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CN-121972103-A - Preparation system and preparation method of battery-grade lithium carbonate

CN121972103ACN 121972103 ACN121972103 ACN 121972103ACN-121972103-A

Abstract

The application relates to the technical field of preparation processes of battery-grade lithium carbonate and discloses a preparation system and a preparation method of the battery-grade lithium carbonate, wherein the preparation system of the battery-grade lithium carbonate comprises a beating tank, a homogenizing pump, a first reactor, a carbonization buffer tank, a first circulating pump, a filter, an ion exchange device, a conveying pump, a second reactor, a slurry buffer tank, a second circulating pump and post-treatment equipment which are sequentially connected through a main pipeline, wherein a first proportional regulating valve is arranged between the homogenizing pump and the first reactor, the first proportional regulating valve is connected with the beating tank through a first return pipeline, a second proportional regulating valve is arranged between the first circulating pump and the filter, the second proportional regulating valve is connected with the first reactor through a second return pipeline, a third proportional regulating valve is arranged between the second circulating pump and the post-treatment equipment, and the third proportional regulating valve is connected with the second reactor through a third return pipeline. The application simplifies the preparation process, reduces the use cost and improves the preparation efficiency.

Inventors

  • YANG CHUNXIA

Assignees

  • 万华化学集团电池科技有限公司
  • 万华化学(烟台)电池产业有限公司
  • 万华化学(烟台)电池材料科技有限公司

Dates

Publication Date
20260505
Application Date
20241028

Claims (10)

