Device for producing battery-grade titanium-doped iron phosphate

Abstract

The utility model relates to a device for producing battery-grade titanium-doped iron phosphate, which is characterized in that an outlet of an iron source dissolving tank is connected with a feed port of a first filter press, a liquid outlet of the first filter press is connected with an iron source clear liquid storage tank, an outlet of the iron source clear liquid storage tank is connected with an iron-titanium mixing tank, and a discharge pipe of a titanium source metering tank is connected with the iron-titanium mixing tank. An outlet of the iron-titanium mixing tank is connected with an iron source metering tank; an outlet of the iron source metering tank is connected into the synthetic reaction kettle; an outlet of the synthetic reaction kettle is connected with a second filter press, a solid outlet of the second filter press is connected with an aging reaction kettle through a first belt conveyor, an outlet of the aging reaction kettle is connected with a third filter press through an aging slurry delivery pump, a solid outlet of the third filter press is connected into a flash dryer through a second belt conveyor, and an outlet of the flash dryer is connected with a kiln. The layout is reasonable, and full-automatic monitoring and control are realized. The use amount of the pH regulator can be effectively reduced, the generation of impurity byproducts is reduced, the energy consumption and the wastewater generation amount are reduced, the stable operation of production is ensured, and the product quality is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of ferric phosphate production, in particular to a device for producing battery-grade titanium-doped ferric phosphate. Background Art

[0002] In recent years, my country's new energy vehicle industry has flourished. Lithium iron phosphate batteries have become the primary power source for electric vehicles due to their excellent cost-performance ratio. The electrochemical performance of lithium iron phosphate batteries can be improved by doping them with metal cations.

[0003] Conventional industrial titanium-doped iron phosphate production processes typically combine titanium and iron sources under acidic conditions for co-precipitation, followed by high-temperature sintering to achieve the desired doping effect. This production process requires a large amount of pH regulator, which increases the production cost of the iron phosphate and increases byproducts, ultimately driving up costs. Utility Model Content

[0004] The purpose of the present utility model is to solve the above problems and provide a device for producing battery-grade titanium-doped ferric phosphate.

[0005] To achieve the above-mentioned purpose, the utility model adopts the following technical scheme: a device for producing battery-grade titanium-doped ferric phosphate, characterized in that: a ferrous bin and a regulating tank are arranged above the iron source dissolving tank, the discharge pipes at the bottom of the ferrous bin and the regulating tank are connected to the iron source dissolving tank, the lower outlet of the iron source dissolving tank is connected to the feed port of the first filter press through an iron source slurry delivery pump, the liquid outlet of the first filter press is connected to the iron source clear liquid storage tank, the lower outlet of the iron source clear liquid storage tank is connected to the iron-titanium mixing tank through the iron source clear liquid delivery pump, a titanium source metering tank is arranged above the iron-titanium mixing tank, the bottom discharge pipe of the titanium source metering tank is connected to the iron-titanium mixing tank, the lower outlet of the iron-titanium mixing tank is connected to the iron source metering tank through the iron-titanium mixed liquid delivery pump, and the bottom outlet of the iron source metering tank is connected to the synthesis reactor;

[0006] A phosphate ammonium warehouse is arranged above the phosphorus source dissolving tank, a discharge pipe at the bottom of the phosphate ammonium warehouse is connected to the phosphorus source dissolving tank, a lower outlet of the phosphorus source dissolving tank is connected to the phosphorus source reactor via a phosphorus source dissolving liquid delivery pump, an ammonia water tank and an oxidant metering tank are arranged above the phosphorus source reactor, the bottom outlets of the ammonia water tank and the oxidant metering tank are connected to the phosphorus source reactor, the bottom outlet of the phosphorus source reactor is connected to the phosphorus source metering tank via a phosphorus source delivery pump, and the bottom outlet of the phosphorus source metering tank is connected to the synthesis reactor;

[0007] The bottom outlet of the synthesis reactor is connected to the second filter press through a synthesis slurry delivery pump, the solid outlet of the second filter press is connected to the aging reactor through a first belt conveyor, a phosphoric acid metering tank is arranged above the aging reactor, the bottom discharge pipe of the phosphoric acid metering tank is connected to the aging reactor, the bottom outlet of the aging reactor is connected to the third filter press through an aging slurry delivery pump, the solid outlet of the third filter press is connected to a flash dryer through a second belt conveyor, and the outlet of the flash dryer is connected to a kiln.

