wide lower part. The tapered column is rotatably connected to the inner bottom end of the tank. A plurality of special-shaped plates are evenly installed on the outer end of the lower part of the tapered column, and the special-shaped plates are in contact with the inner bottom surface of the tank. A plurality of connecting rods are evenly arranged on the outer end of the tapered column, and the other ends of the connecting rods are connected to the special-shaped plates.

[0009] Further, a plurality of discharge pipes are uniformly and communicatively arranged at the lower end of the tank body, and a first control valve is assembled on the discharge pipe. The connection position of the discharge pipe and the tank body is located outside the conical column. An exhaust pipe is communicatively installed at the outer end of the tank body, and a one-way valve is assembled on the exhaust pipe. The other end of the exhaust pipe is communicatively provided with a first hose. The other end of the first hose is communicatively installed with a first auxiliary pipe, and the first auxiliary pipe is located outside the cylinder. The other end of the first auxiliary pipe penetrates through the piston and the movable plate, and the first auxiliary pipe is slidably connected to the piston. The first auxiliary pipe is located between the outer rubber cylinder and the inner rubber cylinder.

[0010] Further, a plurality of feed pipes are communicatively installed at equal intervals at the outer end of the tank body, and a second control valve is assembled on the feed pipe. The other ends of the plurality of feed pipes are communicatively provided with second hoses. The other ends of the plurality of second hoses are communicatively installed with second auxiliary pipes, and the second auxiliary pipes are located outside the cylinder. The other ends of the second auxiliary pipes penetrate through the piston and the movable plate, and the second auxiliary pipes are slidably connected to the piston. The second auxiliary pipes are located between the outer rubber cylinder and the inner rubber cylinder; A plurality of feeders are installed at equal intervals inside the left side of the frame, and the plurality of feeders are arranged vertically. The plurality of feeders are respectively detachably and communicatively installed with the plurality of feed pipes. A pipeline is inlaid and installed inside the cylindrical part of the tank body, and the pipeline is in a spiral state. A heater is arranged inside the left side of the frame, and the heater is located below the feeder. The outlet part of the heater is communicatively arranged with the inlet part of the pipeline, and the inlet part of the heater is communicatively arranged with the outlet part of the pipeline. A controller is installed inside the right side of the frame, and the controller is electrically connected to the plurality of feeders, the heater, the plurality of first control valves, the plurality of second control valves, and the driving device respectively.

[0011] A high-selectivity oxygen carrier co-precipitation reaction method containing a high-purity selenium additive includes the following steps: The first step is feeding. Through the controller, the plurality of feeders, and the plurality of second control valves, the metal salt solution, the high-purity selenium additive, and the precipitant are slowly added into the tank body along the corresponding feed pipes, second hoses, and second auxiliary pipes according to a set ratio. At this time, the gas in the space below the movable plate in the tank body is discharged outward through the first auxiliary pipe, the first hose, and the exhaust pipe, and the original liquid level in the tank body is made to fit the lower end surface of the movable plate; The second step is reaction. The driving device is used to drive the rotation shaft and the plurality of large stirring blades to rotate, so as to stir the original liquid in the tank body. At the same time, the heater and the pipeline are used to heat the original liquid in the tank body, so as to adjust the temperature of the original liquid and maintain it at a set temperature. At this temperature, the metal salt solution, the high-purity selenium additive, and the precipitant undergo a co-precipitation reaction, thereby forming a high-selectivity oxygen carrier precursor precipitate; The third step is aging. After the reaction is completed, the stirring operation is stopped, and the precipitate is allowed to stand and age, so that the precipitate grows and perfects the crystal structure; Step 4. Post-treatment: After aging is completed, the precipitate and residual liquid mixture in the tank are discharged through multiple discharge pipes, and then the discharged mixture is subjected to solid-liquid separation treatment. Next, the separated precipitate is washed multiple times, and then the washed precipitate is dried. Subsequently, the dried precipitate is calcined to form a highly selective oxygen carrier. Then, performance tests such as chemical composition analysis, crystal structure analysis, and oxygen-carrying capacity test are carried out on the highly selective oxygen carrier, and the qualified highly selective oxygen carrier is packaged and stored in the warehouse.