  1. 1. The utility model provides a preparation system of battery grade lithium carbonate, its characterized in that, including beating jar (1), homogeneity pump (2), first reactor (3), carbonization buffer tank (4), first circulating pump (5), filter (6), ion exchange device (7), delivery pump (8), second reactor (9), thick liquid buffer tank (10), second circulating pump (11) and aftertreatment equipment (12) that connect gradually through the main line, homogeneity pump (2) with be equipped with first proportional control valve (13) on the pipeline between first reactor (3), first proportional control valve (13) through first return line (14) with beating jar (1) are connected, be equipped with second proportional control valve (15) on the pipeline between first circulating pump (5) with filter (6), second proportional control valve (15) through second return line (16) with first reactor (3) are connected, be equipped with third proportional control valve (17) on second circulating pump (11) with aftertreatment equipment (12) are equipped with third proportional control valve (17) on the pipeline between third return line (17).
  2. 2. The system for preparing the battery-grade lithium carbonate according to claim 1, characterized in that a first buffer tank (20) is arranged on a pipeline between the second proportional control valve (15) and the filter (6), and a second buffer tank (21) is arranged on a pipeline between the ion exchange device (7) and the delivery pump (8).
  3. 3. The system for preparing the battery grade lithium carbonate according to claim 2, characterized in that a heat exchanger (19) is further arranged on the third return line (18), and a preheater (22) is arranged on the line between the transfer pump (8) and the second reactor (9).
  4. 4. A system for preparing lithium carbonate of battery grade according to any of claims 1 to 3, characterized in that the post-treatment device (12) comprises a centrifuge (1201) and a drier (1202), the second circulation pump (11) being connected in sequence with the centrifuge (1201) and the drier (1202) through the main pipe.
  5. 5. A method for producing battery grade lithium carbonate, characterized by using the battery grade lithium carbonate production system according to any one of claims 1 to 4, comprising: Preparing industrial grade lithium carbonate and water into slurry according to a first preset proportion, inputting the slurry into a beating tank (1), and primarily premixing the slurry in the beating tank (1); circulating the primarily premixed slurry between the pulping tank (1) and the homogenizing pump (2) according to preset time; the recycled slurry is returned to the pulping tank (1) and is input into the first reactor (3) according to a second preset proportion; The slurry input into the first reactor (3) is subjected to carbonization reaction when the reaction temperature, the reaction pressure and the reaction residence time meet the first preset conditions, so as to generate reaction liquid; Inputting the reaction liquid into a carbonization buffer tank (4) to obtain a lithium bicarbonate solution; Refluxing the lithium bicarbonate solution into the first reactor (3) according to a third preset proportion and filtering the solution by an input filter (6); inputting the filtered lithium bicarbonate solution into an ion exchange device (7) to adsorb calcium ions and magnesium ions in the lithium bicarbonate solution; inputting the adsorbed lithium bicarbonate solution into a second reactor (9), and performing pyrolysis reaction to generate pyrolysis slurry when the reaction temperature, the reaction pressure and the reaction residence time meet second preset conditions; inputting the pyrolysis slurry into a slurry buffer tank (10) to obtain lithium carbonate slurry; And refluxing the lithium carbonate slurry into the second reactor (9) according to a fourth preset proportion, and inputting the lithium carbonate slurry into post-treatment equipment (12) for filtering, washing and drying to obtain the battery-grade lithium carbonate.
  6. 6. The method for preparing battery grade lithium carbonate according to claim 5, wherein the preparing the industrial grade lithium carbonate and water into slurry according to a first preset ratio is performed in a beating tank (1), and preliminary premixing is performed in the beating tank (1), and comprises: Preparing industrial grade lithium carbonate and water into slurry according to a solid-liquid weight ratio of 1:20-1:30, inputting the slurry into a beating tank (1), and primarily premixing in the beating tank (1).
  7. 7. The method for preparing battery grade lithium carbonate according to claim 5, wherein the recirculating the recycled slurry to the beating tank (1) and into the first reactor (3) according to a second preset ratio comprises: And (3) refluxing the recycled slurry to the pulping tank (1) according to a reflux ratio of 50-90%, and inputting the rest slurry into the first reactor (3), wherein the reflux ratio is determined based on the mixing degree of the mixing water of the homogenizing pump (2) and lithium carbonate.
  8. 8. The method for preparing battery grade lithium carbonate according to claim 5, characterized in that refluxing the lithium bicarbonate solution into the first reactor (3) and filtering by an input filter (6) according to a third preset ratio comprises: refluxing the lithium bicarbonate solution into the first reactor (3) and filtering by an input filter (6) according to a third preset ratio of 10:1 to 80:1, wherein the third preset ratio is determined based on the reaction residence time of the first reactor (3).
  9. 9. The method for preparing battery grade lithium carbonate according to claim 5, wherein the step of refluxing the lithium carbonate slurry into the second reactor (9) according to a fourth preset ratio and inputting the solution into a post-treatment device (12) for filtration, washing and drying to obtain battery grade lithium carbonate comprises the steps of: And refluxing the lithium carbonate slurry into the second reactor (9) according to a fourth preset ratio of 5:1 to 20:1, and inputting the lithium carbonate slurry into post-treatment equipment (12) for filtering, washing and drying to obtain battery-grade lithium carbonate, wherein the fourth preset ratio is determined based on the reaction residence time of the second reactor (9).
  10. 10. The method according to claim 5, wherein the slurry fed to the first reactor (3) is subjected to a carbonization reaction to produce a reaction solution when the reaction temperature, the reaction pressure, and the reaction residence time satisfy a first preset condition, comprising: the slurry fed into the first reactor (3) is subjected to carbonization reaction at the reaction temperature of 15-40 ℃, the reaction pressure of 0.1-0.5 MPa and the reaction residence time of 10-60 min to generate reaction liquid; and/or, the absorbed lithium bicarbonate solution is input into a second reactor (9), and when the reaction temperature, the reaction pressure and the reaction residence time meet second preset conditions, a pyrolysis reaction is performed to generate pyrolysis slurry, which comprises the following steps: And (3) inputting the adsorbed lithium bicarbonate solution into a second reactor (9), and carrying out pyrolysis reaction under the conditions of the reaction temperature of 60-100 ℃, the reaction pressure of 0-0.05 MPa and the reaction residence time of 30-60 min to generate pyrolysis slurry.