[0008] The ferrous warehouse, titanium source metering tank, ammonium phosphate warehouse, oxidant metering tank, phosphorus source metering tank, iron source metering tank, and phosphoric acid metering tank are all installed on their respective weighing devices, and the signal output end of the weighing device is correspondingly connected to the signal input end of the controller.

[0009] The iron source dissolving tank, iron-titanium mixing tank, phosphorus source dissolving tank, phosphorus source reactor, synthesis reactor and aging reactor are all equipped with stirring devices, and the control input end of the stirring device is correspondingly connected to the control output end of the controller.

[0010] The iron source dissolving tank, the phosphorus source dissolving tank and the aging reactor are respectively connected to desalted water pipelines equipped with flow meters, and the signal output ends of the flow meters are correspondingly connected to the signal input ends of the controller.

[0011] The iron source dissolution tank and the phosphorus source reactor are respectively provided with pH meters, and the aging reactor is provided with a thermometer and a pH meter. The signal output ends of the thermometer and the pH meter are correspondingly connected to the signal input end of the controller.

[0012] The outer periphery of the aging reactor is provided with a steam heating pipe or an immersed coil heat exchanger.

[0013] The controller is a DCS controller or a PLC controller.

[0014] The beneficial effects of the present invention are: reasonable layout, fully automated monitoring and control, which can effectively reduce the use of pH regulators, reduce the generation of impurity by-products, reduce energy consumption and wastewater generation, ensure stable production operation and improve product quality, and meet the technical requirements of energy conservation and consumption reduction. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of the present utility model.

[0016] In the figure: 1- iron source dissolution tank, 2- first filter press, 3- iron source clear liquid storage tank, 4- iron-titanium mixing tank, 5- phosphorus source dissolution tank, 6- phosphorus source reactor, 7- synthesis reactor, 8- second filter press, 9- aging reactor, 10- third filter press, 11- flash dryer, 12- kiln;

[0017] A1- ferrous iron tank, A2- regulating tank, A3- titanium source metering tank, A4- ammonium phosphate tank, A5- ammonia water tank, A6- oxidant metering tank, A7- phosphorus source metering tank, A8- iron source metering tank, A9- phosphoric acid metering tank;

[0018] B1- iron source slurry delivery pump, B2- iron source clear liquid delivery pump, B3- iron-titanium mixed liquid delivery pump, B4- phosphorus source dissolved liquid delivery pump, B5- phosphorus source delivery pump, B6- synthetic slurry delivery pump, B7- aged slurry delivery pump; C1- first belt conveyor, C2- second belt conveyor. DETAILED DESCRIPTION

[0019] The present invention is further described below in conjunction with the accompanying drawings: A device for producing battery-grade titanium-doped ferric phosphate: a ferrous bin A1 and a regulating tank A2 are arranged above the iron source dissolving tank 1, and the bottom discharge pipes of the ferrous bin A1 and the regulating tank A2 are connected to the iron source dissolving tank 1, and the lower outlet of the iron source dissolving tank 1 is connected to the feed port of the first filter press 2 through the iron source slurry delivery pump B1, and the liquid outlet of the first filter press 2 is connected to the iron source clear liquid storage tank 3, and the lower outlet of the iron source clear liquid storage tank 3 is connected to the iron-titanium mixing tank 4 through the iron source clear liquid delivery pump B2, and a titanium source metering tank A3 is arranged above the iron-titanium mixing tank 4, and the bottom discharge pipe of the titanium source metering tank A3 is connected to the iron-titanium mixing tank 4, and the lower outlet of the iron-titanium mixing tank 4 is connected to the iron source metering tank A8 through the iron-titanium mixed liquid delivery pump B3, and the bottom outlet of the iron source metering tank A8 is connected to the synthesis reactor 7;

[0020] A phosphate ammonium warehouse A4 is arranged above the phosphorus source dissolving tank 5, and a discharge pipe at the bottom of the phosphate ammonium warehouse A4 is connected to the phosphorus source dissolving tank 5. The lower outlet of the phosphorus source dissolving tank 5 is connected to the phosphorus source reactor 6 through a phosphorus source solution delivery pump B4. An ammonia water tank A5 and an oxidant metering tank A6 are arranged above the phosphorus source reactor 6. The bottom outlets of the ammonia water tank A5 and the oxidant metering tank A6 are connected to the phosphorus source reactor 6. The bottom outlet of the phosphorus source reactor 6 is connected to the phosphorus source metering tank A7 through a phosphorus source delivery pump B5. The bottom outlet of the phosphorus source metering tank A7 is connected to the synthesis reactor 7;

