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CN-117566771-B - Method for preparing lithium carbonate based on supergravity reactor and lithium carbonate

CN117566771BCN 117566771 BCN117566771 BCN 117566771BCN-117566771-B

Abstract

The invention belongs to the field of new energy, and discloses a method for preparing lithium carbonate based on a hypergravity reactor, which comprises the following steps that step 1, a soluble carbonate solution is added into the hypergravity reactor as a base solution; and step 2, continuously adding the first solution containing lithium ions into a hypergravity reactor, and step 3, introducing the product obtained in the step 2 into a reaction kettle, continuously adding the second solution containing lithium ions while stirring, and obtaining lithium carbonate after the reaction is completed. The method adopts a hypergravity reactor to perform preliminary crystallization operation to obtain liquid with uniform initial particle size, and then the liquid after preliminary crystallization is transferred into a reaction kettle to further enlarge crystals. Meanwhile, the invention also discloses lithium carbonate.

Inventors

  • HUANG ZHI
  • CHEN JUN
  • CHEN CHUANLIN
  • LIU YATING
  • WU YUPENG
  • HAN HENG

Assignees

  • 广州天赐高新材料股份有限公司
  • 九江天赐高新材料有限公司

Dates

Publication Date
20260508
Application Date
20231130

Claims (10)

  1. 1. The method for preparing the lithium carbonate based on the hypergravity reactor is characterized by comprising the following steps of: step 1, adding a soluble carbonate solution serving as a base solution into a hypergravity reactor; step 2, continuously adding the first solution containing lithium ions into a hypergravity reactor to obtain a solution containing seed crystals; Step 3, introducing the solution obtained in the step 2 into a reaction kettle, continuously adding a second solution containing lithium ions while stirring, and obtaining lithium carbonate after the reaction is completed; the second solution is lithium-containing brine; The molar quantity of carbonate in the soluble carbonate solution is 0.5-0.8 times of the sum of the molar quantity of lithium ions in the first solution and the molar quantity of lithium ions in the second solution, and the molar ratio of lithium ions in the first solution to lithium ions in the second solution is 5-35:65-95.
  2. 2. The method for preparing lithium carbonate based on a hypergravity reactor according to claim 1, wherein the first solution and the second solution are lithium-containing brine.
  3. 3. The method for preparing lithium carbonate based on a hypergravity reactor according to claim 1, wherein the first solution is a lithium salt solution and the second solution is lithium-containing brine.
  4. 4. The method for preparing lithium carbonate based on a hypergravity reactor according to claim 2 or 3, wherein the concentration of sodium ions in brine is 0-70 g/L, and the concentration of potassium ions is 0-15 g/L; And/or the concentration of lithium ions in the brine is 0.01-8 g/L.
  5. 5. The method for preparing lithium carbonate based on a hypergravity reactor according to claim 1, wherein the independent reaction temperature in the steps 2 to 3 is 50 to 99 ℃; and/or the filling time of the first solution is 0.1-2 h; And/or the filling time of the second solution is 0.5-3 h; and/or, in the step 3, after the second solution is added, continuing to react for 1-3h.
  6. 6. The method for preparing lithium carbonate based on a hypergravity reactor according to claim 1, wherein the concentration of carbonate in the base solution is 10-32wt%; The carbonate is sodium carbonate and/or potassium carbonate.
  7. 7. The method for preparing lithium carbonate based on the hypergravity reactor according to claim 1, wherein the stirring speed of the hypergravity reactor is 2000-5000 r/min.
  8. 8. The method for preparing lithium carbonate based on the hypergravity reactor according to claim 1, wherein the molar amount of carbonate in the soluble carbonate solution is 0.55-0.75 times of the sum of the molar amounts of lithium ions in the first solution and lithium ions in the second solution, and the molar ratio of lithium ions in the first solution to lithium ions in the second solution is 10-25:75-90.
  9. 9. The method for preparing lithium carbonate based on a hypergravity reactor according to claim 1, wherein in the step 3, after the completion of the reaction, a slurry containing lithium carbonate is obtained; the specific operation of separating lithium carbonate solids from a slurry containing lithium carbonate is: Filtering the slurry containing lithium carbonate, pulping and washing filter residues for 2-4 times, wherein the solid ratio of the slurry to the slurry is 2:1-10:1, the temperature of pulping water is 50-99 ℃, and the washing time is 0.5-3h; After washing, the solid is dispersed into water, and is subjected to secondary stirring washing, then is filtered and rinsed once by clean water, and the temperature of the wash water is 50-99 ℃, so that the lithium carbonate is finally prepared.
  10. 10. The lithium carbonate is characterized in that the lithium carbonate is prepared by the method according to any one of claims 1-9, the particle size distribution of the lithium carbonate is D10 more than or equal to 1 mu m, D50 more than or equal to 5 mu m and less than or equal to 90 mu m, D90 more than or equal to 200 mu m, and the purity of the lithium carbonate is battery grade.

