Mixed Metal Oxide Preparation via Glucose Oxidation

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Solution Overview

Problem

Current methods for preparing mixed metal oxides, such as those used in catalysts for methanol and dimethyl ether synthesis, require high-temperature calcination and rigorous reduction steps, leading to instability and high solvent usage, which limits their performance and shelf life.

Innovation Solution

A method involving glucose oxidation assisted precipitation through Fehling's route using sodium potassium tartrate as a metal complexing agent, allowing for in-situ preparation of mixed metal oxides at low temperatures without the need for calcination or rigorous reduction, and enabling the production of bi-functional hybrid catalysts with copper in the intermediate oxidation state of cuprous oxide.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional precipitation method is used to prepare mixed metal oxides, then metal oxides can be obtained, but high-temperature calcination and reduction steps are required leading to instability and high solvent usage

Engineering Contradiction:
Improvestability of metal oxideVSAvoidcalcination temperature
Core Design Contradiction:
ReliabilityVSTemperature

Solution Approach 1:

The invention changes the chemical parameters of the precipitation process by using Fehling's solution and glucose oxidation instead of conventional hydroxide precipitation. This allows formation of metal oxides at lower temperatures (avoiding high-temperature calcination) while achieving stable products through the specific chemical environment provided by tartrate complexation and controlled oxidation

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

Fehling's solution acts as an intermediary system that enables indirect formation of metal oxides. The tartrate complex serves as a mediator that controls metal ion precipitation and oxidation state, allowing stable oxide formation without direct high-temperature treatment. The glucose-Fehling's system mediates the reduction and oxidation processes to achieve stable Cu(I) and Cu(II) oxide mixtures

Inventive Principle:
Principle #24Intermediary (Mediator)

2Ease of manufacture

If conventional co-precipitation method is used for catalyst preparation, then metal oxide catalysts can be produced, but rigorous reduction steps are required leading to high solvent usage and process complexity

Engineering Contradiction:
Improvesimplicity of preparation processVSAvoidsolvent usage
Core Design Contradiction:
Ease of manufactureVSQuantity of substance

Solution Approach 1:

The invention merges multiple steps (precipitation, oxidation control, and oxide formation) into a single integrated process using Fehling's solution and glucose. Instead of separate precipitation followed by calcination and reduction steps, all transformations occur simultaneously in one pot, dramatically reducing solvent usage and process complexity while maintaining catalyst quality

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The system uses glucose as a self-contained reducing agent that automatically regulates the oxidation states of copper during precipitation. The glucose-Fehling's reaction self-regulates to produce the desired Cu(I)/Cu(II) oxide mixture without requiring external reducing agents or multiple treatment steps, simplifying the manufacturing process

Inventive Principle:
Principle #25Self-service

3Productivity

If bi-functional catalysts are prepared for direct syn-gas to DME conversion, then higher conversion efficiency is achieved, but tuning catalytic sites for both reactions requires great and dedicated efforts

Engineering Contradiction:
Improvesyn-gas conversion efficiencyVSAvoidcatalyst structure complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The invention creates local quality variations within the catalyst structure by controlling the distribution of Cu(I) and Cu(II) oxide phases. Different oxidation states provide different catalytic functions: Cu(I) sites favor methanol synthesis while Cu(II) sites facilitate dehydration to DME. The tartrate complexation and glucose oxidation process creates a controlled mixture of these phases with optimal spatial distribution for bi-functional activity

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The catalyst is designed as a composite material containing mixed Cu(I) and Cu(II) oxide phases in specific ratios. This composite structure integrates both methanol synthesis and dehydration functions within a single catalyst entity. The Fehling's solution-based preparation method enables precise control of the composite phase composition, achieving optimal performance for direct syn-gas to DME conversion

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

This approach results in highly selective and stable bi-functional hybrid catalysts capable of direct conversion of syn-gas to dimethyl ether with improved selectivity and yield, while reducing process parameters and avoiding coke formation, thus overcoming the limitations of traditional methods.

Implementation Method 1

glucose oxidation assisted precipitation

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 2

in-situ reduction of Cu2+

Methodology Applied
Scientific EffectReduction: Reduction

Implementation Method 3

sodium potassium tartrate as a metal complexing agent

Methodology Applied
Scientific EffectComplexation: Chemical Bonding

Implementation Method 4

precipitating a mixed metal salt solution with Fehling's reagent B and glucose

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Data Source

PatentUS10661253B2Method of preparation of mixed metal oxide using glucose oxidation assisted precipitation
Publication Date: 2020.05.26 BHARAT PETROLEUM CORP LTD
  • US10661253B2 patent drawing

AI summary

The present invention provides a process for in-situ preparation of metal oxide(s) comprising the step of precipitating a metal salt solution with Fehling's reagent B and glucose at a suitable temperature. The metal oxide(s) prepared according to the present invention can be used for diverse applications including their utility as catalyst(s) in one or more reactions. The present invention further provides a highly selective bi-functional hybrid catalyst for direct conversion of syn-gas to dimethyl ether (DME) and methods of preparation thereof. The one or more metal oxide(s) can be directly obtained from the metal precursors following the method(s) of the present invention instead of metal hydroxides as in conventional known methods, thereby eliminating the necessity of high temperature calcination step(s) and rigorous reduction procedure(s).