Device for producing battery-grade ferromanganese phosphate by using coprecipitation method

Abstract

The utility model relates to a device for producing battery-grade ferromanganese phosphate by using a coprecipitation method. An outlet of a manganese source bin is connected with a manganese source dissolving tank; an outlet of the manganese source dissolving tank is connected into a manganese source metering tank; an outlet of the iron source bin is connected with the iron source dissolving tank, an outlet of the iron source dissolving tank is connected with the iron source metering tank, outlets of the manganese source metering tank and the iron source metering tank are connected into the mixing tank, an outlet of the mixing tank is connected into the mixed liquid metering tank, and outlets of the mixed liquid metering tank and the oxidizing agent metering tank are connected into the reaction kettle; outlets of the phosphorus source bin and the ammonia water metering tank are connected to the phosphorus source synthesis kettle, and an outlet of the phosphorus source synthesis kettle is connected to the reaction kettle; an outlet of the reaction kettle is connected with the solid-liquid separation device through a slurry delivery pump, a solid outlet of the solid-liquid separation device is connected with the drying device through a belt conveyor, and an outlet of the drying device is connected with the calcining device. The equipment layout is simple, all processes are controlled by the controller, production management and control are facilitated, complex production requirements are met, a large amount of manpower is saved, the production cost is reduced, and the production efficiency is improved.

Description

Technical Field

[0001] The utility model belongs to the technical device field of the production of manganese iron phosphate, and particularly relates to a device for producing battery-grade manganese iron phosphate by a coprecipitation method. Background Art

[0002] In recent years, China's new energy industry has developed vigorously. Lithium iron phosphate batteries have become the main power source of current electric vehicles due to their excellent cost performance. However, lithium iron phosphate batteries are limited by a 3.4V voltage platform, and the energy density of lithium iron phosphate batteries cannot be further improved. To improve the power density, lithium manganese iron phosphate batteries have emerged.

[0003] Existing conventional liquid-phase precipitation method and oxidation-coprecipitation method process devices have the disadvantages of a relatively high reaction process temperature, strict corresponding requirements for equipment, high energy consumption, high impurity content, and difficult control of product stability, which are not conducive to large-scale production. Summary of the Utility Model

[0004] The purpose of the utility model is to provide a device for producing battery-grade manganese iron phosphate by a coprecipitation method to solve the above problems.

[0005] To achieve the above purpose, the utility model adopts the following technical solutions: A device for producing battery-grade manganese iron phosphate by a coprecipitation method, characterized in that: the bottom outlet of the manganese source silo is connected to the manganese source dissolution tank, and the lower outlet of the manganese source dissolution tank is connected to the manganese source metering tank through a manganese source transfer pump; the bottom outlet of the iron source silo is connected to the iron source dissolution tank, and the lower outlet of the iron source dissolution tank is connected to the iron source metering tank through an iron source transfer pump. The bottom outlets of the manganese source metering tank and the iron source metering tank are both connected to the mixing tank, and the lower outlet of the mixing tank is connected to the mixed liquid metering tank through a mixed liquid transfer pump. The bottom outlets of the mixed liquid metering tank and the oxidant metering tank are both connected to the reaction kettle; the bottom outlets of the phosphorus source silo and the ammonia water metering tank are both connected to the phosphorus source synthesis kettle. The bottom outlet of the phosphorus source synthesis kettle is connected to a phosphorus source transfer pipe through a phosphorus source transfer pump, and the phosphorus source transfer pipe is connected to the reaction kettle; the bottom outlet of the reaction kettle is connected to a solid-liquid separation device through a slurry transfer pump. The solid outlet of the solid-liquid separation device is connected to a belt conveyor, the discharging end of the belt conveyor is connected to a drying device, and the outlet of the drying device is connected to a calcining device;

[0006] The manganese source silo, the iron source silo, the manganese source metering tank, the iron source metering tank, the phosphorus source silo, the ammonia water metering tank, the mixed liquid metering tank, and the oxidant metering tank are respectively arranged on their respective weighing devices.

