Ni-Co-Mn Oxalate Separation via pH-Controlled Precipitation

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Solution Overview

Problem

Current methods for recovering nickel (Ni), cobalt (Co), and manganese (Mn) from battery scrap require thermal treatment for separation, which complicates the process and reduces efficiency.

Innovation Solution

A process involving the dissolution of a mixture of oxalates in an acid to a pH of -0.5 or less, followed by pH adjustment and solid/liquid separation to precipitate and separate nickel, cobalt, and manganese oxalates without the need for thermal treatment.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If thermal treatment is used for separation of Ni, Co, and Mn, then separation can be achieved, but the process complexity increases and efficiency decreases

Engineering Contradiction:
Improveseparation efficiencyVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent changes the chemical parameters of the solution by adjusting pH to specific ranges (pH 3-5 for nickel oxalate precipitation, pH 6-8 for cobalt oxalate precipitation, pH 9-11 for manganese oxalate precipitation). This allows selective precipitation of different metal oxalates from the leach solution, achieving separation without thermal treatment and simplifying the overall process while maintaining high separation efficiency

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent replaces the thermal treatment mechanism with a chemical precipitation mechanism. Instead of using heat to separate metals, the process uses pH-controlled chemical reactions to selectively precipitate metal oxalates, thereby substituting a complex thermal system with a simpler chemical separation system

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

2Manufacturing precision

If thermal treatment is used for separation, then metals can be separated, but processing time and energy consumption increase

Engineering Contradiction:
Improveseparation capabilityVSAvoidprocessing time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent uses pH parameter adjustment as the controlling factor for separation. By sequentially adjusting pH to different ranges and adding oxalate ions, the process achieves rapid selective precipitation of nickel, cobalt, and manganese oxalates, significantly reducing processing time compared to thermal treatment methods while maintaining effective separation capability

Inventive Principle:
Principle #35Parameter changes

3Quantity of substance

If conventional hydrometallurgical processing is used, then metal recovery is achieved, but the process requires multiple steps including thermal treatment

Engineering Contradiction:
Improvemetal recoveryVSAvoidnumber of process steps
Core Design Contradiction:
Quantity of substanceVSDevice complexity

Solution Approach 1:

The patent merges the leaching step with the separation step by performing selective precipitation directly in the leach solution after pH adjustment. This integration eliminates the need for separate thermal treatment and concentration steps, reducing the total number of process steps while ensuring complete metal recovery through sequential precipitation of nickel, cobalt, and manganese oxalates

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent extracts each metal from the leach solution in sequence by selective precipitation. Nickel oxalate is precipitated first at pH 3-5, then cobalt oxalate at pH 6-8, and finally manganese oxalate at pH 9-11. This stepwise extraction ensures complete metal recovery while simplifying the process by combining extraction with separation in a single integrated flow

Inventive Principle:
Principle #2Taking out (Extraction)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

Enables simultaneous recovery and efficient separation of Ni, Co, and Mn in the liquid phase, streamlining the recycling process and improving the recovery of these metals from battery scrap.

Implementation Method 1

dissolving the mixture of oxalates in an acid to form a solution having a pH -0.5 or less

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 2

adjusting the pH of the solution formed in step (b) to a value ranging from 0.1 to 0.9 by adding a base

Methodology Applied
Scientific EffectpH adjustment:

Implementation Method 3

precipitating nickel oxalate by adjusting the pH of the solution formed in step (b) to a value ranging from 0.1 to 0.9 by adding a base

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 4

separating the precipitated nickel oxalate from the remaining solution of step (c) by solid/liquid separation

Methodology Applied
Scientific EffectSolid/liquid separation: Sedimentation

Implementation Method 5

adjusting the pH of the remaining solution from step (d) to a value ranging from 1 to 6 by adding a base

Methodology Applied
Scientific EffectpH adjustment:

Implementation Method 6

precipitating cobalt oxalate by adjusting the pH of the remaining solution from step (d) to a value ranging from 1 to 6 by adding a base

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 7

separating the precipitated cobalt oxalate from the remaining solution of step (e) by solid/liquid separation

Methodology Applied
Scientific EffectSolid/liquid separation: Sedimentation

Implementation Method 8

adjusting the pH of the remaining solution from step (f) to a value ranging from 8 to 14.5 by adding a base

Methodology Applied
Scientific EffectpH adjustment:

Implementation Method 9

precipitating a precipitate of one or more of manganese oxalate, manganese hydroxide and manganese oxide by adjusting the pH of the remaining solution from step (f) to a value ranging from 8 to 14.5 by adding a base

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 10

separating the precipitate of one or more of manganese oxalate, manganese hydroxide and manganese oxide from the remaining solution of step (g) by solid/liquid separation

Methodology Applied
Scientific EffectSolid/liquid separation: Sedimentation

Data Source

PatentUS20230246259A1Process for separating a mixure of oxalates of two or more of ni, co, and mn
Publication Date: 2023.08.03 BASF SE
  • US20230246259A1 patent drawing

AI summary

The present disclosure is directed to processes for separating a mixture of oxalates of two or more of Ni (nickel), Co (cobalt) and Mn (manganese). Such processes are useful, for example, to separate recovery of two or more of Ni, Co and Mn from used ithium ion batteries or from waste of the production of lithium ion batteries or of cells or components of lithium ion batteries.