Temperature-controllable oxidation reaction device for preparing battery-grade iron oxide red seed

Abstract

The present application relates to the technical field of seed preparation, in particular to a controllable temperature oxidation reaction device for battery-grade red iron oxide seed preparation, comprising a reaction tank, support legs are fixed at the bottom of the reaction tank, a feed pipe is fixed through the top of the reaction tank, the first temperature control mechanism comprises a heat preservation cover fixed with the outer wall of the reaction tank, a second water guide pipe and an annular water spraying pipe are arranged on the inner wall of the heat preservation cover, and a first water tank is fixed at the bottom of the outer wall of the heat preservation cover; through the synergistic effect of the first temperature control mechanism and the second temperature control mechanism, the temperature in the reaction tank is accurately controlled, the first temperature control mechanism sprays water uniformly to the outer wall of the reaction tank through multiple annular water spraying pipes and water spraying holes, heat is rapidly and uniformly exchanged, and the second temperature control mechanism directly heats the material through the spiral annular heating pipe in the reaction tank. The double temperature control design of internal and external combination can accurately maintain the temperature environment required for seed preparation, and effectively improve the seed quality.

Description

Technical Field

[0001] This invention relates to the field of seed crystal preparation technology, specifically to a temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seed crystals. Background Technology

[0002] Battery-grade iron oxide red, as an important inorganic functional material, has been widely used in new energy fields such as lithium-ion battery cathode materials and supercapacitors due to its excellent chemical stability, electrochemical activity, and high purity. Its physicochemical properties, such as particle morphology, particle size distribution, and specific surface area, have a crucial impact on the charge-discharge performance, cycle life, and energy density of the final battery product. Seed crystal preparation, as a core pre-process in the iron oxide red production process, directly determines the morphology and quality of subsequent crystal growth, making it one of the most technically demanding and difficult-to-control links in the entire process chain.

[0003] In traditional battery-grade iron oxide red seed crystal preparation processes, a wet chemical method is typically employed. The process begins by adding ferrous sulfate solution and alkaline solution in a specific ratio to a reaction vessel equipped with a stirrer. A neutralization reaction is then carried out under specific temperature conditions to generate a ferrous hydroxide colloidal precursor. Subsequently, air or oxygen is introduced into the reaction system for aeration and oxidation, gradually converting the ferrous hydroxide into iron hydroxide seed crystals. During this process, operators must regulate the reaction temperature by controlling the amount of steam or cooling water flowing through the jacket or coils, and rely on experience or periodic sampling to determine the reaction endpoint, ultimately obtaining a brownish-red seed crystal suspension.

[0004] However, relying solely on the external jacket of the reaction vessel for heat exchange makes it difficult to quickly and accurately respond to the instantaneous changes in heat release or absorption during the reaction process. This can easily lead to local overheating or undercooling inside the vessel, thereby affecting the uniformity of the seed crystals. Furthermore, temperature control relies heavily on human experience and manual adjustment, resulting in significant fluctuations in product quality between different batches. In addition, traditional equipment has a low rate of recycling and utilizing resources such as cooling water, causing unnecessary energy waste. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds, which can effectively solve the problems mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution: a temperature-controlled oxidation reaction device for preparing battery-grade iron oxide red seed crystals, comprising a reaction vessel, wherein a support leg is fixed at the bottom of the reaction vessel and a feed pipe is fixed through the top of the reaction vessel; The first temperature control mechanism includes a heat insulation cover fixed to the outer wall of the reaction vessel, a second water guide pipe and an annular water spray pipe provided on the inner wall of the heat insulation cover, a first water tank fixed to the bottom of the outer wall of the heat insulation cover, a first water pump fixed through the top of the first water tank, and a first water guide pipe fixed to the outlet end of the first water pump. The second temperature control mechanism includes a second water tank fixed to the bottom of the support leg, a second water pump fixed through the top of the second water tank, a third water guide pipe fixed to the outlet end of the second water pump, and an annular heating pipe fixed to the inner wall of the reaction vessel by a support rod.

[0007] Preferably, the bottom of the reaction vessel is arc-shaped, a discharge pipe is fixedly installed through the bottom of the reaction vessel, a valve is installed on the outer wall of the discharge pipe, and a cover plate is hinged to the top of the feed pipe.

[0008] Preferably, a material guide cover is fixed to the top of the inner wall of the reaction vessel. The bottom of the material guide cover is hollow cylindrical, the top of the material guide cover is conical, and the bottom end of the material guide cover is located in the middle of the annular heating tube.