[0012] Advantages of the present invention: The stock solution in the tank and air are isolated by the piston and the movable plate, effectively reducing the probability of interference with the coprecipitation reaction due to factors such as oxidation of the high-purity selenium additive, etc., and reducing resource waste. The coprecipitation reaction effect and the quality of the highly selective oxygen carrier are effectively ensured. An outer rubber cylinder and an inner rubber cylinder are installed between the piston and the movable plate, and the outer rubber cylinder and the inner rubber cylinder are flexible and elastic. During the stirring process, the movable plate will move up and down cyclically as the stock solution in the tank is stirred, thereby providing space to buffer the stirring operation of the stock solution in the tank, achieving effective stirring of the stock solution in the tank, effectively reducing the probability of hindrance to the stirring in the coprecipitation reaction, and effectively ensuring the coprecipitation reaction effect and the quality of the highly selective oxygen carrier. Description of the drawings

[0013] By reading the following detailed description of the non-restrictive embodiments with reference to the accompanying drawings, other features, objectives, and advantages of the present invention will become more apparent: Figure 1 It is a schematic structural diagram of the coprecipitation reaction device of the highly selective oxygen carrier containing high-purity selenium additive of the present invention; Figure 2 It is a sectional view of the coprecipitation reaction device of the highly selective oxygen carrier containing high-purity selenium additive of the present invention; Figure 3 For Figure 2 The enlarged view of part A in Figure 4 It is an assembly drawing of the piston, outer rubber cylinder, and movable plate in the coprecipitation reaction device of the highly selective oxygen carrier containing high-purity selenium additive of the present invention; Figure 5 It is an assembly drawing of the outer rubber cylinder, movable plate, and inner rubber cylinder in the coprecipitation reaction device of the highly selective oxygen carrier containing high-purity selenium additive of the present invention; Figure 6 It is an assembly drawing of the second gear, connecting shaft, and block in the coprecipitation reaction device of the highly selective oxygen carrier containing high-purity selenium additive of the present invention; Figure 7 It is an assembly drawing of the block, small stirring blade, and cylinder in the coprecipitation reaction device of the highly selective oxygen carrier containing high-purity selenium additive of the present invention; Figure 8 Schematic diagram of another embodiment of the high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to the present invention; Figure 9 is Figure 8 a cross-sectional view of; Figure 10 is Figure 9 an enlarged view of part B in; Figure 11 3D view of the outer shell in the high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to the present invention.

[0014] In the figure: 1, frame, 11, controller, 12, discharge pipe, 13, heater, 14, feeder, 2, motor, 3, rotating shaft, 31, first gear, 32, large stirring blade, 33, connecting rod, 34, special-shaped plate, 35, conical column; 4, tank body, 41, second gear, 42, connecting shaft, 421, cover plate, 422, outer shell, 423, annular gear, 424, drain pipe, 425, screw rod, 426, third gear, 427, filter screen barrel, 428, auxiliary shaft, 4281, positioning block, 4282, magnet, 43, clamping block, 44, clamping groove, 45, small stirring blade, 46, cylinder, 47, exhaust pipe, 48, annular plate; 5, piston, 6, outer rubber cylinder, 7, movable plate, 8, inner rubber cylinder. Specific embodiments

[0015] In order to make the technical means, creative features, achieved purposes and effects of the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.