[0007] Stirrers are arranged in the manganese source dissolution tank, the iron source dissolution tank, the mixing tank, the phosphorus source synthesis kettle, and the reaction kettle, and the control input end of the stirrer is correspondingly connected to the control output end of the controller.

[0008] Both the phosphorus source synthesis kettle and the reaction kettle are equipped with a thermometer and a pH meter; the signal output ends of the thermometer and the pH meter are respectively and correspondingly connected to the signal input end of the controller.

[0009] The outer peripheries of both the phosphorus source synthesis kettle and the reaction kettle are covered with heating devices.

[0010] A first desalination water pipe is connected to the manganese source dissolution tank, a second desalination water pipe is connected to the iron source dissolution tank, a third desalination water pipe is connected to the phosphorus source synthesis kettle, and a fourth desalination water pipe is connected to the solid-liquid separation device; flow meters are provided on the first desalination water pipe, the second desalination water pipe, the third desalination water pipe and the phosphorus source delivery pipe; the signal output ends of the flow meters are respectively and correspondingly connected to the signal input end of the controller.

[0011] The stirrer is controlled by a frequency converter for speed control.

[0012] The heating device is a steam tracing pipe or an immersion coil heat exchanger.

[0013] The signal output end of the weighing device is respectively and correspondingly connected to the signal input end of the controller; the control input ends of the manganese source delivery pump, the iron source delivery pump, the mixed liquid delivery pump, the phosphorus source delivery pump, the slurry delivery pump, the solid-liquid separation device, the belt conveyor, the drying device and the calcining device are respectively and correspondingly connected to the control output end of the controller.

[0014] The controller is a DCS controller or a PLC controller.

[0015] The beneficial effects of the present utility model are as follows: The equipment layout is simple, and each process is controlled by the controller, which is conducive to production management and control, realizes the automated production and production process detection of producing manganese iron phosphate by the coprecipitation method, can meet complex production requirements, saves a large amount of manpower, reduces production costs, improves production efficiency, and meets the technical requirements of energy conservation and consumption reduction. Description of the Drawings

[0016] Figure 1 It is a schematic diagram of the present utility model.

[0017] In the figure: 1 - manganese source dissolution tank, 2 - iron source dissolution tank, 3 - mixing tank, 4 - phosphorus source synthesis kettle, 5 - reaction kettle, 6 - solid-liquid separation device, 7 - belt conveyor, 8 - drying device, 9 - calcining device;

[0018] A1 - Manganese source silo, A2 - Iron source silo, A3 - Manganese source metering tank, A4 - Iron source metering tank, A5 - Phosphorus source silo, A6 - Ammonia water metering tank, A7 - Mixed liquid metering tank, A8 - Oxidant metering tank; B1 - Manganese source transfer pump, B2 - Iron source transfer pump, B3 - Mixed liquid transfer pump, B4 - Phosphorus source transfer pump, B5 - Slurry transfer pump; C1 - First desalinated water pipe 14, C2 - Second desalinated water pipe 24, C3 - Third desalinated water pipe 49, C4 - Fourth desalinated water pipe; L - Phosphorus source transfer pipe. Detailed implementation mode

[0019] The following further explains the present utility model in conjunction with the attached drawings:

