Reaction system for preparing ternary precursor

Abstract

The utility model provides a reaction system for preparing a ternary precursor, which comprises a reaction kettle, the reaction kettle is provided with a jacket, the jacket is provided with a jacket water inlet and a jacket water outlet, the reaction kettle is also provided with a mechanical seal, the mechanical seal is provided with a mechanical seal water inlet and a mechanical seal water outlet, the reaction system also comprises a high-temperature water bath kettle and a low-temperature water bath kettle, the set temperature of the high-temperature water bath kettle is higher than that of the low-temperature water bath kettle. According to the utility model, the heat transfer medium can circulate in the high-temperature water bath kettle and / or the low-temperature water bath kettle and the reaction kettle jacket so as to achieve effective temperature control; and the mechanical seal cooling water is recycled among the high-temperature water bath kettle, the reaction kettle mechanical seal and the low-temperature water bath kettle, so that the waste of the cooling water is greatly reduced.

Description

Technical Field

[0001] This utility model relates to the technical field of sodium-ion battery cathode material preparation device, specifically to a reaction system for preparing ternary precursors. Background Technology

[0002] Ternary precursors are important upstream materials for the production of ternary cathode materials. Their performance levels in various aspects directly determine the performance of ternary cathode materials. For example, the particle size distribution, element ratio, and impurity content of ternary precursors affect the core electrochemical performance of batteries, such as consistency, energy density, and cycle life.

[0003] Currently, ternary precursors are usually prepared by co-precipitation, which involves pumping a nickel-cobalt-manganese soluble salt solution, a sodium hydroxide solution, and an ammonia solution into a reaction vessel filled with protective gas and equipped with a stirrer and jacket. By controlling the stirring speed, reaction temperature, reaction pH, feed flow rate, and material concentration, hydroxide particles with a certain particle size and particle size distribution are generated.

[0004] Unlike nickel-cobalt-manganese ternary precursors, nickel-iron-manganese ternary precursors are more easily oxidized by ferrous ions during the reaction process. Especially at high temperatures, the oxidation of the material leads to a loose, porous, and non-dense precursor structure as well as uneven internal stress, which limits the performance of the subsequent finished cathode material.

[0005] Temperature control in conventional reactors typically involves circulating water in the reactor jacket using a water bath or temperature controller to transfer heat and maintain a stable internal temperature. However, during actual reactions, the high-speed operation of the motor generates heat from both the motor and the agitation, causing the solution temperature inside the reactor to rise. Simply using a water bath to transfer jacket water is insufficient to control temperature stability. Significant temperature fluctuations lead to changes in reaction rate and pH readings, resulting in uncontrollable reaction processes and alterations in precursor structure. Furthermore, the large amount of cooling water used for the motor's mechanical seals during the reaction process represents a waste of water resources.

[0006] Utility model patent CN219334184U discloses an experimental coprecipitation reaction apparatus. The coprecipitation reactor has a lid on top, and a clamp is installed between the lid and the reactor, securing them together. The lid has a pH monitoring port, an air inlet, a feed inlet, and an exhaust port. The feed inlet is connected to a feeding pipe. A stirrer mounting port is located at the geometric center of the lid, and a stirrer is mounted thereon. A constant temperature water bath is located at the bottom of the coprecipitation reactor, and an electromagnetic heater is located at the bottom of the water bath. In application, a control system controls the stirring speed of the stirrer, the heating temperature of the electromagnetic heater, the feeding speed of the peristaltic pump, the pH value at the pH monitoring port, the on / off state of the electromagnetic valve, the pressure setpoint of the pressure alarm, and the data transmitted by the temperature sensor, and connects with relevant equipment to control the entire reaction process. However, this reaction apparatus is only for experimental use and cannot be used for production. Utility Model Content

[0007] To address the aforementioned problems in the existing technology, this utility model provides a reaction system for preparing ternary precursors, including a reaction vessel with a jacket, the jacket having a jacket inlet and a jacket outlet, the reaction vessel also having a mechanical seal with a mechanical seal inlet and a mechanical seal outlet, the reaction system further including a high-temperature water bath and a low-temperature water bath, the set temperature of the high-temperature water bath being higher than the set temperature of the low-temperature water bath.

[0008] The high-temperature water bath has a first outlet, a second outlet, and a first inlet. The first outlet is connected to the jacket inlet via a first outlet pipe. The second outlet is connected to the mechanical seal inlet via a second outlet pipe. The first inlet is connected to the jacket outlet via a first inlet pipe.