[0016] Embodiment 1: As Figures 1 - 5 shown, a high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive is provided, including: a frame 1, the fixed part of the driving device connecting the output shaft to the rotating shaft 3 is installed on the inner rear wall of the frame 1, the rotating shaft 3 is driven to rotate through the driving device, the driving device can adopt a motor 2, and the tank body 4 is arranged in the frame 1, through the tank body 4, a reaction space is provided for the co-precipitation reaction operation, and then the rotating shaft 3 extending into the tank body 4 is rotatably connected to the upper end of the tank body 4, through the rotating shaft 3, components such as the large stirring blade 32 are rotated, and a plurality of large stirring blades 32 located in the tank body 4 are evenly installed on the outer end of the rotating shaft 3, and the plurality of large stirring blades 32 are used in cooperation for stirring operations; The piston 5 that is slidably connected inside the tank body 4 is rotatably connected to the outer end of the rotating shaft 3. Through the piston 5, two sealed spaces are separated inside the tank body 4. And the movable plate 7 that is slidably connected inside the tank body 4 and is located below the piston 5 is slidably connected to the outer end of the rotating shaft 3. Through the movable plate 7, the stock solution inside the tank body 4 is isolated from the air. Then the outer rubber cylinder 6 that fits on the inner wall of the tank body 4 is installed between the piston 5 and the movable plate 7. Through the outer rubber cylinder 6, a sealed connection is formed between the movable plate 7 and the tank body 4. And the inner rubber cylinder 8 that is located outside the rotating shaft 3 and inside the outer rubber cylinder 6 is arranged between the piston 5 and the movable plate 7. The outer rubber cylinder 6 and the inner rubber cylinder 8 are used in cooperation to enable the movable plate 7 to move up and down; A plurality of discharge pipes 12 whose communication positions with the tank body 4 are located outside the conical column 35 are uniformly and communicatively arranged at the lower end of the tank body 4. And a first control valve is assembled on the discharge pipe 12. The plurality of discharge pipes 12 are used in cooperation to enable the mixture after reaction inside the tank body 4 to be discharged. And the exhaust pipe 47 is communicatively installed at the outer end of the tank body 4. And a one-way valve is assembled on the exhaust pipe 47. The exhaust pipe 47 and the one-way valve are used in cooperation to enable the air to flow unidirectionally. Then a first hose is communicatively arranged at the other end of the exhaust pipe 47. Through the first hose, the exhaust pipe 47 and the first auxiliary pipe are communicatively arranged, and the first auxiliary pipe can move up and down. And the first auxiliary pipe that is located outside the cylinder 46 and the other end of which penetrates through the piston 5 and the movable plate 7 is communicatively installed at the other end of the first hose. And the first auxiliary pipe that is located between the outer rubber cylinder 6 and the inner rubber cylinder 8 is slidably connected to the piston 5. The first auxiliary pipe, the first hose and the exhaust pipe 47 enable the air inside the space below the movable plate 7 inside the tank body 4 to be discharged; A plurality of feed pipes whose other ends are communicatively connected to second hoses are equidistantly and communicatively installed at the outer end of the tank body 4. And a second control valve is assembled on the feed pipe. Through the feed pipe, the second hose and the feeder 14 are communicatively connected. And a plurality of second auxiliary pipes that are located outside the cylinder 46 are respectively communicatively installed at the other ends of the plurality of second hoses. Through the second hose, the second auxiliary pipe and the corresponding feed pipe are communicatively connected. Then the second auxiliary pipe that is located between the outer rubber cylinder 6 and the inner rubber cylinder 8 and the other end of which penetrates through the piston 5 and the movable plate 7 is slidably connected to the piston 5. The second auxiliary pipe, the second hose and the feed pipe are used in cooperation to perform the feeding operation into the tank body 4. And a plurality of feeders 14 arranged vertically are equidistantly installed inside the left side of the frame 1. And the plurality of feeders 14 are respectively detachably and communicatively installed with the plurality of feed pipes. Through the feeder 14, raw materials are conveyed into the feed pipe; The spirally-shaped pipe is inlaid and installed inside the cylindrical part of the tank body 4. Through the pipe, a flow channel is provided for the medium with heat, and the heater 13 located below the feeder 14 is arranged inside the left side of the frame 1. The outlet part of the heater 13 is communicated with the inlet part of the pipe, and the inlet part of the heater 13 is communicated with the outlet part of the pipe. Through the heater 13, the medium with heat is conveyed into the pipe. Then, the controller 11, which is electrically connected to the plurality of feeders 14, heaters 13, a plurality of first control valves, a plurality of second control valves, and the driving device respectively, is installed inside the right side of the frame 1. Through the controller 11, the opening and closing of electronic devices such as the heater 13 are controlled.

[0017] During use, the controller 11 starts the plurality of feeders 14 in sequence according to the pre-designed sequence. When the feeder 14 works, the raw materials enter the space below the movable plate 7 inside the tank body 4 along the corresponding feed pipes, second hoses, and second auxiliary pipes, so that the metal salt solution, high-purity selenium additive, and precipitant are slowly added into the tank body 4 at a set ratio. At this time, the gas in the space below the movable plate 7 inside the tank body 4 is discharged outwards through the first auxiliary pipe, first hose, and exhaust pipe 47, and the original liquid level inside the tank body 4 fits the lower end face of the movable plate 7, realizing the isolation of the original liquid inside the tank body 4 from the air, effectively reducing the probability of interference with the coprecipitation reaction due to factors such as oxidation of the high-purity selenium additive, etc., and reducing resource waste, effectively ensuring the coprecipitation reaction effect and the quality of the high-selectivity oxygen carrier. Then, the heater 13 and the motor 2 are started in sequence by control. When the heater 13 works, it conveys the medium with heat into the pipe and makes the medium flow in the pipe, thereby heating the original liquid inside the tank body 4, adjusting the temperature of the original liquid and maintaining it at the set temperature. When the motor 2 works, it drives the rotating shaft 3 to rotate, thereby driving the plurality of large stirring blades 32 to rotate, thereby stirring the original liquid. Under the conditions of temperature and stirring, the metal salt solution, high-purity selenium additive, and precipitant inside the tank body 4 undergo a coprecipitation reaction, thereby forming a high-selectivity oxygen carrier precursor precipitate. Since the outer rubber cylinder 6 and the inner rubber cylinder 8 are flexible and elastic in themselves, during the stirring process, the movable plate 7 will move up and down cyclically with the agitation of the original liquid inside the tank body 4 with the assistance of the outer rubber cylinder 6 and the inner rubber cylinder 8, thereby providing space to buffer the agitation operation of the original liquid inside the tank body 4, realizing effective stirring of the original liquid inside the tank body 4, effectively reducing the probability of obstacles to the stirring in the coprecipitation reaction, and effectively ensuring the coprecipitation reaction effect and the quality of the high-selectivity oxygen carrier. After the reaction is completed, stop the stirring and heating operations, let the precipitate undergo a static aging operation to allow the precipitate to grow and perfect its crystal structure, then open the first control valves on the multiple discharge pipes 12, so that the precipitate and the residual liquid mixture in the tank body 4 are discharged through the multiple discharge pipes 12, then perform a solid-liquid separation treatment on the discharged mixture, then perform multiple washing treatments on the separated precipitate, then dry the washed precipitate, and then perform a calcination treatment on the dried precipitate to form a highly selective oxygen carrier, thus completing the production of the highly selective oxygen carrier.

