Graphene Oxide Manufacture from Kish Graphite

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Solution Overview

Problem

Conventional methods for manufacturing graphene oxide from Kish graphite are environmentally unfriendly due to the production of toxic gases and require lengthy chemical treatments, leading to reduced productivity and lower quality graphene oxide with poor properties.

Innovation Solution

A method involving a pre-treatment step that includes sieving, flotation, and acid leaching of Kish graphite, followed by an oxidation step using ammonium nitrate and potassium permanganate, with controlled temperature and addition of a chemical element to stop the oxidation reaction, resulting in high-purity graphene oxide with enhanced properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If conventional Hummer method is used with sodium nitrate and sulfuric acid, then graphene oxide can be synthesized, but toxic gases (NO2, N2O4, NH3) are produced which are harmful to the environment

Engineering Contradiction:
Improvegraphene oxide productionVSAvoidtoxic gases emission
Core Design Contradiction:
Quantity of substanceVSObject-generated harmful factors

Solution Approach 1:

The patent changes the chemical parameters of the oxidation system by replacing sodium nitrate with ammonium nitrate and adjusting the oxidizing agent concentration ratios. This substitution fundamentally alters the reaction pathway to eliminate toxic nitrogen oxide gases while maintaining effective oxidation of graphite to graphene oxide, thus resolving the contradiction between production quantity and harmful emissions

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent converts the potentially harmful oxidation process into a beneficial one by selecting oxidizing agents and conditions that produce non-toxic byproducts. The oxidation reaction still achieves the desired conversion of graphite to graphene oxide, but the harmful toxic gases are replaced with harmless products, turning a harmful process into a beneficial one

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

2Manufacturing precision

If two-step chemical pretreatment (flushing and purification) is applied to Kish graphite, then purification is improved, but chemical waste increases and process complexity increases

Engineering Contradiction:
Improvegraphite purification qualityVSAvoidpretreatment process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent merges the flushing and purification steps into a single integrated acid leaching process using nitric acid. This combined approach achieves both removal of surface contaminants and purification of the graphite structure in one operation, reducing process complexity and chemical waste while maintaining high purification quality

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The acid leaching step serves multiple functions simultaneously: it acts as both a flushing agent to remove surface impurities and a purification medium to clean the graphite structure. This multi-functional approach eliminates the need for separate treatment steps, reducing overall process complexity

Inventive Principle:
Principle #6Universality (Multi-functionality)

3Quantity of substance

If conventional oxidation with sodium nitrate is used, then oxidation reaction proceeds, but oxidation time is prolonged reducing productivity

Engineering Contradiction:
Improvegraphene oxide yieldVSAvoidoxidation reaction speed
Core Design Contradiction:
Quantity of substanceVSProductivity

Solution Approach 1:

The patent changes the chemical parameters by using ammonium nitrate instead of sodium nitrate and optimizing the oxidizing agent concentration and temperature conditions. These parameter changes accelerate the oxidation reaction kinetics, significantly reducing oxidation time while maintaining high graphene oxide yield, thus resolving the contradiction between quantity and productivity

Inventive Principle:
Principle #35Parameter changes

4Quantity of substance

If modified Hummer method is used to obtain graphene oxide, then production is achieved, but lateral size is reduced to about 3 μm leading to poor properties

Engineering Contradiction:
Improvegraphene oxide productionVSAvoidgraphene oxide lateral size
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The patent applies preliminary acid leaching treatment to Kish graphite before oxidation to remove impurities and prepare the graphite structure. This preliminary action prevents unwanted side reactions during oxidation and helps maintain larger lateral sizes in the final graphene oxide product, avoiding the size reduction problem of conventional methods

Inventive Principle:
Principle #10Preliminary action

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

The method produces high-quality graphene oxide with increased oxygen functional groups, reduced environmental impact, and shorter oxidation times, making it suitable for industrial-scale production with improved thermal and electrical conductivities.

Implementation Method 1

an oxidation step of the pre-treated kish-graphite obtained after step B) in order to obtain graphene oxide comprising the following successive sub-steps: i. the preparation of a mixture comprising the pre-treated kish-graphite, an acid and ammonium nitrate (NH4NO3), the mixture being kept at a temperature below 5° C., ii. the addition of an oxidizing agent into the mixture obtained in step C.i)

Methodology Applied
Scientific EffectOxidation: Oxidation

Data Source

PatentUS12103852B2Method for the manufacture of graphene oxide from Kish graphite
Publication Date: 2024.10.01 ARCELORMITTAL SA
  • US12103852B2 patent drawing

AI summary

A method for the manufacture of graphene oxide from Kish graphite including the pretreatment of kish graphite and the oxidation of pre-treated kish graphite into graphene oxide, the graphene oxide obtained with at least 45% by weight of oxygen functional groups and the use of the graphene oxide.