[0009] The low-temperature water bath has a third outlet and a second inlet. The third outlet is connected to the jacket inlet via a third outlet pipe, and the second inlet is connected to the mechanical seal outlet via a second inlet pipe.

[0010] Water from the high-temperature water bath and water from the low-temperature water bath enter the jacket of the reactor through the first water outlet pipe and the third water outlet pipe, respectively, and then return to the high-temperature water bath through the first water inlet pipe for circulation.

[0011] Water from the high-temperature water bath enters the mechanical seal of the reactor through the second outlet pipe, and then enters the low-temperature water bath through the second inlet pipe, thus achieving the circulation of cooling water for the mechanical seal.

[0012] Furthermore, a first water pump is installed on the first water outlet pipe, a second water pump is installed on the second water outlet pipe, and a third water pump is installed on the third water outlet pipe.

[0013] Furthermore, the first, second, and third water pumps are all centrifugal pumps, which can quickly transport large amounts of water.

[0014] Furthermore, the first outlet pipe is provided with a first shut-off valve downstream of the first water pump; the third outlet pipe is provided with a second shut-off valve downstream of the third water pump, which is used to regulate the flow rate of water in the corresponding water pipe.

[0015] Furthermore, the first outlet pipe is also provided with a first check valve downstream of the first shut-off valve; the third outlet pipe is also provided with a second check valve downstream of the second shut-off valve, which is used to prevent the water in the pipe from flowing back after the water pump stops, so as to protect the water pump and reaction system upstream.

[0016] Furthermore, the first and third outlet pipes are merged into a single pipe downstream of the first and second check valves and then connected to the jacket inlet.

[0017] Furthermore, the top surface of the reactor is equipped with a salt inlet, an alkali inlet, a complexing agent inlet, a gas outlet, a gas inlet, pH and temperature detection ports, and a viewing window. The salt inlet, alkali inlet, and complexing agent inlet are used to add the mixed salt solution, alkali solution, and complexing agent into the reactor, respectively; the gas inlet is used to introduce nitrogen gas into the reactor, and the gas outlet is used to exhaust gas during nitrogen introduction; the pH and temperature detection ports are used to house probes or sensors for detecting the pH and temperature of the materials in the reactor; the viewing window allows operators to directly observe the internal state of the reactor without opening it.

[0018] The beneficial effects of this utility model are as follows:

[0019] This invention provides a reaction system for preparing ternary precursors, which allows the heat transfer medium to circulate between a high-temperature water bath and / or a low-temperature water bath and the reactor jacket, thereby achieving effective temperature control. The mechanical seal cooling water is circulated between the high-temperature water bath, the reactor mechanical seal, and the low-temperature water bath, significantly reducing cooling water waste. This reaction system can effectively maintain a stable reactor temperature, thereby improving the stability of the reaction process control and synthesizing materials with excellent performance. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the reaction system used to prepare ternary precursors in this invention.

[0021] Figure 2 This is a schematic diagram of the top surface of the reactor in this utility model.

[0022] Figure reference numerals: Reactor 1, Jacket 11, Jacket inlet 111, Jacket outlet 112, Mechanical seal 12, Mechanical seal inlet 121, Mechanical seal outlet 122, Salt inlet 13, Alkali inlet 14, Complexing agent inlet 15, Gas outlet 16, Gas inlet 17, pH and temperature detection ports 18, Viewing window 19, High-temperature water bath 2, First outlet 21, Second outlet 22, First inlet 23

[0023] Low-temperature water bath 3, third water outlet 31, second water inlet 32

[0024] First outlet pipe 4, first water pump 41, first shut-off valve 42, first check valve 43

[0025] Second water outlet pipe 5, second water pump 51

[0026] Third water outlet pipe 6, third water pump 61, second shut-off valve 62, second check valve 63

[0027] First water inlet pipe 7, second water inlet pipe 8. Detailed Implementation

[0028] like Figures 1-2 As shown, an embodiment of this application provides a reaction system for preparing a ternary precursor, including a reactor 1. The reactor 1 has a jacket 11, with a jacket inlet 111 and a jacket outlet 112. The reactor 1 also has a mechanical seal 12, with a mechanical seal inlet 121 and a mechanical seal outlet 122. The top surface of the reactor 1 is provided with a salt inlet 13, an alkali inlet 14, a complexing agent inlet 15, a gas outlet 16, a gas inlet 17, pH and temperature detection ports 18, and a viewing window 19. The reaction system also includes a high-temperature water bath 2 and a low-temperature water bath 3, with the set temperature of the high-temperature water bath 2 being higher than that of the low-temperature water bath 3.