[0018] Example 2: In the preparation process of the highly selective oxygen carrier, first, drive the large stirring blade 32 to rotate by means of the motor 2 and the rotating shaft 3, and carry out a stirring operation on the stock solution composed of the metal salt solution, the high-purity selenium additive, and the precipitant configured in the tank body 4 in a set ratio. At the same time, use the heater 13 and the pipeline to heat the stock solution. Under suitable temperature conditions and continuous stirring, a coprecipitation reaction occurs among the metal salt solution, the high-purity selenium additive, and the precipitant in the tank body 4, thereby forming a precipitate of the highly selective oxygen carrier precursor.

[0019] To ensure the smooth progress of the reaction, use the piston 5 and the movable plate 7 to effectively isolate the stock solution and the stock solution and air in the tank body 4. This measure can greatly reduce the possibility of interfering with the coprecipitation reaction due to factors such as the oxidation of the high-purity selenium additive. In addition, install an outer rubber cylinder 6 and an inner rubber cylinder 8 between the piston 5 and the movable plate 7. In this way, the movable plate 7 can perform an up-and-down cyclic movement during the stirring process, providing a buffer space for the agitation of the stock solution in the tank body 4, so as to stir the stock solution more effectively.

[0020] However, the isolation treatment method of the stock solution in the tank body 4 also brings new problems. This treatment makes it easy to have insufficient stirring in the upper and lower regions of the stock solution in the tank body 4, resulting in an uneven flow field. And the uneven flow field significantly increases the probability of hindering the coprecipitation reaction, affecting the production efficiency and quality of the final product.

[0021] To solve the above problems, as Figures 1 - 7 shown, arrange the first gear 31 located at the upper end of the tank body 4 at the outer end of the rotating shaft 3. Through the first gear 31, make multiple second gears 41 rotate synchronously, and equally space and engage the multiple second gears 41 at the outer end of the first gear 31. Through the second gear 41, make the connecting shaft 42 rotate. Then install the annular plate 48 attached to the lower end of the movable plate 7 on the inner wall of the tank body 4. Through the annular plate 48, limit the installation of the annular plate 48, and respectively install the multiple connecting shafts 42 passing through the tank body 4 at the lower end and rotatably connected to the tank body 4 at the middle part of the lower end of the second gear 41. Through the connecting shaft 42, provide an installation carrier for components such as the block 43; A plurality of cylinders 46 that penetrate through the upper end of the movable plate 7 and the piston 5 and are slidably connected to the piston 5 are rotatably connected to the lower end of the movable plate 7, and the cylinders 46 are located between the outer rubber cylinder 6 and the inner rubber cylinder 8. Through the cylinders 46, an installation carrier is provided for the small stirring blades 45. On the upper end surfaces of the plurality of cylinders 46 located above the large stirring blades 32, grooves 44 are formed by downward depressions. Through the grooves 44, an installation space is provided for the clamping blocks 43. A plurality of clamping blocks 43 with rectangular cross-sections are respectively installed on the lower ends of the plurality of connecting shafts 42, and the plurality of clamping blocks 43 extending into the grooves 44 are respectively slidably connected to the upper ends of the plurality of grooves 44. The clamping blocks 43 and the grooves 44 are used in cooperation to enable the cylinders 46 and the connecting shafts 42 to rotate synchronously, and relative up-and-down movement occurs between the cylinders 46 and the connecting shafts 42. Then, a plurality of small stirring blades 45 located below the movable plate 7 and inside the annular plate 48 are equidistantly installed on the outer ends of the cylinders 46. The plurality of small stirring blades 45 are used in cooperation to perform auxiliary stirring on the surface of the stock solution in the tank body 4. The conical column 35, which is arranged with a narrow upper part and a wide lower part and is rotatably connected to the inner bottom end of the tank body 4, is installed on the lower end of the rotating shaft 3. Through the conical column 35, an installation carrier is provided for components such as the special-shaped plate 34. A plurality of special-shaped plates 34 that are attached to the inner bottom end surface of the tank body 4 are equidistantly installed on the outer lower ends of the conical column 35. The plurality of special-shaped plates 34 are used in cooperation to perform stirring in the inner bottom space of the tank body 4. Then, a plurality of connecting rods 33 with the other ends connected to the special-shaped plates 34 are uniformly arranged on the outer end of the conical column 35. Through the connecting rods 33, the installation strength of the special-shaped plates 34 is increased.