[0021] The bottom outlet of the synthesis reactor 7 is connected to the second filter press 8 through the synthesis slurry delivery pump B6, and the solid outlet of the second filter press 8 is connected to the aging reactor 9 through the first belt conveyor C1. A phosphoric acid metering tank A9 is arranged above the aging reactor 9, and the bottom discharge pipe of the phosphoric acid metering tank A9 is connected to the aging reactor 9; the bottom outlet of the aging reactor 9 is connected to the third filter press 10 through the aging slurry delivery pump B7, and the solid outlet of the third filter press 10 is connected to the flash dryer 11 through the second belt conveyor C2, and the outlet of the flash dryer 11 is connected to the kiln 12.

[0022] The ferrous warehouse A1, titanium source metering tank A3, ammonium phosphate warehouse A4, oxidant metering tank A6, phosphorus source metering tank A7, iron source metering tank A8, and phosphoric acid metering tank A9 are all installed on their respective weighing devices, and the signal output end of the weighing device is correspondingly connected to the signal input end of the controller.

[0023] The iron source dissolving tank 1, the iron-titanium mixing tank 4, the phosphorus source dissolving tank 5, the phosphorus source reactor 6, the synthesis reactor 7 and the aging reactor 9 are all equipped with a stirring device, and the control input end of the stirring device is correspondingly connected to the control output end of the controller.

[0024] The iron source dissolving tank 1, the phosphorus source dissolving tank 5 and the aging reactor 9 are respectively connected to desalted water pipelines equipped with flow meters, and the signal output ends of the flow meters are correspondingly connected to the signal input ends of the controller.

[0025] The iron source dissolving tank 1 and the phosphorus source reactor 6 are respectively provided with pH meters, and the aging reactor 9 is provided with a thermometer and a pH meter. The signal output ends of the thermometer and the pH meter are correspondingly connected to the signal input end of the controller.

[0026] The aging reactor 9 is provided with a steam heating pipe or an immersed coil heat exchanger on the periphery thereof.

[0027] The controller is a DCS controller or a PLC controller.

[0028] The iron source dissolution tank 1, iron source clear liquid storage tank 3, iron-titanium mixing tank 4, phosphorus source dissolution tank 5, phosphorus source reactor 6, synthesis reactor 7, aging reactor 9, ferrous warehouse A1, ammonium phosphate warehouse A4, regulating tank A2, ammonia water tank A5, oxidant metering tank A6, titanium source metering tank A3, phosphorus source metering tank A7, iron source metering tank A8, and phosphoric acid metering tank A9 are installed with necessary level measuring instruments.

[0029] Necessary pressure measuring instruments are installed on the outlet pipes of the iron source slurry delivery pump B1, iron source clear liquid delivery pump B2, iron-titanium mixed liquid delivery pump B3, phosphorus source dissolved liquid delivery pump B4, phosphorus source delivery pump B5, synthetic slurry delivery pump B6, and aged slurry delivery pump B7.

[0030] The stirring devices installed on the synthesis reactor 7 and the aging reactor 9 are controlled by frequency converters, which facilitates the controller to change the rotation speed by frequency adjustment, thereby realizing the rotation speed control of the stirring paddle during the reaction.

[0031] Working process:

[0032] Step 1: Add a certain amount of desalted water to the iron source dissolving tank 1 through the desalted water pipeline. The amount of water added can be measured by a flow meter installed on the desalted water pipeline, and then turn on the stirring device. Place solid ferrous sulfate heptahydrate as a raw material in the ferrous bin A1, weigh it through a weighing device and add it to the iron source dissolving tank 1 to obtain a ferrous sulfate solution. After the dissolution is completed, add a pH regulator to the iron source dissolving tank 1 through the regulating tank A2, and use a pH meter to monitor and control the amount of pH regulator added to make the pH value of the solution between 3-6. At this time, the impurities in the ferrous sulfate solution begin to precipitate and ferrous sulfate slurry is obtained;

