Continuous carbonization device

Abstract

The invention discloses a continuous carbonization device which comprises a shell, a reactor, a reaction kettle and a complete set of automatic control station, the reactor is connected with a first feeding pipe and a second feeding pipe, and the reactor is connected with the reaction kettle through a discharging pipe; a first adjusting valve, a first feeding pump, a first check valve, a first flow meter and a first pressure transmitter are sequentially installed on the pipe section of the first feeding pipe, and a second adjusting valve, a second flow meter, a second check valve and a second pressure transmitter are sequentially installed on the pipe section of the second feeding pipe. And a third pressure transmitter and a temperature transmitter are sequentially mounted on the pipe section of the discharge pipe. The device is simpler to operate, high in efficiency, automatic in control and high in raw material utilization rate.

Description

Technical Field

[0001] The invention relates to the technical field of carbonization devices, and in particular to a continuous carbonization device. Background Art

[0002] Lithium carbonate is an important raw material for lithium battery manufacturing. Improving its purity plays a key role in improving battery performance and stability. In the process of purifying industrial-grade lithium carbonate to prepare battery-grade lithium carbonate, it is necessary to form an intermediate product, lithium bicarbonate, and remove impurities and purify it. The purified lithium bicarbonate solution decomposes under heating conditions to release carbon dioxide and water, and high-purity lithium carbonate is precipitated. The solid-liquid separation, washing and drying are then performed to obtain battery-grade lithium carbonate crystals.

[0003] At present, the traditional preparation of lithium bicarbonate uses a four-step carbonization tower technology, which requires a reaction time of more than 2 hours and has a relatively low efficiency. In addition, during the reaction, carbon dioxide is introduced in excess, which will cause a lot of waste in production. To solve this problem, we propose a continuous carbonization device to solve this problem. Summary of the invention

[0004] The purpose of the present invention is to solve the shortcomings of the prior art and to propose a continuous carbonization device.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions: A continuous carbonization device comprises a shell, a reactor, a reaction kettle, and a complete set of automatic control stations. The reactor is connected to a first feed pipe and a second feed pipe. The reactor is connected to the reaction kettle through a discharge pipe. A first regulating valve, a first feed pump, a first check valve, a first flow meter, and a first pressure transmitter are sequentially installed on the pipe section of the first feed pipe. A second regulating valve, a second flow meter, a second check valve, and a second pressure transmitter are sequentially installed on the pipe section of the second feed pipe. A third pressure transmitter and a temperature transmitter are sequentially installed on the pipe section of the discharge pipe.

[0006] Preferably, the reactor is installed inside the shell, and the complete set of automatic control stations is installed on the outer surface of the shell.

[0007] Preferably, the first regulating valve is a liquid regulating valve, the first flow meter is a liquid flow meter, the first pressure transmitter is a liquid pressure transmitter, the third pressure transmitter is a liquid pressure transmitter, and the temperature transmitter is a liquid temperature transmitter.

[0008] Preferably, the reactor is a variable frequency gas-liquid reactor, the second regulating valve is a gas regulating valve, the second flow meter is a gas flow meter, and the second pressure transmitter is a gas pressure transmitter.

[0009] Preferably, the reactor is a variable frequency liquid phase reactor, the second regulating valve is a liquid regulating valve, the second flow meter is a liquid flow meter, the second pressure transmitter is a liquid pressure transmitter, a second feed pump is installed on the pipe section of the second feed pipe, and the second feed pump is located between the second regulating valve and the second flow meter.