[0022] During use, first, through a plurality of feeders 14, a plurality of feed pipes, a plurality of second hoses, and a plurality of second auxiliary pipes, the metal salt solution, the high-purity selenium additive, and the precipitant are slowly added into the tank body 4 in a set ratio. Then, through the heater 13 and the pipeline, the stock solution in the tank body 4 is heated, so as to adjust the temperature of the stock solution and maintain it at a set temperature. At the same time, the motor 2 is used to drive the rotating shaft 3 and a plurality of large stirring blades 32 to rotate, so as to stir the stock solution. Under the conditions of temperature and stirring, the metal salt solution, the high-purity selenium additive, and the precipitant in the tank body 4 undergo a coprecipitation reaction, thereby forming a high-selectivity oxygen carrier precursor precipitate. During the rotation of the rotating shaft 3, the first gear 31 will rotate. Since the first gear 31 meshes with multiple second gears 41, the rotation of the first gear 31 will cause the multiple second gears 41 to rotate synchronously, and then cause the multiple connecting shafts 42 to rotate synchronously. With the assistance of multiple clamping blocks 43 and multiple clamping grooves 44, the multiple cylinders 46 will rotate synchronously, and then the multiple small stirring blades 45 will rotate synchronously, so as to perform auxiliary stirring in the space between the movable plate 7 and the large stirring blade 32. At the same time, the rotation of the rotating shaft 3 will cause the conical column 35 to rotate, and then cause the multiple special-shaped plates 34 to rotate, so as to perform auxiliary stirring in the space between the large stirring blade 32 and the inner bottom end of the tank body 4, realizing the auxiliary stirring of the stock solution in the tank body 4, effectively reducing the probability of uneven stirring flow field in the upper and lower regions of the stock solution in the tank body 4 due to factors such as isolation, effectively reducing the probability of hindering the coprecipitation reaction, and effectively ensuring the coprecipitation reaction effect and the quality of the highly selective oxygen carrier; After the reaction is completed, stop the stirring and heating operations, let the precipitate carry out the static aging operation to make the precipitate grow and perfect the crystal structure, then open the first control valves on the multiple discharge pipes 12, so that the precipitate and residual liquid mixture in the tank body 4 are discharged through the multiple discharge pipes 12, then perform solid-liquid separation on the discharged mixture, then perform multiple washing operations on the separated precipitate, then dry the washed precipitate, and then perform roasting treatment on the dried precipitate to form a highly selective oxygen carrier, thus completing the production of the highly selective oxygen carrier.

[0023] Example 3: During the preparation of the highly selective oxygen carrier, the motor 2 and the rotating shaft 3 drive the large stirring blade 32 to rotate, so as to fully stir the stock solution composed of the metal salt solution, high-purity selenium additive and precipitant mixed in a set ratio in the tank body 4. At the same time, use the heater 13 and the pipeline to heat the stock solution. Under the synergistic action of a specific temperature and continuous stirring, the metal salt solution, high-purity selenium additive and precipitant in the tank body 4 undergo a coprecipitation reaction, and then a highly selective oxygen carrier precursor precipitate is generated. Subsequently, the mixture of the precipitate and the residual liquid in the tank body 4 is discharged through the discharge pipe 12.

[0024] However, there are some drawbacks in this process. On the one hand, the precipitate is extremely easy to remain at the bottom of the tank body 4 and is difficult to be completely drained; on the other hand, the discharged mixture needs to be separated subsequently. To ensure the separation effect, the separated precipitate also needs to be dehydrated. These additional steps not only greatly increase the equipment cost, but also prolong the working time, resulting in low working efficiency and having an adverse impact on the overall production process.

[0025] To solve the above problems, as Figures 8 - 11As shown, a magnet is embedded at the lower end of the conical column 35, and a magnet 4282 that is attracted to the magnet and located directly below the magnet is attached to the middle of the lower end of the tank body 4. The magnet 4282 is located inside multiple discharge pipes 12. The magnet and the magnet 4282 are used in cooperation to enable the rotating shaft 3 and the auxiliary shaft 428 to rotate synchronously. Then, the auxiliary shaft 428 is installed at the middle position of the lower end of the magnet 4282. Through the auxiliary shaft 428, the filter screen barrel 427 is rotated, and the cover plate 421 is rotatably connected to the outer end of the auxiliary shaft 428. The lower ends of multiple discharge pipes 12 all penetrate through the cover plate 421. Through the cover plate 421, an installation carrier is provided for the outer shell 422. The outer shell 422 with a T-shaped cross-section is attached to the lower end of the cover plate 421. Through the outer shell 422, an installation carrier is provided for components such as the filter screen barrel 427. The filter screen barrel 427 attached to the lower end of the cover plate 421 is rotatably connected to the inner wall of the outer shell 422. Multiple discharge pipes 12 are all located inside the filter screen barrel 427. Through the filter screen barrel 427, the mixture after the reaction in the tank body 4 is filtered. A square hole is recessed upward on the lower end surface of the auxiliary shaft 428. Through the square hole, an installation space is provided for the positioning block 4281. Then, the positioning block 4281 located in the square hole is installed on the inner bottom end of the filter screen barrel 427. The square hole and the positioning block 4281 are used in cooperation to enable the filter screen barrel 427 and the auxiliary shaft 428 to rotate synchronously. A drain pipe 424 with a valve is connected and installed at the lower end of the outer shell 422. Through the drain pipe 424, the liquid separated inside the outer shell 422 is discharged. The annular gear 423 is rotatably connected to the lower end of the horizontal part of the outer shell 422. Through the annular gear 423, multiple third gears 426 rotate synchronously. Multiple third gears 426 located outside the vertical part of the outer shell 422 are equidistantly meshed on the inner wall of the annular gear 423. Through the third gears 426, the screw 425 rotates. Multiple threaded holes penetrating through the cover plate 421 are recessed upward on the lower end surface of the cover plate 421. Through the threaded holes, an installation space is provided for the screw 425. Then, multiple screws 425 that penetrate through the horizontal part of the outer shell 422 and are rotatably connected to the outer shell 422 are respectively arranged on the upper ends of multiple third gears 426. Multiple screws 425 are respectively threadedly connected to multiple threaded holes. The multiple screws 425 and the multiple threaded holes are used in cooperation to enable the cover plate 421 and the outer shell 422 to be detachably connected.