[0033] Step 2: The ferrous sulfate slurry is transported to the first filter press 2 through the iron source slurry delivery pump B1 for filtration treatment. The mother liquor squeezed out is the ferrous sulfate clear liquid, which is collected into the iron source clear liquid storage tank 3 for storage;

[0034] Step 3: The ferrous sulfate clear liquid is transferred to the iron-titanium mixing tank 4 through the iron source clear liquid delivery pump B2, and stirring is started. At the same time, a certain weight of titanium dopant is slowly added into the iron-titanium mixing tank 4 through the titanium source metering tank A3 installed on the weighing device. After mixing evenly, an iron-titanium mixed liquid is obtained, and the iron-titanium mixed liquid is transferred to the iron source metering tank A8 through the iron-titanium mixed liquid delivery pump B3;

[0035] Step 4: Add a certain amount of desalted water to the phosphorus source dissolution tank 5 through the desalted water pipeline. The amount of water added can be measured by a flow meter installed on the desalted water pipeline. Then, turn on the stirring device. Place solid ammonium phosphate as the raw material in the ammonium phosphate tank A4, weigh it using a weighing device, and add it to the phosphorus source dissolution tank 5 to obtain an ammonium phosphate solution.

[0036] Step 5: The ammonium phosphate solution is transferred to the phosphorus source reactor 6 through the phosphorus source dissolving liquid delivery pump B4, the stirring device is turned on, and a certain amount of ammonia water is slowly added to the phosphorus source reactor 6 through the ammonia water tank A5. The amount of ammonia water added is monitored and controlled by the pH meter installed on the phosphorus source reactor 6 to make the pH value of the solution between 7 and 8. Hydrogen peroxide is slowly added to the phosphorus source reactor 6 through the oxidant metering tank A6 installed on the weighing device. After mixing, a phosphorus source mixed solution is obtained, and the phosphorus source mixed solution is transferred to the phosphorus source metering tank A7 through the phosphorus source delivery pump B5;

[0037] Step 6: Add a certain weight of iron-titanium mixed liquid to the synthesis reactor 7 through the iron source metering tank A8, turn on the stirring device, and then slowly add a certain weight of phosphorus source mixed liquid to the synthesis reactor 7 through the phosphorus source metering tank A7. After sufficient reaction, a yellow synthetic slurry is obtained;

[0038] Step 7: The synthetic slurry is delivered to the second filter press 6 through the synthetic slurry delivery pump B6 for squeezing, and the filter cake after squeezing is washed with desalted water. Whether the washing is qualified can be judged by the conductivity. After the washing is qualified, the titanium-doped basic ferric phosphate filter cake is obtained;

[0039] Step 8: Add a certain amount of desalted water to the aging reactor 9 through the desalted water pipeline, turn on the agitator, and move the titanium-doped basic ferric phosphate filter cake to the aging reactor 9 through the first belt conveyor C1. Add a certain amount of phosphoric acid to the aging reactor 9 through the phosphoric acid metering tank A9, monitor the pH value of the material with a pH meter to ensure that the reaction pH is around 2, heat the aging reactor 9 through a steam heating pipe, and detect the temperature of the material with a thermometer to ensure that the reaction temperature is between 70-90 degrees. After the reaction is completed, titanium-doped ferric phosphate dihydrate slurry is obtained;

[0040] Step 9: The titanium-doped ferric phosphate dihydrate slurry is delivered to the third filter press 10 through the aged slurry delivery pump B7 for squeezing, and the filter cake is washed with desalted water. Whether the washing is qualified can be judged by the conductivity; after the washing is qualified, the titanium-doped ferric phosphate dihydrate is obtained;

[0041] Step 10: The titanium-doped ferric phosphate dihydrate is moved to the flash dryer 11 through the second belt conveyor C2 for drying to remove free water and obtain titanium-doped ferric phosphate dihydrate; the dried and dehydrated titanium-doped ferric phosphate dihydrate is transported to the kiln 12 for calcination to remove crystallization water and obtain the finished titanium-doped ferric phosphate product.

[0042] The above embodiments are only preferred embodiments of the present invention and are not limitations on the technical solutions of the present invention. Any technical solution that can be implemented on the basis of the above embodiments without creative work should be deemed to fall within the scope of protection of the patent of the present invention.

