Method for recycling residual lithium in reaction mother liquid of electrode material by hydrothermal method

A technology of electrode material and recycling, which is applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems that lithium sulfate cannot be recycled, the recycling scheme is cost-effective, and the scope of application is narrow, so as to be conducive to large-scale promotion and application, recycling Good recycling effect and wide application range

Active Publication Date: 2019-03-22
德阳威旭锂电科技有限责任公司
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Residual lithium leads to high production (raw material) costs for the preparation of electrode materials by the hydrothermal process, which also makes it difficult for the hydrothermal process to be widely used in the industrial production of lithium battery electrode materials at this stage
[0006] Some studies have begun to explore the method of fully recycling lithium in the mother liquor of the hydrothermal method. Patent CN107915239A discloses a method for preparing high-purity lithium sulfate by reacting mother liquor with lithium iron phosphate. This method can obtain lithium sulfate with a purity of more than 99%. , but the method can only be used for the reaction mother liquor of lithium iron phosphate material, the scope of application is narrow, and sodium ions are introduced, and the recovered lithium sulfate cannot be directly recycled as raw materials for hydrothermal reaction, which reduces the use value
In addition, there are also some chemical methods, adding a precipitating agent such as barium hydroxide to the reaction mother liquor, and obtaining lithium hydroxide after separating the barium sulfate precipitation, but this method will introduce new impurities (such as barium ions) and lose part of the organic solvent. And additionally prolong the preparation process, increase the difficulty of preparation control and energy consumption, the recycling scheme is less cost-effective, and it is easy to cause adverse effects on the environment

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  • Method for recycling residual lithium in reaction mother liquid of electrode material by hydrothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take the hydrothermal method to prepare the reaction mother liquor of lithium iron phosphate, raise the temperature to 80°C, add lithium hydroxide, adjust the pH value to greater than 11, keep it for 2 hours, and form lithium phosphate and iron hydroxide precipitate suspension; centrifuge to separate the solid and liquid to obtain solid precipitate respectively substances and clear solutions.

[0035] Add the solid precipitate to phosphoric acid at a temperature of 60°C, add 60 mL of water to 5 g of the precipitate, and add phosphoric acid to 1.05 times the theoretical molar value of the reaction with the precipitate. Insulated for 2 hours to obtain a white iron phosphate precipitate, its XRD pattern is shown in figure 1 , Centrifugal separation to obtain a mixed clear solution of lithium dihydrogen phosphate and phosphoric acid, no other chemical raw materials are added, no need to remove impurities, high purity, can be used as raw material for the production of lithiu...

Embodiment 2

[0039] Take the mother liquor of lithium manganese phosphate, raise the temperature to 60°C, add lithium hydroxide, adjust the pH value to be greater than 11, and keep it warm for 3 hours to form lithium phosphate and manganese hydroxide precipitated suspension; centrifuge to separate solid and liquid to obtain solid precipitate and clarified solution respectively.

[0040] Add the solid precipitate to the phosphoric acid solution at a temperature of 40°C, add 60 mL of water to 5 g of the precipitate, and add phosphoric acid to 1.05 times the theoretical molar value of the precipitate. After heat preservation for 10 hours, a white manganese phosphate precipitate was obtained, and centrifuged to obtain a mixed clear solution of lithium dihydrogen phosphate and phosphoric acid, which can be used as a raw material for producing lithium manganese phosphate by the hydrothermal method. The recovery of lithium in the precipitate was >95%.

[0041] Put the clarified solution into a homo...

Embodiment 3

[0044] Take the mother liquor of lithium manganese iron phosphate, raise the temperature to 100°C, add lithium hydroxide, adjust the pH value to be greater than 10, and keep it warm for 1 hour to form lithium phosphate, manganese hydroxide and iron hydroxide precipitate suspension; centrifuge to separate the solid and liquid to obtain solid precipitate respectively substances and clear solutions.

[0045] Add the solid precipitate to phosphoric acid at a temperature of 80°C, add 60 mL of water to 5 g of the precipitate, and add phosphoric acid to 1.05 times the theoretical molar value of the reaction with the precipitate. After 1.5 hours of heat preservation reaction, white manganese phosphate and iron phosphate precipitates were obtained, and centrifuged to obtain a mixed clear solution of lithium dihydrogen phosphate and phosphoric acid, which can be used as a raw material for producing lithium manganese iron phosphate by the hydrothermal method. The recovery of lithium in t...

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Abstract

The invention discloses a method for recycling residual lithium in reaction mother liquid of an electrode material by a hydrothermal method. Lithium hydroxide is added into the reaction mother liquid, solid and liquid are separated after a heating reaction, after a reaction of precipitate and phosphoric acid, the solid and liquid are separated again, and a clarified solution is obtained and usedas a raw material of the electrode material by the hydrothermal method; lithium sulphate is separated from the first separated clarified solution through an ion exchange membrane, a remaining solventis concentrated and recycled to obtain a lithium sulfate aqueous solution to pass through a bipolar membrane, a lithium ion and a sulfate ion are separated and combined with a hydroxide ion and a hydrogen ion obtained by water electrolysis correspondingly, and a lithium hydroxide solution and a sulfuric acid solution are finally obtained correspondingly; and the concentrated lithium hydroxide solution is used as the raw material of the electrode material by the hydrothermal method. According to the method for recycling the residual lithium in the reaction mother liquid of the electrode material by the hydrothermal method, the application range is wide, the raw material cost of hydrothermal method process production is greatly lowered, no new raw materials are added, the recycling effect isgood, the process is simple, cost performance is high, and application and promotion in industrial production are facilitated.

Description

technical field [0001] The invention belongs to the field of lithium battery electrode materials, and in particular relates to a method for recycling residual lithium in a reaction mother liquor of electrode materials prepared by a hydrothermal method. Background technique [0002] Lithium phosphate compounds with an olivine structure in lithium-ion batteries, such as lithium iron phosphate, lithium cobalt phosphate, lithium nickel phosphate, lithium manganese iron phosphate, lithium manganese phosphate, etc., can be used as cathode materials for lithium-ion secondary batteries. Lithium iron phosphate has been widely used in new energy buses, solar and wind power storage and other fields. [0003] The current industrial production technology of olivine structure electrode materials is based on the high-temperature solid-state method, but a large amount of polluting gases will be generated during the sintering process of the high-temperature solid-state method, and the batch ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B26/12H01M4/58
CPCC22B7/006C22B26/12H01M4/5825Y02E60/10Y02P10/20
Inventor 王强吴强黄建新朱禄发
Owner 德阳威旭锂电科技有限责任公司
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