[0026] In use, first, through multiple feeders 14, multiple feed pipes, multiple second hoses, and multiple second auxiliary pipes, the metal salt solution, high-purity selenium additive, and precipitant are slowly added into the tank body 4 in a set ratio. Then, through the heater 13 and the pipeline, the stock solution in the tank body 4 is heated, so as to adjust the temperature of the stock solution and maintain it at a set temperature. At the same time, the motor 2 is used to drive the rotating shaft 3 and multiple large stirring blades 32 to rotate, so as to stir the stock solution. Under the conditions of temperature and stirring, the metal salt solution, high-purity selenium additive, and precipitant in the tank body 4 undergo a coprecipitation reaction, thereby forming a high-selectivity oxygen carrier precursor precipitate; After the reaction is completed, stop the stirring and heating operations, and let the precipitate carry out a static aging operation to make the precipitate grow and improve the crystal structure. Then, open the first control valve on the multiple discharge pipes 12, so that the precipitate and residual liquid mixture in the tank body 4 are transported to the filter screen barrel 427 through the multiple discharge pipes 12. The filter screen barrel 427 will filter the mixture, and then carry out a solid-liquid separation treatment on the mixture. Then, start the motor 2, so that the rotating shaft 3 rotates, and the conical column 35 rotates, and then the multiple special-shaped plates 34 rotate along the inner bottom end surface of the tank body 4, so as to push the mixture remaining on the inner bottom end of the tank body 4 to the opening position of the discharge pipe 12 for assisting the discharging operation; At the same time, the rotation of the conical column 35 will cause the magnet to rotate. Because the magnet and the magnet 4282 are arranged to adsorb each other, the rotation of the magnet will cause the magnet 4282 to rotate at the same time, and then cause the auxiliary shaft 428 to rotate. With the assistance of the square hole and the positioning block 4281, the filter screen barrel 427 rotates, realizing the direct dehydration operation on the precipitate in the filter screen barrel 427, achieving the linkage between the dehydration operation and the stirring operation, effectively reducing the equipment cost and working time, and having high working efficiency; Then rotate the ring gear 423. Because the ring gear 423 meshes with multiple third gears 426, the rotation of the ring gear 423 will cause the multiple third gears 426 to rotate synchronously, and then cause the multiple screws 425 to rotate. Also, because the screw 425 is threadedly connected to the threaded hole, the rotation of the screw 425 will cause the screw 425 to move downward along the threaded hole at the same time, so that the screw 425 is separated from the threaded hole, and then the cover plate 421 and the outer shell 422 are disassembled. Then, transfer components such as the outer shell 422 and the filter screen barrel 427 to the next station, and then carry out multiple washing treatments on the dehydrated precipitate in the filter screen barrel 427. Then, take out the washed precipitate and carry out a drying treatment, and then carry out a roasting treatment on the dried precipitate to form a high-selectivity oxygen carrier, and then complete the production of the high-selectivity oxygen carrier.