[0009] Preferably, the top end of the first water guide pipe penetrates the outer wall of the heat insulation cover and is connected to the second water guide pipe. Multiple annular water spray pipes are provided, and the multiple annular water spray pipes are arranged vertically and equidistantly inside the heat insulation cover. The second water guide pipe is used to connect the multiple annular water spray pipes, and the inner side of the multiple annular water spray pipes is provided with water spray holes in a circumferentially equidistant manner.

[0010] Preferably, the top of the first water tank near the insulation cover is connected to the insulation cover, the bottom of the insulation cover is inclined, and the bottommost end of the insulation cover is used in conjunction with the water inlet on one side of the first water tank.

[0011] Preferably, the annular heating tube is located in the middle of the inside of the reaction vessel, the annular heating tube is arranged in a spiral shape, the top of the third water guide tube is connected to the top of the annular heating tube, and the outer wall of the third water guide tube is provided with heat insulation cotton. The top of the annular heating tube passes through the bottom of the reaction vessel and is sealed to one side of the second water tank.

[0012] Preferably, the first water tank is provided with a first temperature control knob on its outer wall, and the second water tank is provided with a second temperature control knob on its outer wall. Both the first and second water tanks are fixed with heating rods that are vertically equidistant inside. The heating rods are arranged in an S-shape, and the two sets of heating rods are electrically connected to the first temperature control knob and the second temperature control knob, respectively.

[0013] Preferably, a second temperature sensor is fixed through one side of both the first and second water tanks, and a connecting rod is fixed through one side of the reaction vessel. A display screen is fixed at one end of the connecting rod on the outer wall of the reaction vessel, and a first temperature sensor is fixed on the connecting rod.

[0014] Preferably, there are two first temperature sensors, one of which is located in the middle of the annular heating tube, and the other is located in the middle of the outer wall of the annular heating tube and the inner wall of the reaction vessel. Both first temperature sensors are coated with anti-corrosion coatings, and both first temperature sensors and both second temperature sensors are electrically connected to the display screen.

[0015] Compared with the prior art, the beneficial effects of the present invention are: 1. This invention achieves precise temperature control within the reaction vessel through the synergistic action of a first and a second temperature control mechanism. The first temperature control mechanism uniformly sprays water onto the outer wall of the reaction vessel via multiple annular water spray pipes and nozzles, enabling rapid and uniform heat exchange. The second temperature control mechanism directly heats the materials through a spiral annular heating pipe inside the reaction vessel. This dual temperature control design, combining internal and external mechanisms, can precisely maintain the temperature environment required for seed crystal preparation, effectively improving seed crystal quality. 2. This invention constructs a refined temperature closed-loop control system by setting up two first temperature sensors, two second temperature sensors, and a display screen. The first temperature sensor monitors the internal temperature of the annular heating tube and the material temperature in the area between the outer wall of the annular heating tube and the inner wall of the reaction vessel. The second temperature sensor monitors the water temperature of the first water tank and the second water tank, respectively. This allows the operator to accurately judge the heat distribution inside and outside the vessel and precisely adjust the first and second temperature control knobs based on these values, thereby achieving refined closed-loop control of the temperature throughout the entire seed crystal preparation process. 3. The present invention guides the raw materials vertically into the middle area of ​​the annular heating tube by setting a guide cover at the top of the reaction tank, which effectively avoids the raw materials directly impacting the pipeline and causing damage, making the device more durable. The bottom of the heat insulation cover of the first temperature control mechanism is inclined, which can collect the sprayed water and guide it back to the first water tank. The water flow of the second temperature control mechanism circulates through the annular heating tube, thereby realizing the recycling of water and making the whole device more energy-saving and environmentally friendly. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the overall structure of the device of the present invention.

[0017] Figure 2 This is a schematic cross-sectional view of the reaction vessel of the device of the present invention.

[0018] Figure 3 This is a schematic diagram of the structure of the first temperature control mechanism in the device of the present invention.

[0019] Figure 4 This is a schematic diagram of the internal structure of the heat insulation cover of the device of the present invention.

[0020] Figure 5This is a schematic diagram of the internal structure of the water tank in the device of the present invention.

[0021] Figure 6 This is a schematic diagram of the internal structure of the reaction vessel of the device of the present invention.

[0022] Figure 7 This is a schematic diagram of the structure of the display screen of the device of the present invention.

