Recycled Graphite Purification by Iterative Roasting and Washing

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Solution Overview

Problem

Conventional recycling methods for lithium-ion batteries struggle to achieve high purity graphite for anode material due to residual impurities like aluminum oxide, which complicates meeting customer specifications for performance and physical characteristics.

Innovation Solution

A two-phase roasting process combined with washing, involving multiple iterations of sintering with hydroxide-based solutions and subsequent washing with DI water and optional acid wash, effectively converts water-insoluble metal impurities into water-soluble forms for removal, achieving graphite purity of at least 99.5%.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional leaching and washing processes are used to recover graphite from spent Li-ion batteries, then the recovery process is simple and fast, but the graphite product contains substantial impurities like aluminum oxide that fail to meet battery-grade purity specifications

Engineering Contradiction:
Improvegraphite purityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The purification process is divided into multiple sequential stages: initial leaching, first roasting with acid wash, second roasting with base wash, and optional third roasting. Each stage targets specific impurities and progressively increases graphite purity from ~80% to 99.5% or higher, breaking down the complex purification challenge into manageable steps.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process utilizes parameter changes by alternating between acidic and basic chemical environments during different roasting stages. The pH conditions are systematically varied to selectively dissolve different types of impurities, with each roasting-washing cycle optimizing chemical parameters to remove specific contaminants while preserving graphite.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If multiple roasting and washing cycles are implemented to achieve high purity graphite, then impurity removal is effective, but the processing time and operational complexity increase

Engineering Contradiction:
Improvegraphite purityVSAvoidprocessing time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The initial leaching stage performs preliminary removal of soluble cathode materials and loosely bound impurities before the main roasting cycles. This preliminary action reduces the impurity load entering the subsequent roasting stages, making the overall process more efficient and reducing the time required for later purification steps.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The process employs periodic alternation between roasting (heating) and washing (cooling/chemical treatment) cycles. This periodic action allows impurities to be converted to soluble forms during roasting, then removed during washing phases, creating an efficient rhythm of impurity transformation and removal that accelerates overall purification.

Inventive Principle:
Principle #19Periodic action

3Quantity of substance

If acid leaching is used to recover graphite from black mass, then cathode materials are effectively extracted, but aluminum oxide and other metal impurities remain as residues in the graphite product

Engineering Contradiction:
Improvecathode material recoveryVSAvoidgraphite purity
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The process selectively extracts different components at different stages: initial acid leaching extracts cathode materials (Ni, Mn, Co), while subsequent base washing extracts aluminum oxide and other metal impurities from the graphite. Each extraction stage targets specific substances, separating them systematically from the graphite product.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The roasting process acts as an intermediary that transforms insoluble metal impurities into water-soluble metal salts or hydroxides. This chemical transformation mediates between the initial mixed impurity state and the final purified graphite state, enabling efficient removal of aluminum oxide and other contaminants through subsequent washing.

Inventive Principle:
Principle #24Intermediary (Mediator)

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

This approach significantly improves the purity of recycled graphite, achieving up to 99.9% purity and meeting stringent battery-grade standards, enhancing the quality and performance of recycled anode material.

Implementation Method 1

A roasting process iterates multiple times for purifying the graphite, combined with washing, and is believed to convert water insoluble metal impurities into water-soluble metal salts

Methodology Applied
Scientific EffectRoasting: Heat Treatment

Implementation Method 2

Removal of the metal salts in the graphite occurs by leaching in a dilute sodium hydroxide solution and washing the purified graphite for further removal of the water-soluble impurities

Methodology Applied
Scientific EffectLeaching: Solvation

Data Source

PatentUS20240286905A1Recycled graphite for li-ion batteries
Publication Date: 2024.08.29 ASCEND ELEMENTS INC
  • US20240286905A1 patent drawing
  • US20240286905A1 patent drawing
  • US20240286905A1 patent drawing

AI summary

A method of producing a purified graphite from a recycled battery stream for use in as anode material in Li-ion batteries is described. The method comprises a leaching step to obtain a precipitate comprising graphite by filtration, which is then iteratively roasted as a slurry with an aqueous solution of a hydroxide base and subsequently washed to form a purified graphite.