[0020] A device for producing battery-grade manganese iron phosphate by coprecipitation method. The bottom outlet of the manganese source silo A1 is connected to the manganese source dissolution tank 1. The lower outlet of the manganese source dissolution tank 1 is connected to the manganese source metering tank A3 through the manganese source transfer pump B1. The bottom outlet of the iron source silo A2 is connected to the iron source dissolution tank 2. The lower outlet of the iron source dissolution tank 2 is connected to the iron source metering tank A4 through the iron source transfer pump B2. The bottom outlets of the manganese source metering tank A3 and the iron source metering tank A4 are both connected to the mixing tank 3. The lower outlet of the mixing tank 3 is connected to the mixed liquid metering tank A7 through the mixed liquid transfer pump B3. The bottom outlets of the mixed liquid metering tank A7 and the oxidant metering tank A8 are both connected to the reaction kettle 5. The bottom outlets of the phosphorus source silo A5 and the ammonia water metering tank A6 are both connected to the phosphorus source synthesis kettle 4. The bottom outlet of the phosphorus source synthesis kettle 4 is connected to the phosphorus source transfer pipe L through the phosphorus source transfer pump B4. The phosphorus source transfer pipe L is connected to the reaction kettle 5. The bottom outlet of the reaction kettle 5 is connected to the solid-liquid separation device 6 through the slurry transfer pump B5. The solid outlet of the solid-liquid separation device 6 is connected to the belt conveyor 7. The discharge end of the belt conveyor 7 is connected to the drying device 8. The outlet of the drying device 8 is connected to the calcination device 9;

[0021] The manganese source silo A1, iron source silo A2, manganese source metering tank A3, iron source metering tank A4, phosphorus source silo A5, ammonia water metering tank A6, mixed liquid metering tank A7 and oxidant metering tank A8 are respectively arranged on their respective weighing devices.

[0022] Stirrers are provided in the manganese source dissolution tank 1, iron source dissolution tank 2, mixing tank 3, phosphorus source synthesis kettle 4 and reaction kettle 5. The control input end of the stirrer is correspondingly connected to the control output end of the controller.

[0023] Thermometers and pH meters are provided on both the phosphorus source synthesis kettle 4 and the reaction kettle 5. The signal output ends of the thermometer and the pH meter are respectively correspondingly connected to the signal input end of the controller.

[0024] Heating devices are covered on the outer peripheries of the phosphorus source synthesis kettle 4 and the reaction kettle 5.

[0025] A first desalination water pipe C1 is connected to the manganese source dissolving tank 1, a second desalination water pipe C2 is connected to the iron source dissolving tank 2, a third desalination water pipe C3 is connected to the phosphorus source synthesis kettle 4, and a fourth desalination water pipe C4 is connected to the solid-liquid separation device 6; flow meters are provided on the first desalination water pipe C1, the second desalination water pipe C2, the third desalination water pipe C3 and the phosphorus source conveying pipe L; the signal output end of the flow meter is correspondingly connected to the signal input end of the controller.

[0026] The agitator is controlled by a frequency converter for speed control.

[0027] The heating device is a steam tracing pipe or an immersed coil heat exchanger.

[0028] The signal output end of the weighing device is correspondingly connected to the signal input end of the controller; the control input ends of the manganese source transfer pump B1, the iron source transfer pump B2, the mixed liquid transfer pump B3, the phosphorus source transfer pump B4, the slurry transfer pump B5, the solid-liquid separation device 6, the belt conveyor 7, the drying device 8 and the calcining device 9 are all correspondingly connected to the control output end of the controller.

[0029] The controller is a DCS controller or a PLC controller.

[0030] Level measuring instruments are installed on the manganese source dissolving tank 1, the manganese source storage bin A1, the iron source dissolving tank 2, the iron source storage bin A2, the mixing tank 3, the manganese source metering tank A3, the iron source metering tank A4, the phosphorus source synthesis kettle 4, the phosphorus source storage bin A5, the ammonia water metering tank A6, the reaction kettle 5, the mixed liquid metering tank A7 and the oxidant metering tank A8.

[0031] Pressure measuring instruments are installed on the outlet pipelines of the manganese source transfer pump B1, the iron source transfer pump B2, the mixed liquid transfer pump B3, the phosphorus source transfer pump B4 and the slurry transfer pump B5.