Claims

1. A device for producing battery-grade titanium-doped iron phosphate, characterized in that: A ferrous bin (A1) and a regulating tank (A2) are provided above the iron source dissolving tank (1); the bottom discharge pipes of the ferrous bin (A1) and the regulating tank (A2) are connected to the iron source dissolving tank (1); the lower outlet of the iron source dissolving tank (1) is connected to the feed port of the first filter press (2) via an iron source slurry delivery pump (B1); the liquid outlet of the first filter press (2) is connected to the iron source clear liquid storage tank (3); the lower outlet of the iron source clear liquid storage tank (3) is connected to the iron-titanium mixing tank (4) via an iron source clear liquid delivery pump (B2); a titanium source metering tank (A3) is provided above the iron-titanium mixing tank (4); the bottom discharge pipe of the titanium source metering tank (A3) is connected to the iron-titanium mixing tank (4); the lower outlet of the iron-titanium mixing tank (4) is connected to the iron source metering tank (A8) via an iron-titanium mixed liquid delivery pump (B3); and the bottom outlet of the iron source metering tank (A8) is connected to the synthesis reactor (7); A phosphate ammonium bin (A4) is provided above the phosphorus source dissolving tank (5), a discharge pipe at the bottom of the phosphate ammonium bin (A4) is connected to the phosphorus source dissolving tank (5), a lower outlet of the phosphorus source dissolving tank (5) is connected to the phosphorus source reactor (6) via a phosphorus source dissolving liquid delivery pump (B4), an ammonia water tank (A5) and an oxidant metering tank (A6) are provided above the phosphorus source reactor (6), the bottom outlets of the ammonia water tank (A5) and the oxidant metering tank (A6) are connected to the phosphorus source reactor (6), the bottom outlet of the phosphorus source reactor (6) is connected to the phosphorus source metering tank (A7) via a phosphorus source delivery pump (B5), and the bottom outlet of the phosphorus source metering tank (A7) is connected to the synthesis reactor (7); The bottom outlet of the synthesis reactor (7) is connected to the second filter press (8) via a synthesis slurry delivery pump (B6), the solid outlet of the second filter press (8) is connected to the aging reactor (9) via a first belt conveyor (C1), a phosphoric acid metering tank (A9) is arranged above the aging reactor (9), the bottom discharge pipe of the phosphoric acid metering tank (A9) is connected to the aging reactor (9), the bottom outlet of the aging reactor (9) is connected to the third filter press (10) via an aging slurry delivery pump (B7), the solid outlet of the third filter press (10) is connected to a flash dryer (11) via a second belt conveyor (C2), and the outlet of the flash dryer (11) is connected to a kiln (12).

2. The device for producing battery-grade titanium-doped ferric phosphate according to claim 1, characterized in that: The ferrous iron bin (A1), titanium source metering tank (A3), ammonium phosphate bin (A4), oxidant metering tank (A6), phosphorus source metering tank (A7), iron source metering tank (A8), and phosphoric acid metering tank (A9) are all installed on respective weighing devices, and the signal output end of the weighing device is correspondingly connected to the signal input end of the controller.

3. The device for producing battery-grade titanium-doped ferric phosphate according to claim 1, characterized in that: The iron source dissolving tank (1), the iron-titanium mixing tank (4), the phosphorus source dissolving tank (5), the phosphorus source reactor (6), the synthesis reactor (7) and the aging reactor (9) are all equipped with stirring devices, and the control input end of the stirring device is correspondingly connected to the control output end of the controller.

4. The device for producing battery-grade titanium-doped ferric phosphate according to claim 1, characterized in that: The iron source dissolving tank (1), the phosphorus source dissolving tank (5) and the aging reactor (9) are respectively connected to desalted water pipelines equipped with flow meters, and the signal output ends of the flow meters are correspondingly connected to the signal input ends of the controller.

5. The device for producing battery-grade titanium-doped ferric phosphate according to claim 1, characterized in that: The iron source dissolving tank (1) and the phosphorus source reactor (6) are respectively provided with a pH meter, and the aging reactor (9) is provided with a thermometer and a pH meter. The signal output ends of the thermometer and the pH meter are correspondingly connected to the signal input end of the controller.

6. The device for producing battery-grade titanium-doped ferric phosphate according to claim 1, characterized in that: The aging reactor (9) is provided with a steam heating pipe or an immersed coil heat exchanger on the periphery thereof.

7. The device for producing battery-grade titanium-doped ferric phosphate according to any one of claims 2, 3, 4, and 5, characterized in that: The controller is a DCS controller or a PLC controller.

Images