[0027] A method for coprecipitation reaction of a high-selectivity oxygen carrier containing a high-purity selenium additive includes the following steps: Step 1: Feeding. Through the controller 11, multiple feeders 14, and multiple second control valves, the metal salt solution, high-purity selenium additive, and precipitant are slowly added into the tank body 4 at a set ratio along the corresponding feed pipes, second hoses, and second auxiliary pipes respectively. At this time, the gas in the space below the movable plate 7 in the tank body 4 is discharged outward through the first auxiliary pipe, first hose, and exhaust pipe 47, and the original liquid level in the tank body 4 is made to fit the lower end surface of the movable plate 7; Step 2: Reaction. The rotating shaft 3 and multiple large stirring blades 32 are driven to rotate by the driving device, so as to stir the original liquid in the tank body 4. At the same time, the original liquid in the tank body 4 is heated by the heater 13 and the pipeline, so as to adjust the temperature of the original liquid and maintain it at the set temperature. At this temperature, the metal salt solution, high-purity selenium additive, and precipitant undergo a coprecipitation reaction, thereby forming a high-selectivity oxygen carrier precursor precipitate; Step 3: Aging. After the reaction is completed, the stirring operation is stopped, and the precipitate is allowed to stand for aging, so that the precipitate grows and perfects its crystal structure; Step 4: Post-treatment. After aging is completed, the precipitate and residual liquid mixture in the tank body 4 are discharged through multiple discharge pipes 12, and then the discharged mixture is subjected to solid-liquid separation treatment. Then, the separated precipitate is washed multiple times, and then the washed precipitate is dried. Then, the dried precipitate is calcined to form a high-selectivity oxygen carrier. Then, performance tests such as chemical composition analysis, crystal structure analysis, and oxygen-carrying capacity test are carried out on the high-selectivity oxygen carrier, and the qualified high-selectivity oxygen carriers are packaged and stored in the warehouse.

[0028] Although this specification is described according to the embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive, characterized in that, Comprising: A frame (1), with a driving device installed on the inner rear wall of the frame (1); A rotating shaft (3), connected to the output shaft of the driving device; A tank body (4), connected inside the frame (1), with the upper end of the tank body (4) rotatably connected to the rotating shaft (3), and the rotating shaft (3) extending into the tank body (4); Large stirring blades (32), with a plurality of the large stirring blades (32) evenly installed on the outer end of the rotating shaft (3), and the large stirring blades (32) being located inside the tank body (4); A piston (5), slidably connected inside the tank body (4), and the piston (5) is rotatably connected to the outer end of the rotating shaft (3); A movable plate (7), slidably connected inside the tank body (4), the movable plate (7) is slidably connected to the outer end of the rotating shaft (3), and the movable plate (7) is located below the piston (5); An outer rubber cylinder (6), fitting against the inner wall of the tank body (4), and the outer rubber cylinder (6) is installed between the piston (5) and the movable plate (7); An inner rubber cylinder (8), the inner rubber cylinder (8) is arranged between the piston (5) and the movable plate (7), and the inner rubber cylinder (8) is located outside the rotating shaft (3) and inside the outer rubber cylinder (6); A first auxiliary part, connected to the upper end of the tank body (4), the first auxiliary part is installed on the outer end of the rotating shaft (3), the lower end of the first auxiliary part passes through the tank body (4), the piston (5) and the movable plate (7), and the first auxiliary part is located above the large stirring blades (32); A second auxiliary part, connected to the lower end of the rotating shaft (3), and the second auxiliary part is rotatably connected to the inner bottom end of the tank body (4).

2. The high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to claim 1, characterized in that: The first auxiliary part includes a first gear (31), the first gear (31) is arranged on the outer end of the rotating shaft (3), and the first gear (31) is located at the upper end of the tank body (4). A plurality of second gears (41) are evenly meshed with the outer end of the first gear (31). Connection components are arranged in the middle of the lower ends of the plurality of second gears (41). The lower ends of the plurality of connection components pass through the tank body (4), the piston (5) and the movable plate (7). A plurality of small stirring blades (45) are evenly installed on the outer ends of the plurality of connection components, and the small stirring blades (45) are located below the movable plate (7). An annular plate (48) is installed on the inner wall of the tank body (4), and the annular plate (48) fits against the lower end of the movable plate (7). The small stirring blades (45) are located inside the annular plate (48).

3. The high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to claim 2, wherein: The connecting component includes a connecting shaft (42) and a cylinder (46). The connecting shaft (42) is installed at the middle of the lower end of the second gear (41), and the lower end of the connecting shaft (42) passes through the tank body (4). The connecting shaft (42) is rotatably connected to the tank body (4). A clamping block (43) is installed at the lower end of the connecting shaft (42), and the cross-section of the clamping block (43) is rectangular. The cylinder (46) is rotatably connected to the lower end of the movable plate (7), and the upper end of the movable plate (7) penetrates through the movable plate (7) and the piston (5). The cylinder (46) is slidably connected to the piston (5), and the cylinder (46) is located between the outer rubber cylinder (6) and the inner rubber cylinder (8). A clamping groove (44) is formed by downward depression on the upper end surface of the cylinder (46), and the cylinder (46) is located above the large stirring blade (32). The clamping block (43) is slidably connected to the upper end of the clamping groove (44), and the clamping block (43) extends into the clamping groove (44). Small stirring blades (45) are equidistantly installed on the outer end of the cylinder (46).