[0023] In the diagram: 1. Reaction vessel; 2. Support leg; 3. Discharge pipe; 4. Feed pipe; 5. Cover plate; 60. First temperature control mechanism; 61. Insulation cover; 62. First water tank; 63. Heating rod; 64. First temperature control knob; 65. First water pump; 66. First water guide pipe; 67. Second water guide pipe; 68. Annular water spray pipe; 681. Water spray hole; 70. Second temperature control mechanism; 71. Second water tank; 72. Second water pump; 73. Third water guide pipe; 74. Annular heating tube; 75. Support rod; 76. Second temperature control knob; 8. Display screen; 9. Connecting rod; 10. First temperature sensor; 11. Second temperature sensor; 12. Feed guide cover. Detailed Implementation

[0024] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example 1

[0025] Please see Figures 1 to 7 The first embodiment of the present invention provides a technical solution for a temperature-controlled oxidation reaction device for preparing battery-grade iron oxide red seeds: including a reaction tank 1, a support leg 2 fixed at the bottom of the reaction tank 1, and a feed pipe 4 fixed through the top of the reaction tank 1; The first temperature control mechanism 60 includes a heat insulation cover 61 fixed to the outer wall of the reaction vessel 1, a second water guide pipe 67 and an annular water spray pipe 68 provided on the inner wall of the heat insulation cover 61, a first water tank 62 fixed to the bottom of the outer wall of the heat insulation cover 61, a first water pump 65 fixed through the top of the first water tank 62, and a first water guide pipe 66 fixed to the outlet end of the first water pump 65. The second temperature control mechanism 70 includes a second water tank 71 fixed to the bottom of the support leg 2, a second water pump 72 fixed through the top of the second water tank 71, a third water guide pipe 73 fixed to the outlet end of the second water pump 72, and an annular heating pipe 74 fixed to the inner wall of the reaction tank 1 by a support rod 75.

[0026] Reference Appendix Figure 1The bottom of the reaction tank 1 is arc-shaped, and a discharge pipe 3 is fixed through the bottom of the reaction tank 1. A valve is installed on the outer wall of the discharge pipe 3. A cover plate 5 is hinged to the top of the feed pipe 4. The arc-shaped bottom allows for faster and more thorough discharge. Raw materials are fed into the top of the feed pipe 4, and the cover plate 5 is put on after feeding to achieve internal sealing of the reaction tank 1.

[0027] Reference Appendix Figure 2 The reaction vessel 1 has a material guide cover 12 fixed to the top of the inner wall. The bottom of the material guide cover 12 is hollow cylindrical and the top of the material guide cover 12 is conical. The bottom of the material guide cover 12 is located in the middle of the annular heating tube 74. The conical top of the material guide cover 12 can better guide the material, gather the raw material fed into the feed pipe 4 towards the middle, and guide the material vertically downward through the bottom cylindrical shape, so as to avoid the raw material impacting the annular heating tube 4 and causing damage.

[0028] Reference Appendix Figure 3 and 4 The first water guide pipe 66 penetrates the outer wall of the insulation cover 61 at its top and is connected to the second water guide pipe 67. Multiple annular water spray pipes 68 are provided, which are arranged vertically and equidistantly inside the insulation cover 61. The second water guide pipe 67 is used to connect the multiple annular water spray pipes 68. The inner side of the multiple annular water spray pipes 68 is provided with spray holes 681 in a circumferentially equidistant pattern. Water from the first water tank 62 is pumped into the first water guide pipe 66 by the first water pump 65, and then introduced into the multiple annular water spray pipes 68 through the second water guide pipe 67. This allows the multiple spray holes 681 to spray evenly onto the outside of the reaction tank 1, and the outer wall of the reaction tank 1 is largely exposed to the water flow, achieving rapid and uniform heat exchange.

[0029] Reference Appendix Figure 3 The first water tank 62 is connected to the top of the insulation cover 61 on the side closest to the insulation cover 61. The bottom of the insulation cover 61 is set at an angle. The bottom of the insulation cover 61 is matched with the water inlet on the side of the first water tank 62. The water sprayed on the outer wall of the reaction tank 1 falls naturally due to gravity and collects at the bottom of the insulation cover 61. The bottom of the insulation cover 61 is tilted to introduce the collected water into the first water tank 62, so as to realize the reuse of water.

[0030] Reference Appendix Figure 5 The annular heating tube 74 is located in the middle of the interior of the reaction vessel 1. The annular heating tube 74 is arranged in a spiral shape. The top of the third water guide tube 73 is connected to the top of the annular heating tube 74. The outer wall of the third water guide tube 73 is provided with heat insulation cotton. The top of the annular heating tube 74 passes through the bottom of the reaction vessel 1 and is sealed to one side of the second water tank 71.

