Washing method of ternary precursor

A washing method and precursor technology, applied in the direction of chemical instruments and methods, inorganic chemistry, nickel compounds, etc., can solve the problems of drying equipment damage, prolonging the drying time, and high water content of the drying material, so as to achieve easy drying, The effect of loose microscopic appearance and excellent washing consistency

Pending Publication Date: 2022-03-15
HUNAN BRUNP RECYCLING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most enterprises use centrifuges or filter presses when washing the precursors of ternary materials. 4 2- ions, and then wash off the excess metal cations and obtain the material to be baked. The current technology can control the pH of the reaction section, the washing amount of alkaline washing and water washing in the washing section, the washing temperature, etc., to wash off most of the impurity ions. Control within a reasonable range, however, the water content in the material to be dried after washing is often easily ignored. Even if you notice this and constantly adjust the process parameters of the washing equipment, the water content in the material to be dried is sti

Method used

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  • Washing method of ternary precursor
  • Washing method of ternary precursor
  • Washing method of ternary precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] In this example, the synthesis steps of the ternary precursor are as follows:

[0050] S1: Put the soluble transition mixed metal salt (nickel, cobalt, manganese or aluminum) and sodium hydroxide solution, complexing agent, etc. into the reactor and stir in parallel, control the stirring frequency to 40Hz, and the temperature in the reactor to 60°C. The pH is 10.8-11.3, the reaction time is 4h, and the ternary precursor is obtained by co-precipitation;

[0051] S2: Transfer the ternary precursor to the alkali immersion tank after removing the mother liquor, control the concentration of sodium hydroxide in the alkali immersion tank to 1.5mol / L, the temperature to 50-60°C, the stirring frequency to 15Hz, and the alkali immersion time to 5min , transfer the ternary precursor with alkali solution to the plate and frame filter press through the feed pipe, first use 0.2mol / L sodium hydroxide solution at 40-45°C as the alkali washing solution for 10 minutes, and then Wash with ...

Embodiment 2

[0056] In this embodiment, step S1 and step S3 in the synthesis steps of the ternary precursor are the same as in embodiment 1, and step S2 is:

[0057] Remove the mother liquor from the ternary precursor and transfer it to an alkali immersion tank. Control the concentration of sodium hydroxide in the alkali immersion tank to 1.5mol / L, the temperature is 50-60°C, the stirring frequency is 15Hz, and the alkali immersion time is 5min. The feeding pipe transfers the ternary precursor with alkali solution to the plate and frame filter press, first washes it with 0.2mol / L sodium hydroxide solution at 40-45°C as the alkali washing solution for 10 minutes, and then washes it with 60 Wash with an aqueous solution of ethanol with a mass fraction of 10% at ~65°C for 30 minutes, wash with an aqueous solution of ethanol with a mass fraction of 50% at 55 to 60°C for 10 minutes, wash with an aqueous solution of 85% ethanol at 50°C for 5 minutes, and then wash with 40 0.5 MPa compressed air ...

Embodiment 3

[0059] In this embodiment, step S1 and step S3 in the synthesis steps of the ternary precursor are the same as in embodiment 1, and step S2 is:

[0060] Remove the mother liquor from the ternary precursor and transfer it to an alkali immersion tank. Control the concentration of sodium hydroxide in the alkali immersion tank to 1.5mol / L, the temperature to 50-60°C, the stirring frequency to 15Hz, and the alkali immersion time to 5min. The feeding pipe transfers the ternary precursor with alkali solution to the plate and frame filter press, first washes it with 0.2mol / L sodium hydroxide solution at 40-45°C as the alkali washing solution for 10 minutes, and then washes it with 60 Wash with pure water at ~65°C for 30min, then wash with 10% ethanol aqueous solution at 60~65°C for 30min, wash with 85% ethanol aqueous solution at 50°C for 5min, compress with 0.5MPa at 40°C The air was purged for 8 minutes to obtain the material to be baked.

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Abstract

The invention provides a washing method of a ternary precursor, which is characterized in that through multi-stage alcohol washing, on the premise of ensuring that various properties of a washed to-be-dried material are equivalent to those of a to-be-dried material in a conventional washing process, moisture contained in the to-be-dried material is less, and the to-be-dried material is easier to dry. According to the washing method of the ternary precursor, a washing procedure in a back-end program of an existing washing procedure is replaced by at least two stages of echelon multi-stage washing procedures, and the mass fraction of an alcoholic solution in the back washing procedure is higher than that of an alcoholic solution in the front washing procedure. The washing process follows the basic principle of washing for a small amount and multiple times, the washing consistency is better, and on the premise that it is guaranteed that all properties of the washed to-be-dried material are basically equivalent to those of the to-be-dried material in the conventional washing process, moisture contained in the to-be-dried material is less, and the to-be-dried material is easier to dry.

Description

technical field [0001] The invention belongs to the technical field of battery preparation, and in particular relates to a washing method of a ternary precursor. Background technique [0002] Lithium-ion battery cathode material is a decisive factor affecting the electrochemical performance, safety and cost of the entire battery. Among related technologies, the most widely commercialized lithium-ion battery cathode material is LiNi x co y mn 1-x-y o 2 Ternary material. [0003] At present, the preparation methods of ternary cathode materials mainly include high-temperature solid-phase method, liquid-phase co-precipitation controlled crystallization method, sol-gel method, spray pyrolysis method and hydrothermal method. At present, most enterprises use the liquid-phase co-precipitation controlled crystallization method for large-scale production of ternary material precursors. This method combines soluble transition mixed metal salts (nickel, cobalt, manganese or aluminum...

Claims

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Application Information

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IPC IPC(8): C01G53/00
CPCC01G53/006C01P2006/12C01P2004/03C01P2002/72Y02E60/10
Inventor 赵微伍文丽曹凯峰刘勇奇巩勤学李长东
Owner HUNAN BRUNP RECYCLING TECH
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