4. The high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to claim 3, characterized in that: The second auxiliary part includes a tapered column (35). The tapered column (35) is installed at the lower end of the rotating shaft (3), and the tapered column (35) is arranged with a narrower upper part and a wider lower part. The tapered column (35) is rotatably connected to the inner bottom end of the tank body (4). A plurality of special-shaped plates (34) are equidistantly installed on the outer end of the lower part of the tapered column (35), and the special-shaped plates (34) are attached to the inner bottom end surface of the tank body (4). A plurality of connecting rods (33) are uniformly arranged on the outer end of the tapered column (35), and the other ends of the connecting rods (33) are connected to the special-shaped plates (34).

5. The high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to claim 4, characterized in that: A plurality of discharge pipes (12) are uniformly and communicatively arranged at the lower end of the tank body (4), and a first control valve is assembled on the discharge pipes (12). The communicating position between the discharge pipes (12) and the tank body (4) is located outside the tapered column (35). An exhaust pipe (47) is communicatively installed at the outer end of the tank body (4), and a check valve is assembled on the exhaust pipe (47). A first hose is communicatively arranged at the other end of the exhaust pipe (47). A first auxiliary pipe is communicatively installed at the other end of the first hose, and the first auxiliary pipe is located outside the cylinder (46). The other end of the first auxiliary pipe penetrates through the piston (5) and the movable plate (7), and the first auxiliary pipe is slidably connected to the piston (5). The first auxiliary pipe is located between the outer rubber cylinder (6) and the inner rubber cylinder (8).

6. The high-selectivity oxygen carrier co-precipitation reaction device containing a high-purity selenium additive according to claim 5, wherein: A plurality of feed pipes are communicatively installed at equal intervals at the outer end of the tank body (4), and a second control valve is assembled on the feed pipes. The other ends of the plurality of feed pipes are all communicatively provided with second hoses. A second auxiliary pipe is communicatively installed at the other ends of the plurality of second hoses, and the second auxiliary pipe is located outside the cylinder (46). The other end of the second auxiliary pipe penetrates through the piston (5) and the movable plate (7), and the second auxiliary pipe is slidably connected to the piston (5). The second auxiliary pipe is located between the outer rubber cylinder (6) and the inner rubber cylinder (8); On the left side inside the frame (1), a plurality of feeders (14) are equidistantly installed, and the plurality of feeders (14) are arranged vertically. The plurality of feeders (14) are respectively detachably connected and installed with a plurality of feed pipes. A pipeline is inlaid and installed inside the cylindrical part of the tank body (4), and the pipeline is in a spiral state. A heater (13) is arranged inside the left side of the frame (1), and the heater (13) is located below the feeder (14). The outlet part of the heater (13) is communicated with the inlet part of the pipeline, and the inlet part of the heater (13) is communicated with the outlet part of the pipeline. A controller (11) is installed inside the right side of the frame (1), and the controller (11) is electrically connected to the plurality of feeders (14), the heater (13), a plurality of first control valves, a plurality of second control valves, and the driving device respectively.

7. A co-precipitation reaction method of a highly selective oxygen carrier containing a high-purity selenium additive, applying the co-precipitation reaction device of the highly selective oxygen carrier containing a high-purity selenium additive described in claim 6, characterized in that, It includes the following steps: The first step, feeding: Through the controller (11), the plurality of feeders (14), and the plurality of second control valves, the metal salt solution, the high-purity selenium additive, and the precipitant are slowly added into the tank body (4) along the corresponding feed pipes, the second hoses, and the second auxiliary pipes according to a set ratio. At this time, the gas in the space below the movable plate (7) inside the tank body (4) is discharged outward through the first auxiliary pipe, the first hose, and the exhaust pipe (47), and the original liquid level inside the tank body (4) is made to fit the lower end surface of the movable plate (7). The second step, reaction: The driving device is used to drive the rotation of the rotating shaft (3) and the plurality of large stirring blades (32), so as to stir the original liquid inside the tank body (4). At the same time, the heater (13) and the pipeline are used to heat-treat the original liquid inside the tank body (4), so as to adjust the temperature of the original liquid and maintain it at a set temperature. At this temperature, the metal salt solution, the high-purity selenium additive, and the precipitant undergo a coprecipitation reaction, thereby forming a highly selective oxygen carrier precursor precipitate. The third step, aging: After the reaction is completed, the stirring operation is stopped, and the precipitate is allowed to stand and age, so that the precipitate grows and perfects the crystal structure. The fourth step, post-treatment: After the aging is completed, the precipitate and the residual liquid mixture inside the tank body (4) are discharged through the plurality of discharge pipes (12), and then the discharged mixture is subjected to solid-liquid separation treatment. Then, the separated precipitate is subjected to multiple washing treatments, and then the washed precipitate is dried. Then, the dried precipitate is subjected to a calcination treatment to form a highly selective oxygen carrier. Then, performance tests such as chemical composition analysis, crystal structure analysis, and oxygen-carrying capacity test are carried out on the highly selective oxygen carrier, and the qualified highly selective oxygen carrier is packaged and stored in the warehouse.

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