[0032] Working process:

[0033] First step: Place solid manganese sulfate in the manganese source storage bin A1, add it to the manganese source dissolving tank 1 by weighing, and at the same time add a certain amount of desalinated water to the manganese source dissolving tank 1 through the first desalination water pipe C1, and obtain a manganese source solution after stirring and dissolving; transfer the manganese source solution to the manganese source metering tank A3 through the manganese source transfer pump B1;

[0034] Second step: Place solid ferrous sulfate heptahydrate in the iron source storage bin A2, add it to the iron source dissolving tank 2 by weighing, and at the same time add a certain amount of desalinated water to the iron source dissolving tank 2 through the second desalination water pipe C2, and obtain an iron source solution after stirring and dissolving; transfer the iron source solution to the iron source metering tank A4 through the iron source transfer pump B2,

[0035] Step 3: Add the iron source solution and manganese source solution into the mixing tank 3 by weighing according to the ratio, and stir and mix evenly to obtain a mixed solution; transfer the mixed solution to the mixed solution metering tank A7 through the mixed solution transfer pump B3;

[0036] Step 4: Place the ammonium dihydrogen phosphate solid in the phosphorus source bin A5, add it into the phosphorus source synthesis kettle 4 by weighing. At the same time, add a certain amount of desalted water into the phosphorus source synthesis kettle 4 through the third desalted water pipe C3, and heat the phosphorus source synthesis kettle 4 through the steam tracing pipe. Monitor the reaction temperature in the phosphorus source synthesis kettle 4 through a thermometer. After stirring and dissolving, add a certain weight of ammonia water into the phosphorus source synthesis kettle 4 through the ammonia water metering tank A6. During the reaction process, detect the pH value of the material with a pH meter. After the reaction ends, obtain the phosphorus source solution;

[0037] Step 5: Transfer the phosphorus source solution in the phosphorus source synthesis kettle 4 to the reaction kettle 5 through the phosphorus source transfer pump B4. Weigh and add a certain weight of the mixed solution into the reaction kettle 5 through the mixed solution metering tank A7. The addition process is carried out slowly. At the same time, slowly add a certain amount of oxidant into the reaction kettle 5 through the oxidant metering tank A8. Start the stirrer during the whole reaction process, control the stirring rate according to the process technical requirements, heat the reaction kettle 5 through the steam tracing pipe. During the reaction process, monitor the temperature and pH value of the material through a thermometer and a pH meter. After the reaction ends, obtain the suspension slurry of iron manganese phosphate;

[0038] Step 6: Pump the suspension slurry of iron manganese phosphate into the solid-liquid separation device 6 through the slurry transfer pump B5 for solid-liquid separation, and wash the filter cake through the fourth desalted water pipe C4. After the washing is qualified, transfer the filter cake to the drying device 8 through the belt conveyor 7 for drying to remove the free water and obtain the iron manganese phosphate containing crystal water; transfer the iron manganese phosphate containing crystal water to the calcination device 9 for calcination to remove the crystal water and obtain the iron manganese phosphate.

[0039] The above embodiments are only the preferred embodiments of the present invention, and do not limit the technical solutions of the present invention. As long as the technical solutions that can be achieved on the basis of the above embodiments without creative labor shall be regarded as falling within the scope of the patent rights of the present invention.