[0031] Referring to the attached drawings, a first temperature control knob 64 is provided on the outer wall of the first water tank 62, and a second temperature control knob 76 is provided on the outer wall of the second water tank 71. Heating rods 63 are vertically and equidistantly fixed inside both the first water tank 62 and the second water tank 71. The heating rods 63 are S-shaped and electrically connected to the first temperature control knob 64 and the second temperature control knob 76, respectively. The two sets of heating rods 63 heat the water inside the first water tank 62 and the second water tank 71. The multiple S-shaped heating rods 63 can quickly and evenly raise the temperature of the water in the tanks. The water temperature inside the first water tank 62 and the second water tank 71 can be controlled by adjusting the first temperature control knob 64 and the second temperature control knob 76 according to the required reaction temperature inside the reaction vessel 1.

[0032] During use, first open the cover plate 5 and feed the raw materials required for seed crystal preparation into the feed pipe 4. After the raw materials are gathered at the conical top of the guide cover 12, they fall vertically into the middle area of ​​the annular heating tube 74 from the hollow cylindrical outlet at the bottom, avoiding direct impact on the annular heating tube 74. Then, set the target heating temperature of the electric heating rod 63 in the first water tank 62 and the second water tank 71 using the first temperature control knob 64 and the second temperature control knob 76. Then, start the first water pump 65 and the second water pump 72 to circulate the water in the two water tanks in the first temperature control mechanism 60 and the second temperature control mechanism 70 respectively. The first water pump 65 pumps the water in the first water tank 62 into the first water guide pipe 66, and then distributes it to each water tank through the second water guide pipe 67. A ring-shaped water spray pipe 68 sprays water evenly onto the outer wall of the reaction tank 1 through spray holes 681 to exchange heat. The water then flows back to the first water tank 62 through the inclined bottom of the heat insulation cover 61, realizing recycling. At the same time, the second water pump 72 pumps the hot water in the second water tank 71 into the spiral ring heating pipe 74 inside the reaction tank 1 through the third water guide pipe 73 to directly heat the materials. The water after heat exchange flows back to the second water tank 71. The two temperature control mechanisms operate stably. During the reaction, the temperature inside the tank is precisely maintained through the synergistic action of the first temperature control mechanism 60 and the second temperature control mechanism 70. After the reaction is completed, the valve of the discharge pipe 3 is opened. The arc-shaped bottom of the tank helps the seed crystal suspension to be discharged quickly and completely. Example 2

[0033] Please see Figure 1 and Figure 7 This is the second embodiment of the present invention, which differs from the first embodiment in that: Reference Appendix Figure 7The first water tank 62 and the second water tank 71 are both fixed with a second temperature sensor 11 through one side, and the reaction vessel 1 is fixed with a connecting rod 9 through one side. The connecting rod 9 is fixed with a display screen 8 at one end of the outer wall of the reaction vessel 1, and the first temperature sensor 10 is fixed on the connecting rod 9. The temperature of the first water tank 62 and the second water tank 71 can be monitored in real time by the two second temperature sensors 11, so that the first temperature control knob 64 and the second temperature control knob 76 can be operated to control the temperature better.

[0034] Reference Appendix Figure 1 and 7 There are two first temperature sensors 10. One first temperature sensor 10 is located in the middle of the annular heating tube 74, and the other first temperature sensor 10 is located in the middle of the outer wall of the annular heating tube 74 and the inner wall of the reaction vessel 1. The two first temperature sensors 10 are coated with anti-corrosion coating. The two first temperature sensors 10 and the two second temperature sensors 11 are electrically connected to the display screen 8. The display screen 8 displays the temperature inside the annular heating tube 74, the temperature outside the annular heating tube 74, and the temperature of the first water tank 62 and the second water tank 71 in real time. Based on this, the first temperature control knob 64 and the second temperature control knob 76, the first water pump 65 and the second water pump 72 are started and stopped.

[0035] During operation, the operator reads the temperature data returned by the two first temperature sensors 10 and two second temperature sensors 11 in real time through the display screen 8. One of the first temperature sensors 10 monitors the temperature inside the annular heating tube 74, while the other monitors the material temperature in the area between the outer wall of the annular heating tube 74 and the inner wall of the reaction vessel 1. Its external anti-corrosion coating ensures long-term stable operation in corrosive materials. The two second temperature sensors 11 monitor the water temperature of the first water tank 62 and the second water tank 71, respectively. Based on these intuitive temperature values ​​on the display screen 8, the operator can accurately judge the heat distribution and status inside and outside the reaction vessel 1, and then precisely adjust the first temperature control knob 64 and the second temperature control knob 76 to control the heating power of the electric heating rods 63 in the two water tanks, and start and stop the first water pump 65 and the second water pump 72 in a timely manner, so as to achieve precise closed-loop control of the temperature of the entire seed crystal preparation process.