[0029] The high-temperature water bath 2 has a first water outlet 21, a second water outlet 22 and a first water inlet 23. The first water outlet 21 is connected to the jacket water inlet 111 through the first water outlet pipe 4. The second water outlet 22 is connected to the mechanical seal water inlet 121 through the second water outlet pipe 5. The first water inlet 23 is connected to the jacket water outlet 112 through the first water inlet pipe 7.

[0030] The low-temperature water bath 3 has a third outlet 31 and a second inlet 32. The third outlet 31 is connected to the jacket inlet 111 through the third outlet pipe 6, and the second inlet 32 ​​is connected to the mechanical seal outlet 122 through the second inlet pipe 8.

[0031] On the first water outlet pipe 4, from the first water outlet 21 to the jacket inlet 111, a first water pump 41, a first shut-off valve 42 and a first check valve 43 are sequentially provided.

[0032] A second water pump 51 is installed on the second water outlet pipe 5, between the second water outlet 22 and the mechanical seal inlet 121.

[0033] On the third water outlet pipe 6, from the third water outlet 31 to the jacket inlet 111, a third water pump 61, a second shut-off valve 62, and a second check valve 63 are sequentially installed.

[0034] Among them, the first water pump 41, the second water pump 51 and the third water pump 61 are all centrifugal pumps.

[0035] The first outlet pipe 4 and the third outlet pipe 6 are merged into a single pipe downstream of the first check valve 43 and the second check valve 63, and then connected to the jacket inlet 111.

[0036] Water from the high-temperature water bath 2 and water from the low-temperature water bath 3 enter the reactor jacket 11 through the first water outlet pipe 4 and the third water outlet pipe 6, respectively, and then return to the high-temperature water bath 2 through the first water inlet pipe 7 for circulation.

[0037] Water from the high-temperature water bath 2 enters the mechanical seal 12 of the reactor through the second water outlet pipe 5, and then enters the low-temperature water bath 3 through the second water inlet pipe 8, thus achieving the circulation of cooling water for the mechanical seal 12.

[0038] During operation, the temperature in the reactor can be controlled by adjusting the temperatures of the high-temperature water bath and the low-temperature water bath, as well as the flow rate of water supplied from the high-temperature water bath and the low-temperature water bath to the reactor.

Claims

1. A reaction system for preparing ternary precursors, comprising a reaction vessel, the reaction vessel having a jacket, the jacket having a jacket inlet and a jacket outlet, the reaction vessel further having a mechanical seal, the mechanical seal having a mechanical seal inlet and a mechanical seal outlet, characterized in that, The reaction system also includes a high-temperature water bath and a low-temperature water bath, wherein the set temperature of the high-temperature water bath is higher than the set temperature of the low-temperature water bath. The high-temperature water bath has a first water outlet, a second water outlet, and a first water inlet. The first water outlet is connected to the jacket water inlet through a first water outlet pipe. The second water outlet is connected to the mechanical seal water inlet through a second water outlet pipe. The first water inlet is connected to the jacket water outlet through a first water inlet pipe. The low-temperature water bath has a third outlet and a second inlet. The third outlet is connected to the jacket inlet via a third outlet pipe, and the second inlet is connected to the mechanical seal outlet via a second inlet pipe.

2. The reaction system for preparing ternary precursors according to claim 1, characterized in that, The first water outlet pipe is equipped with a first water pump, the second water outlet pipe is equipped with a second water pump, and the third water outlet pipe is equipped with a third water pump.

3. The reaction system for preparing ternary precursors according to claim 2, characterized in that, The first, second, and third water pumps are all centrifugal pumps.

4. The reaction system for preparing ternary precursors according to claim 2, characterized in that, The first outlet pipe is equipped with a first shut-off valve downstream of the first water pump; the third outlet pipe is equipped with a second shut-off valve downstream of the third water pump.

5. The reaction system for preparing ternary precursors according to claim 4, characterized in that, The first outlet pipe is also equipped with a first check valve downstream of the first shut-off valve; the third outlet pipe is also equipped with a second check valve downstream of the second shut-off valve.

6. The reaction system for preparing ternary precursors according to claim 5, characterized in that, The first and third outlet pipes are merged into a single pipe downstream of the first and second check valves and then connected to the jacket inlet.

7. The reaction system for preparing ternary precursors according to claim 1, characterized in that, The top surface of the reactor is equipped with a salt inlet, an alkali inlet, a complexing agent inlet, an outlet, an inlet, pH and temperature detection ports, and a viewing window.

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