[0010] Compared with the prior art, the present invention has the following beneficial effects: 1. In the present invention, the reactor is provided with a multi-stage reaction element, which can control the radial uniform distribution of carbon dioxide gas in the reaction vessel, and drive the lithium carbonate slurry to turbulently move at a high speed in the reactor, so as to promote the rapid reaction of lithium carbonate and carbon dioxide molecules to generate a clear lithium bicarbonate solution; the one-step carbonization method of electrocarbon is realized, and the reaction time is greatly shortened, which greatly improves the production efficiency compared with the reaction time of more than 2 hours of the traditional four-step carbonization tower technology; by controlling the injection and quality of carbon dioxide gas, the precise proportional addition control of carbon dioxide gas is realized, and the maximum amount of carbon dioxide gas in the reactor is guaranteed to react, the utilization rate of carbon dioxide is improved, and the escape of carbon dioxide is reduced. Compared with the carbon dioxide consumption of several times of the traditional carbonization tower, the consumption cost of carbon dioxide is greatly reduced, the carbonization rate is improved, and the full utilization of lithium carbonate is guaranteed relative to the traditional carbonization tower; 2. In the present invention, the reactor is provided with a multi-stage reaction element, which can control the uniform distribution of various lithium solutions and sodium carbonate solutions for lithium precipitation in the reaction vessel, and drive the lithium carbonate seed mixed slurry to turbulently move at a high speed in the reactor, accelerate the lithium precipitation reaction and control the crystal particle size, reduce the existence of lithium precipitation peritectic, ensure the elution and stirring of subsequent products to remove impurities, and obtain high-purity products; similarly, for multi-phase liquid solutions, it can ensure that each component is quickly stirred and mixed according to the distribution ratio and sent out of the continuous reaction system; the continuous carbonization and lithium precipitation of lithium solutions is realized, and the reaction time is greatly shortened. Compared with the traditional lithium precipitation reaction, the production efficiency is greatly improved, and at the same time, the number of production supporting reactors can be reduced, the system area can be reduced, and the investment can be reduced; the excess carbonate content can be reduced, the amount of sodium carbonate used for lithium precipitation can be reduced, and the amount of by-product frozen nitrate in the mother liquor can be reduced, which saves energy and consumption; 3. In the present invention, the complete set of automatic control stations can control the mixing ratio according to demand, and can also realize the liquid phase continuous reaction crystallization process. A set of equipment has multiple process uses and can adapt to the application of multiple working conditions. It has a high degree of intelligence, improves the overall production efficiency, and reduces production costs and labor costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 This is a flow chart of Embodiment 1 of the present invention; Figure 2 This is a flow chart of Embodiment 2 of the present invention.

[0012] In the figure: 1 first regulating valve, 2 first feeding pump, 3 first flow meter, 4 first pressure transmitter, 5 second regulating valve, 6 second flow meter, 7 second pressure transmitter, 8 reactor, 9 third pressure transmitter, 10 temperature transmitter, 11 reactor, 12 shell, 13 complete automatic control station, 14 first check valve, 15 second check valve, 16 second feeding pump. DETAILED DESCRIPTION

[0013] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0014] A continuous carbonization device comprises a shell 12, a reactor 8, a reactor 11, and a complete set of automatic control stations 13. The reactor 8 is connected to a first feed pipe and a second feed pipe. The reactor 8 is connected to the reactor 11 through a discharge pipe. A first regulating valve 1, a first feed pump 2, a first check valve 14, a first flow meter 3, and a first pressure transmitter 4 are sequentially installed on the pipe section of the first feed pipe. A second regulating valve 5, a second flow meter 6, a second check valve 15, and a second pressure transmitter 7 are sequentially installed on the pipe section of the second feed pipe. A third pressure transmitter 9 and a temperature transmitter 10 are sequentially installed on the pipe section of the discharge pipe. The reactor 8 is installed inside the shell 12, and the complete set of automatic control stations 13 is installed on the outer surface of the shell 12 for easy control and observation. The first regulating valve 1 is a liquid regulating valve, the first flow meter 3 is a liquid flow meter, the first pressure transmitter 4 is a liquid pressure transmitter, the third pressure transmitter 9 is a liquid pressure transmitter, and the temperature transmitter 10 is a liquid temperature transmitter. Example 1

[0015] Reference Figure 1 The reactor 8 is a variable frequency gas-liquid reactor, the second regulating valve 5 is a gas regulating valve, the second flow meter 6 is a gas flow meter, and the second pressure transmitter 7 is a gas pressure transmitter.

