Reduced Graphene Oxide Manufacture from Kish Graphite

Solution Overview

Problem

Conventional methods for manufacturing reduced graphene oxide from Kish graphite are environmentally unfriendly and inefficient, involving multiple chemical treatments that generate toxic gases and require long processing times, making them difficult to manage at an industrial scale.

Innovation Solution

A method involving sieving, flotation, and acid leaching of Kish graphite, followed by oxidation with ammonium nitrate and controlled oxidation to produce graphene oxide, which is then reduced using a environmentally friendly reducing agent, resulting in high-purity reduced graphene oxide with reduced oxygen content and smaller lateral size.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional Hummer Method is used for oxidation with sodium nitrate, sulfuric acid and potassium permanganate, then graphene oxide can be produced, but toxic gases such as NO2, N2O4 and NH3 are generated which are not environmentally friendly

Engineering Contradiction:
Core Design Contradiction:
Ease of manufactureVSObject-generated harmful factors

Solution Approach 1:

The patent changes the chemical parameters of the oxidation process by replacing sodium nitrate with ammonium nitrate and adjusting the oxidizing agent to potassium dichromate or sodium chlorate, thereby eliminating toxic gas generation while maintaining effective oxidation of graphite to graphene oxide

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent converts the harmful effect of nitrate decomposition into a beneficial outcome by using ammonium nitrate instead of sodium nitrate, which decomposes to produce nitrogen and water vapor instead of toxic nitrogen oxides, thus eliminating environmental harm while preserving the oxidation function

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

2Manufacturing precision

If chemical pretreatment composition is used for purification of Kish graphite, then the graphite can be purified, but a lot of chemical waste has to be treated and the stability of composition is difficult to control

Engineering Contradiction:
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent extracts and removes the problematic chemical pretreatment composition step entirely, replacing it with a simplified acid leaching process using only dilute sulfuric acid or hydrochloric acid, thereby eliminating the need for complex multi-component chemical compositions and their associated waste treatment issues

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent makes the acid leaching step serve multiple functions simultaneously: it acts as both the pretreatment and purification step, eliminating the need for separate flushing and purification steps while achieving effective graphite purification

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

3Manufacturing precision

If flushing process and purification process are used for pretreatment of Kish graphite, then the graphite can be purified, but the productivity is slowed due to long preparation time

Engineering Contradiction:
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent merges the flushing process and purification process into a single acid leaching step, combining multiple sequential operations into one unified process that achieves the same purification effect in less time, thereby improving productivity without sacrificing purification quality

Inventive Principle:
Principle #5Merging (Combining)

4Manufacturing precision

If reduction of graphene oxide is performed during 24 hours, then reduced graphene oxide can be obtained, but the productivity is very low

Engineering Contradiction:
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent changes the physical parameters of the reduction process by increasing temperature to 90-110°C and optimizing the reducing agent concentration and type, thereby reducing the reduction time from 24 hours to 2-6 hours while maintaining high-quality reduced graphene oxide production

Inventive Principle:
Principle #35Parameter changes

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 reduced graphene oxide with reduced oxygen content and smaller lateral size, is less polluting, and significantly reduces processing time, making it more efficient and suitable for industrial-scale production.

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)

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 2

D. a reduction of graphene oxide into reduced graphene oxide

Methodology Applied
Scientific EffectReduction: Reduction

Implementation Method 3

ii. a flotation step with the fraction b) of kish graphite having a size above or equal to 50 μm

Methodology Applied
Scientific EffectFlotation: Froth Floatation

Implementation Method 4

iii. an acid leaching step wherein an acid is added so that the ratio in weight (acid amount)/(kish graphite amount) is between 0.25 and 1.0

Methodology Applied
Scientific EffectAcid leaching: Chemical Bonding

Data Source

PatentUS12162759B2Method for the manufacture of reduced graphene oxide from Kish graphite
Publication Date: 2024.12.10
  • US12162759B2 patent drawing

AI summary

A method for the manufacture of reduced graphene oxide from Kish graphite including the pretreatment of kish graphite, the oxidation of pre-treated kish graphite into graphene oxide and the reduction of graphene oxide into reduced graphene oxide, the reduced graphene oxide and the use of the graphene oxide.