[0036] The remaining structure is the same as that in Example 1.

[0037] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds, characterized in that, include: The reaction vessel (1) has a support leg (2) fixed at the bottom and a feed pipe (4) fixed through the top of the reaction vessel (1). The first temperature control mechanism (60) includes a heat insulation cover (61) fixed to the outer wall of the reaction vessel (1), a second water guide pipe (67) and an annular water spray pipe (68) provided on the inner wall of the heat insulation cover (61), a first water tank (62) fixed to the bottom of the outer wall of the heat insulation cover (61), a first water pump (65) fixed through the top of the first water tank (62), and a first water guide pipe (66) fixed to the outlet end of the first water pump (65). The second temperature control mechanism (70) includes a second water tank (71) fixed to the bottom of the support leg (2), a second water pump (72) is fixed through the top of the second water tank (71), a third water pipe (73) is fixed to the outlet end of the second water pump (72), and an annular heating pipe (74) is fixed to the inner wall of the reaction tank (1) by a support rod (75).

2. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 1, characterized in that: The bottom of the reaction vessel (1) is arc-shaped, and a discharge pipe (3) is fixed through the bottom of the reaction vessel (1). A valve is provided on the outer wall of the discharge pipe (3), and a cover plate (5) is hinged to the top of the feed pipe (4).

3. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 2, characterized in that: The top of the inner wall of the reaction vessel (1) is fixed with a material guide cover (12). The bottom of the material guide cover (12) is set in a hollow cylindrical shape, and the top of the material guide cover (12) is set in a conical shape. The bottom end of the material guide cover (12) is located in the middle of the annular heating tube (74).

4. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 1, characterized in that: The top end of the first water guide pipe (66) penetrates the outer wall of the heat insulation cover (61) and is connected to the second water guide pipe (67). Multiple annular water spray pipes (68) are provided. The multiple annular water spray pipes (68) are arranged vertically and equidistantly inside the heat insulation cover (61). The second water guide pipe (67) is used to connect the multiple annular water spray pipes (68). The inner side of the multiple annular water spray pipes (68) is provided with water spray holes (681) in a circumferentially equidistant manner.

5. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 4, characterized in that: The top of the first water tank (62) near the heat insulation cover (61) is connected to the heat insulation cover (61) through the top. The bottom of the heat insulation cover (61) is set in an inclined position. The bottom of the heat insulation cover (61) is used in conjunction with the water inlet on one side of the first water tank (62).

6. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 1, characterized in that: The annular heating tube (74) is located in the middle of the interior of the reaction vessel (1). The annular heating tube (74) is arranged in a spiral shape. The top of the third water guide tube (73) is connected to the top of the annular heating tube (74). The outer wall of the third water guide tube (73) is provided with heat insulation cotton. The top of the annular heating tube (74) passes through the bottom of the reaction vessel (1) and is sealed to one side of the second water tank (71).

7. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 1, characterized in that: The first water tank (62) is provided with a first temperature control knob (64) on its outer wall, and the second water tank (71) is provided with a second temperature control knob (76) on its outer wall. The first water tank (62) and the second water tank (71) are both fixed with heating rods (63) in a vertical and equidistant manner inside. The heating rods (63) are arranged in an S-shape. The two sets of heating rods (63) are electrically connected to the first temperature control knob (64) and the second temperature control knob (76) respectively.

8. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 1, characterized in that: A second temperature sensor (11) is fixed through one side of the first water tank (62) and the second water tank (71). A connecting rod (9) is fixed through one side of the reaction vessel (1). A display screen (8) is fixed at one end of the connecting rod (9) on the outer wall of the reaction vessel (1). A first temperature sensor (10) is fixed on the connecting rod (9).

9. The temperature-controlled oxidation reaction apparatus for preparing battery-grade iron oxide red seeds according to claim 8, characterized in that: Two first temperature sensors (10) are provided. One of the first temperature sensors (10) is located in the middle of the annular heating tube (74), and the other first temperature sensor (10) is located in the middle of the outer wall of the annular heating tube (74) and the inner wall of the reaction vessel (1). The two first temperature sensors (10) are provided with anti-corrosion coatings, and the two first temperature sensors (10) and the two second temperature sensors (11) are electrically connected to the display screen (8).

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