Nitrate Salt-Based Graphite Oxide Process

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Solution Overview

Problem

Conventional chlorate salt-based graphite oxidation processes using nitric acid pose hazards due to nitric acid evaporation and chlorine dioxide gas buildup, leading to explosive concentrations and equipment corrosion, which necessitates maintaining low reaction temperatures, thereby reducing the solubility and reactivity of chlorate salts and increasing chlorine dioxide concentrations.

Innovation Solution

A nitrate salt-based process is developed, involving a reaction mixture of sulfuric acid, an inorganic nitrate salt, water, and a chlorate salt with graphite, which eliminates the use of nitric acid by forming graphite oxide at higher temperatures without compromising the quality of the graphite oxide produced, allowing for controlled ClO2 gas purging and minimizing hazardous conditions.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If nitric acid is used in the reaction mixture, then the oxidation of graphite to graphite oxide is effective, but nitric acid evaporates and condenses in gas outlet lines, corrodes equipment, and contributes to chlorine dioxide gas buildup reaching explosive concentrations

Engineering Contradiction:
Improveoxidation effectivenessVSAvoidnitric acid evaporation and equipment corrosion
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The patent removes nitric acid from the reaction mixture entirely, replacing it with alternative oxidizing agents (permanganate salts, persulfates, or chlorate salts combined with sulfuric acid and nitrate salts). This extraction of the harmful substance eliminates the evaporation and corrosion problems while maintaining oxidation effectiveness through the alternative chemical systems.

Inventive Principle:
Principle #2Taking out (Extraction)

2Object-affected harmful factors

If temperature is kept low (0-5°C) to minimize nitric acid evaporation and chlorine dioxide buildup, then safety is improved, but solubility and reactivity of chlorate salt are reduced

Engineering Contradiction:
Improvechlorine dioxide gas concentrationVSAvoidchlorate salt solubility and reactivity
Core Design Contradiction:
Object-affected harmful factorsVSProductivity

Solution Approach 1:

The patent changes the chemical parameters of the reaction system by replacing nitric acid with alternative oxidizing agents that have different temperature-dependent behaviors. This allows the reaction to proceed effectively at higher temperatures where chlorate salt solubility and reactivity are improved, without the same safety constraints that limited the nitric acid-based system.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If nitric acid is used to achieve effective oxidation, then graphite oxide quality is maintained, but the process generates hazardous chlorine dioxide gas that builds up to explosive concentrations

Engineering Contradiction:
Improvegraphite oxide qualityVSAvoidchlorine dioxide gas generation
Core Design Contradiction:
Manufacturing precisionVSObject-generated harmful factors

Solution Approach 1:

The patent converts the harmful chlorine dioxide gas generation into a beneficial or controlled process by using alternative oxidizing agents. The harmful ClO2 gas is replaced with other oxidation products that are less hazardous, while the oxidation effectiveness and graphite oxide quality are maintained through the alternative chemical pathways using permanganate salts, persulfates, or controlled chlorate salt systems.

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

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 process effectively produces high-quality graphite oxide with increased BET surface area, reducing the risks associated with nitric acid and chlorine dioxide, enabling the production of highly exfoliated graphite suitable for various composite applications while maintaining safe operational conditions.

Implementation Method 1

Graphite oxide is a class of an intercalated layered material that is prepared by oxidizing a graphite with an oxidizing agent

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 2

allowing the reaction mixture to react to form graphite oxide

Methodology Applied
Scientific EffectChemical reaction: Reaction (physics)

Implementation Method 3

The process also generates hazardous chlorine dioxide (ClO2) gas, which is believed to be associated with effective oxidation of the graphite to graphite oxide

Methodology Applied
Scientific EffectDecomposition: Decomposition (biological)

Data Source

PatentUS9199851B2Nitrate salt-based process for manufacture of graphite oxide
Publication Date: 2015.12.01 DOW GLOBAL TECHNOLOGIES LLC

AI summary

The present invention relates to a nitrate salt-based process for preparing a graphite oxide. The invention nitrate salt-based process employs starting materials comprising a sulfuric acid, an inorganic nitrate salt, an amount of water, a first amount of chlorate salt, and a graphite.