[0016] In this embodiment, the following steps are included: S1, solid lithium carbonate and pure water are fully dissolved in a dissolving and mixing system to form a uniform lithium carbonate slurry, and the lithium carbonate slurry is transported to a reactor 8 through a first feed pump 2, and a first check valve 14 can prevent the lithium carbonate slurry from flowing back; S2. During the transportation of lithium carbonate slurry, the first flow meter 3 measures the flow rate of lithium carbonate slurry, the first pressure transmitter 4 measures the pressure of lithium carbonate slurry, and transmits the flow signal and the pressure signal to the complete set of automatic control station 13. After receiving the flow signal and the pressure signal of lithium carbonate slurry, the complete set of automatic control station 13 automatically and accurately adds carbon dioxide gas to the reactor 8 in proportion. During the transportation of carbon dioxide gas, the second flow meter 6 measures the flow rate of carbon dioxide gas, the second pressure transmitter 7 measures the pressure of carbon dioxide gas, and the second check valve 15 can prevent the backflow of carbon dioxide gas; S3, the reactor 8 shears the lithium carbonate slurry, thereby reducing the diameter of the lithium carbonate particles, and quickly disperses the carbon dioxide gas, accelerating the reaction speed, and finally generating a clear lithium bicarbonate solution, and the solution is transported to the reactor 11. The insoluble impurity salts mixed in the reactor 11 are separated by filtration, thereby achieving the goal of carbonization. The reactor 8 can control the radial uniform distribution of the carbon dioxide gas in the reaction vessel, and drive the lithium carbonate slurry to turbulently at a high speed in the reactor, so as to promote the rapid reaction of lithium carbonate and carbon dioxide molecules to generate a clear lithium bicarbonate solution.

[0017] Reactor 8 is provided with a multi-stage reaction element, which can control the radial uniform distribution of carbon dioxide gas in the reaction vessel, and drive the lithium carbonate slurry to turbulently at a high speed in the reactor, so as to promote the rapid reaction of lithium carbonate and carbon dioxide molecules to generate a clear lithium bicarbonate solution; the one-step carbonization method of electrocarbon is realized, and the reaction time is greatly shortened, which greatly improves the production efficiency compared with the traditional four-step carbonization tower technology with a reaction time of more than 2 hours; through the control of carbon dioxide gas injection and quality, the precise proportional addition control of carbon dioxide gas is realized, which ensures that the maximum amount of carbon dioxide gas reacts in the reactor, improves the utilization rate of carbon dioxide, reduces the escape of carbon dioxide, and greatly reduces the consumption cost of carbon dioxide and improves the carbonization rate compared with the traditional carbonization tower with several times the carbon dioxide consumption. Compared with the traditional carbonization tower, the full utilization of lithium carbonate is guaranteed. Example 2

[0018] Reference Figure 2 The reactor 8 is a variable frequency liquid phase reactor, the second regulating valve 5 is a liquid regulating valve, the second flow meter 6 is a liquid flow meter, the second pressure transmitter 7 is a liquid pressure transmitter, and a second feed pump 16 is installed on the pipe section of the second feed pipe. The second feed pump 16 is located between the second regulating valve 5 and the second flow meter 6.

[0019] In this embodiment, the following steps are included: S1. The first solution produced by various processes such as lithium extraction from ore, lithium extraction from salt lakes, and battery recycling (the first solution is a pure lithium salt solution, such as lithium sulfate solution, lithium chloride solution, lithium nitrate solution, etc.) is preheated to a target temperature of 70-80°C in a storage kettle according to the lithium precipitation process, and is transported to the reactor 8 through the outlet of the storage kettle in sequence through the first regulating valve 1, the first feeding pump 2, and the first check valve 14. At the same time, a second solution (the second solution is 290-300g / l soda ash sodium carbonate solution, sodium hydroxide solution, or lithium precipitation mother liquor, etc.) is prepared, purified, and preheated to a target temperature of 70-80°C. According to the set target flow value, the second solution is accurately added to the reactor 8 through the second regulating valve 5, the second feeding pump 16, and the second check valve 15; S2. During the delivery of the first solution, the first flowmeter 3 measures the flow of the first solution, the first pressure transmitter 4 measures the supply pressure of the first solution, and transmits the flow signal and the pressure signal to the complete set of automatic control station 13. During the delivery of the second solution, the second flowmeter 6 measures the flow of the second solution, the second pressure transmitter 7 measures the pressure of the second solution, and transmits the measured flow signal and the pressure signal of the second solution to the complete set of automatic control station 13. After receiving the flow signal and the pressure signal of the first solution and the second solution, the complete set of automatic control station 13 performs liquid phase continuous reaction and continuously delivers the slurry after the reaction in combination with the system setting operation parameters. When the delivered slurry enters the reactor 11, the third pressure transmitter 9 and the temperature transmitter 10 detect the pressure and temperature indicators of the liquid after the actual reaction, and send the signals to the complete set of automatic control station 13 for storage and record; S3, reactor 8 performs particle size refinement shearing and high-speed stirring and breaking on the lithium carbonate slurry produced by the continuous reaction of lithium precipitation, so as to control the particle size of lithium carbonate particles. This process simultaneously quickly disperses the reaction components in the liquid-liquid two phases, expands the contact ratio of molecules or ions, accelerates the reaction rate, and combines lithium ions with carbonate ions to form lithium carbonate with low solubility and precipitate crystals. Finally, a slurry after lithium precipitation is obtained, and the slurry is transported to the reactor 11. The precipitated lithium carbonate crystals and unreacted excess sodium carbonate, water, etc. are mixed in the reactor 11. The target product lithium carbonate is obtained after centrifugal filtration and separation. The mother liquor and washing water are returned to the batching and beating system according to the design, or concentrated and frozen to crystallize and precipitate sodium sulfate, so as to achieve the goal of reacting lithium sulfate and sodium carbonate to produce carbon lithium and produce sodium sulfate as a by-product.