Description

Preparation system and preparation method of battery-grade lithium carbonate Technical Field The application relates to the technical field of preparation processes of battery-grade lithium carbonate, in particular to a preparation system and a preparation method of battery-grade lithium carbonate. Background Lithium carbonate is an important lithium salt in lithium compounds, is an important raw material for preparing other lithium compounds and lithium alloys, and is widely applied to industries such as electronics, optical materials, ceramics, medicines and the like. In recent years, with the rapid development of new energy technologies, particularly in the lithium battery industry, the demand for high-quality lithium carbonate has increased. At present, the lithium carbonate purification process mainly comprises a carbonization method, an electrolysis method, an extraction method, an ion exchange method, an adsorption method and the like, wherein the carbonization method gradually becomes the main process for producing the lithium carbonate due to the characteristics of high reaction efficiency, simple process, strong operability, low cost, small pollution and the like. However, in the existing production process of battery-grade lithium carbonate, since multiple purification reactions are needed and the granularity of lithium carbonate is unevenly distributed before the reaction, the problems of numerous production equipment, longer production period, lower product quality and the like exist. Disclosure of Invention The application provides a preparation system and a preparation method of battery-grade lithium carbonate, which are used for solving the problems of the existing production process of the battery-grade lithium carbonate, such as a large number of production equipment, a long production period, low product quality and the like. In a first aspect, the application provides a preparation system of battery-grade lithium carbonate, which comprises a pulping tank, a homogenizing pump, a first reactor, a carbonization buffer tank, a first circulating pump, a filter, an ion exchange device, a delivery pump, a second reactor, a slurry buffer tank, a second circulating pump and post-treatment equipment which are sequentially connected through a main pipeline, wherein a first proportional regulating valve is arranged on a pipeline between the homogenizing pump and the first reactor, the first proportional regulating valve is connected with the pulping tank through a first return pipeline, a second proportional regulating valve is arranged on a pipeline between the first circulating pump and the filter, the second proportional regulating valve is connected with the first reactor through a second return pipeline, and a third proportional regulating valve is arranged on a pipeline between the second circulating pump and the post-treatment equipment and is connected with the second reactor through a third return pipeline. In an alternative embodiment, a first buffer tank is arranged on a pipeline between the second proportional control valve and the filter, and a second buffer tank is arranged on a pipeline between the ion exchange device and the delivery pump. In an alternative embodiment, a heat exchanger is further arranged on the third return line, and a preheater is arranged on the line between the transfer pump and the second reactor. In an alternative embodiment, the post-treatment device comprises a centrifuge and a disc dryer, and the second circulating pump is connected with the centrifuge and the disc dryer in sequence through the main pipeline. In a second aspect, the present application further provides a preparation method of battery grade lithium carbonate, where the preparation system of battery grade lithium carbonate includes: preparing industrial grade lithium carbonate and water into slurry according to a first preset proportion, inputting the slurry into a beating tank, and preliminarily premixing the slurry in the beating tank; circulating the primarily premixed slurry between the pulping tank and the homogenizing pump according to preset time; the recycled slurry is returned to the pulping tank according to a second preset proportion and is input into a first reactor; The slurry fed into the first reactor is subjected to carbonization reaction when the reaction temperature, the reaction pressure and the reaction residence time meet the first preset conditions, so as to generate reaction liquid; inputting the reaction liquid into a carbonization buffer tank to obtain a lithium bicarbonate solution; Refluxing the lithium bicarbonate solution into the first reactor according to a third preset proportion and filtering the solution by an input filter; Inputting the filtered lithium bicarbonate solution into an ion exchange device to adsorb calcium ions and magnesium ions in the lithium bicarbonate solution; inputting the adsorbed lithium bicarbonate solution into a second reactor, and pe