Ferrite Catalyst Preparation via Epoxide Sol-Gel Method

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Solution Overview

Problem

Conventional methods for preparing metal oxide catalysts, such as the coprecipitation method, result in catalysts with low catalytic activity due to the formation of an α-Fe2O3 phase and bulk form, which consumes time and reduces reactivity, especially in oxidative dehydrogenation processes for butadiene production.

Innovation Solution

A method using an epoxide-based sol-gel process to prepare a ferrite catalyst with a pure spinel phase structure and large surface area, involving specific steps of precursor solution preparation, gel aging, drying, and controlled burning to achieve a catalyst with high reactivity, including a first burning step at 70-90°C to 170-200°C and a second burning step at 200-250°C to 630-900°C with controlled heating rates.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If the coprecipitation method is used to prepare the catalyst, then the catalyst is prepared in bulk form, but the catalytic activity is reduced

Engineering Contradiction:
Improvecatalyst preparation simplicityVSAvoidcatalytic activity
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent employs a sol-gel method to create a porous catalyst structure with high surface area. The gel formation process creates an interconnected porous network that maintains catalyst activity while enabling simple bulk preparation. The porous structure allows reactant access to active sites throughout the catalyst matrix, resolving the contradiction between bulk form and catalytic activity.

Inventive Principle:
Principle #31Porous materials

Solution Approach 2:

The patent changes the preparation parameters from conventional coprecipitation to sol-gel chemistry, controlling pH, temperature, and aging conditions to form a gel structure. This parameter change transforms the catalyst morphology from dense bulk to porous structure, maintaining ease of manufacture while dramatically improving catalytic activity through increased surface area and accessible active sites.

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If the coprecipitation method is used, then the catalyst is prepared in bulk form, but the filtration/washing step consumes much time

Engineering Contradiction:
Improvecatalyst preparation simplicityVSAvoidfiltration/washing time
Core Design Contradiction:
Ease of manufactureVSLoss of time

Solution Approach 1:

The porous gel structure formed by the sol-gel method creates a self-supporting catalyst matrix that retains shape during drying. This structure eliminates the need for extensive filtration and washing steps required in coprecipitation methods, as the gel can be directly dried and calcined. The interconnected pores allow efficient solvent removal through evaporation rather than filtration, significantly reducing processing time.

Inventive Principle:
Principle #31Porous materials

Solution Approach 2:

The sol-gel process performs preliminary consolidation of the catalyst precursors into a gel structure before drying. This preliminary action creates a rigid network that prevents particle disintegration during solvent removal, eliminating the need for subsequent filtration and washing operations. The gel structure is formed in advance, allowing direct transition to drying and calcination steps.

Inventive Principle:
Principle #10Preliminary action

3Stability of the object's composition

If an α-Fe2O3 phase is formed after burning, then the catalyst structure is stable, but the catalytic reactivity is reduced

Engineering Contradiction:
Improvecatalyst structure stabilityVSAvoidcatalytic reactivity
Core Design Contradiction:
Stability of the object's compositionVSReliability

Solution Approach 1:

The patent carefully controls the burning temperature and atmosphere parameters to prevent α-Fe2O3 formation. By limiting the maximum burning temperature and controlling oxygen exposure during calcination, the catalyst maintains a stable spinel phase structure with high catalytic reactivity. The parameter control ensures structural stability while avoiding the formation of less active iron oxide phases.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The catalyst forms a composite spinel structure where multiple metal oxides are integrated in a cooperative arrangement. This composite structure provides both structural stability and high catalytic activity, as the different metal components work synergistically. The spinel phase composition resists transformation to α-Fe2O3 while maintaining active sites for oxidation reactions, resolving the contradiction between stability and reactivity.

Inventive Principle:
Principle #40Composite materials

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 a ferrite catalyst with high reactivity and a macroporous structure, eliminating the α-Fe2O3 phase, thereby enhancing catalytic performance and butadiene yield in oxidative dehydrogenation reactions, with improved surface area and carbon content, leading to efficient butadiene production.

Implementation Method 1

an epoxide compound is mixed with the precursor solution to obtain a gel

Methodology Applied
Scientific EffectSol-gel process: Gel

Implementation Method 2

an epoxide-based sol-gel method, involving specific steps of precursor solution preparation, gel aging, drying, and controlled burning

Methodology Applied
Scientific EffectHydrolysis and condensation: Hydrolysis

Implementation Method 3

a step of obtaining a synthetic product by drying the aged gel

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 4

a step of burning the synthetic product, wherein step (e) comprises a first burning step, wherein, in the first burning step, temperature is raised from a temperature range of 70 to 90 °C to a temperature range of 170 to 200 °C

Methodology Applied
Scientific EffectThermal decomposition: Pyrolysis

Implementation Method 5

in the second burning step, temperature is raised from a temperature range of more than 200 °C to 250 °C to a temperature range of 630 to 900 °C, and then maintained at 630 to 900 °C for 4 to 8 hours

Methodology Applied
Scientific EffectSintering: Sintering

Implementation Method 6

butene reacts with oxygen in the presence of a metal oxide catalyst to generate butadiene and water

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 7

oxidative dehydrogenation of butene, wherein butene reacts with oxygen

Methodology Applied
Scientific EffectOxidation: Oxidation

Data Source

PatentEP3560589B1Ferrite catalyst for oxidative dehydrogenation reaction, method for preparing same, and method for preparing butadiene by using same
Publication Date: 2024.10.09 LG CHEM LTD
  • EP3560589B1 patent drawingFigure 1
  • EP3560589B1 patent drawingFigure 2

AI summary

The present invention relates to a ferrite catalyst for oxidative dehydrogenation and a method of preparing the same. More specifically, the present invention relates to a method of preparing a ferrite catalyst for oxidative dehydrogenation using an epoxide-based sol-gel method, wherein a step of burning includes a first burning step, in which burning is performed at a temperature of 70 to 200 °C; and a second burning step, in which burning is performed after temperature is raised from a temperature range of more than 200 °C to 250 °C to a temperature range of 600 to 900 °C.