Description

Method for preparing lithium carbonate based on supergravity reactor and lithium carbonate Technical Field The invention relates to the field of new energy, in particular to a method for preparing lithium carbonate based on a hypergravity reactor and lithium carbonate. Background The uniformity of particles and the particle size of the lithium battery cathode material directly influence the battery performance, so that manufacturers of the lithium battery cathode material reduce the content of large particles in lithium carbonate from several aspects such as shearing, sieving, jet milling and the like in order to improve the quality of lithium carbonate products. The prior art discloses a method for preparing high-quality lithium carbonate by adopting a hypergravity reactor, for example, CN110817907A discloses a treatment method for purifying high-purity lithium carbonate, the scheme only discloses that impurities are removed through the hypergravity reactor, the hypergravity reactor does not participate in any crystallization process, the particle size distribution of the prepared lithium carbonate is wide, CN110304643A discloses a hypergravity preparation method for battery-grade superfine lithium carbonate, the battery-grade superfine lithium carbonate is prepared by taking high-lithium-content brine and sodium carbonate aqueous solution as raw materials, starting the hypergravity reactor, adjusting the rotating speed of a rotating disc, controlling hypergravity acceleration, the dispersed materials are radially thrown away under the action of centrifugal force and then impact on the inner wall of the reactor, finally converged liquid flows out from a liquid outlet under the action of a gravity field, and is collected in a product storage tank, aged, washed with alcohol and filtered, so that battery-grade superfine lithium carbonate powder can be obtained. However, only the hypergravity reactor participates in the crystallization process, and the sodium ion and potassium ion contents are higher, so that the purity of the prepared lithium carbonate is lower. Therefore, the technical problem solved by the scheme is how to prepare the lithium carbonate with high purity and narrow particle size distribution. Disclosure of Invention The invention mainly aims to provide a method for preparing lithium carbonate based on a hypergravity reactor, which adopts the hypergravity reactor to perform preliminary crystallization operation to obtain liquid with uniform initial particle size, and then transfers the liquid subjected to preliminary crystallization into a reaction kettle to further enlarge crystals. Meanwhile, the invention also discloses lithium carbonate. In order to achieve the above purpose, the present invention provides the following technical solutions: A method for preparing lithium carbonate based on a hypergravity reactor, comprising the following steps: step 1, adding a soluble carbonate solution serving as a base solution into a hypergravity reactor; step 2, continuously adding the first solution containing lithium ions into a hypergravity reactor to obtain a solution containing seed crystals; And 3, introducing the solution obtained in the step 2 into a reaction kettle, continuously adding a second solution containing lithium ions while stirring, and obtaining lithium carbonate after the reaction is completed. Preferably, the molar amount of carbonate in the soluble carbonate solution is 0.5-0.8 times of the sum of the molar amounts of lithium ions in the first solution and lithium ions in the second solution, and the molar ratio of lithium ions in the first solution to lithium ions in the second solution is 5-60:40-95. In some embodiments of the invention, the molar amount of carbonate in the soluble carbonate solution may be selected to be 0.5, 0.6, 0.7, or 0.8 times the sum of the molar amounts of lithium ions in the first solution and lithium ions in the second solution; the molar amount of lithium ions in the first solution and the molar ratio of lithium ions in the second solution may be selected to be 5:95, 10:90, 15:85, 20:80, 25:75, 30:70, 35:65 or 40:60, 60:40; in the method for preparing lithium carbonate based on the hypergravity reactor, the first solution and the second solution are lithium-containing brine; as the brine commonly used in the field, salt lake brine, salt lake intercrystalline brine and underground brine can be selected; As possible potential raw materials, brine can also be selected from lithium-rich eluent after extraction treatment of oilfield water, coalbed methane field produced water, salt lake brine, salt lake intercrystalline brine, geothermal water, underground brine, seawater and hot spring water in the oilfield exploration process; regardless of the raw materials, the impurities in the brine are mainly sodium ions and/or potassium ions; If the raw materials contain metal ions which are easy to react with carbonate to generate carbonate sediment, the metal i