Claims

1. An apparatus for producing battery-grade manganese iron phosphate by coprecipitation method, characterized in that: The bottom outlet of the manganese source silo (A1) is connected to the manganese source dissolution tank (1), and the lower outlet of the manganese source dissolution tank (1) is connected to the manganese source metering tank (A3) through the manganese source transfer pump (B1); the bottom outlet of the iron source silo (A2) is connected to the iron source dissolution tank (2), and the lower outlet of the iron source dissolution tank (2) is connected to the iron source metering tank (A4) through the iron source transfer pump (B2). The bottom outlets of the manganese source metering tank (A3) and the iron source metering tank (A4) are both connected to the mixing tank (3), and the lower outlet of the mixing tank (3) is connected to the mixed liquid metering tank (A7) through the mixed liquid transfer pump (B3). The bottom outlets of the mixed liquid metering tank (A7) and the oxidant metering tank (A8) are both connected to the reaction kettle (5); the bottom outlets of the phosphorus source silo (A5) and the ammonia water metering tank (A6) are both connected to the phosphorus source synthesis kettle (4), and the bottom outlet of the phosphorus source synthesis kettle (4) is connected to the phosphorus source transfer pipe (L) through the phosphorus source transfer pump (B4), and the phosphorus source transfer pipe (L) is connected to the reaction kettle (5); the bottom outlet of the reaction kettle (5) is connected to the solid-liquid separation device (6) through the slurry transfer pump (B5), the solid outlet of the solid-liquid separation device (6) is connected to the belt conveyor (7), the discharge end of the belt conveyor (7) is connected to the drying device (8), and the outlet of the drying device (8) is connected to the calcining device (9). The manganese source silo (A1), iron source silo (A2), manganese source metering tank (A3), iron source metering tank (A4), phosphorus source silo (A5), ammonia water metering tank (A6), mixed liquid metering tank (A7) and oxidant metering tank (A8) are respectively arranged on their own weighing devices.

2. The device for producing battery-grade manganese iron phosphate by coprecipitation method according to claim 1, characterized in that: Stirrers are provided in the manganese source dissolution tank (1), iron source dissolution tank (2), mixing tank (3), phosphorus source synthesis kettle (4) and reaction kettle (5), and the control input ends of the stirrers are correspondingly connected to the control output ends of the controller.

3. The device for producing battery-grade manganese iron phosphate by coprecipitation method according to claim 1, wherein: Thermometers and pH meters are provided on both the phosphorus source synthesis kettle (4) and the reaction kettle (5); the signal output ends of the thermometers and pH meters are correspondingly connected to the signal input ends of the controller.

4. An apparatus for producing battery-grade manganese iron phosphate by coprecipitation method as claimed in claim 1, wherein: Heating devices are covered on the outer peripheries of both the phosphorus source synthesis kettle (4) and the reaction kettle (5).

5. The device for producing battery-grade manganese iron phosphate by coprecipitation method according to claim 1, wherein: A first desalting water pipe (C1) is connected to the manganese source dissolution tank (1), a second desalting water pipe (C2) is connected to the iron source dissolution tank (2), a third desalting water pipe (C3) is connected to the phosphorus source synthesis kettle (4), and a fourth desalting water pipe (C4) is connected to the solid-liquid separation device (6); flow meters are provided on the first desalting water pipe (C1), second desalting water pipe (C2), third desalting water pipe (C3) and phosphorus source transfer pipe (L); the signal output ends of the flow meters are correspondingly connected to the signal input ends of the controller.

6. The device for producing battery-grade manganese iron phosphate by coprecipitation method as described in claim 2, wherein: The stirrer is controlled by a frequency converter for speed control.

7. The device for producing battery-grade manganese iron phosphate by coprecipitation method according to claim 4, characterized in that: The heating device is a steam tracing pipe or an immersion coil heat exchanger.

8. The device for producing battery-grade manganese iron phosphate by coprecipitation method as described in claim 1, characterized in that: The signal output end of the weighing device is correspondingly connected to the signal input end of the controller; the control input ends of the manganese source delivery pump (B1), iron source delivery pump (B2), mixed liquid delivery pump (B3), phosphorus source delivery pump (B4), slurry delivery pump (B5), solid-liquid separation device (6), belt conveyor (7), drying device (8) and calcination device (9) are all correspondingly connected to the control output end of the controller.

9. A device for producing battery-grade manganese iron phosphate by coprecipitation method according to any one of claims 2, 3, 5, and 8, characterized in that: The controller is a DCS controller or a PLC controller.

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