[0020] Reactor 8 is provided with a multi-stage reaction element, which can control the uniform distribution of various lithium solutions and sodium carbonate solutions for lithium precipitation in the reaction vessel, and drive the lithium carbonate seed mixed slurry to turbulently at high speed in the reactor, accelerate the lithium precipitation reaction and crystal particle size control, reduce the existence of lithium precipitation peritectic, ensure the elution and stirring of subsequent products to obtain high-purity products; similarly, for multi-phase liquid solutions, it can ensure that the incoming liquid of each component is quickly stirred and mixed according to the distribution ratio and sent out of the continuous reaction system; the continuous carbonization and lithium precipitation of lithium-lithium solutions is realized, and the reaction time is greatly shortened. Compared with the traditional lithium precipitation reaction, the production efficiency is greatly improved. At the same time, the number of production supporting reactors can be reduced, the system area can be reduced, and the investment can be reduced; the excess carbonate content can be reduced, the amount of sodium carbonate used for lithium precipitation can be reduced, and the amount of by-product frozen nitrate in the mother liquor can be reduced, saving energy and consumption.

[0021] The complete set of automatic control station 13 can control the mixing ratio according to demand, and can also realize the liquid phase continuous reaction crystallization process. A set of equipment has multiple process uses and can adapt to the application of multiple working conditions. It has a high degree of intelligence, improves the overall production efficiency, and reduces production costs and labor costs.

[0022] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A continuous carbonization device, comprising a housing (12), a reactor (8), a reaction kettle (11), and a complete set of automatic control stations (13), characterized in that: The reactor (8) is connected to a first feed pipe and a second feed pipe. The reactor (8) is connected to a reaction kettle (11) via a discharge pipe. A first regulating valve (1), a first feed pump (2), a first check valve (14), a first flow meter (3), and a first pressure transmitter (4) are sequentially installed on a pipe section of the first feed pipe. A second regulating valve (5), a second flow meter (6), a second check valve (15), and a second pressure transmitter (7) are sequentially installed on a pipe section of the second feed pipe. A third pressure transmitter (9) and a temperature transmitter (10) are sequentially installed on a pipe section of the discharge pipe.

2. A continuous carbonization device according to claim 1, characterized in that: The reactor (8) is installed inside the shell (12), and the complete set of automatic control stations (13) is installed on the outer surface of the shell (12).

3. A continuous carbonization device according to claim 1, characterized in that: The first regulating valve (1) is a liquid regulating valve, the first flow meter (3) is a liquid flow meter, the first pressure transmitter (4) is a liquid pressure transmitter, the third pressure transmitter (9) is a liquid pressure transmitter, and the temperature transmitter (10) is a liquid temperature transmitter.

4. A continuous carbonization device according to claim 3, characterized in that: The reactor (8) is a variable frequency gas-liquid reactor, the second regulating valve (5) is a gas regulating valve, the second flow meter (6) is a gas flow meter, and the second pressure transmitter (7) is a gas pressure transmitter.

5. A continuous carbonization device according to claim 3, characterized in that: The reactor (8) is a variable frequency liquid phase reactor, the second regulating valve (5) is a liquid regulating valve, the second flow meter (6) is a liquid flow meter, the second pressure transmitter (7) is a liquid pressure transmitter, and a second feed pump (16) is installed on the pipe section of the second feed pipe, and the second feed pump (16) is located between the second regulating valve (5) and the second flow meter (6).

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