TEMPO-Mediated Photoelectrochemical Oxidation of HMF to FDCA

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Solution Overview

Problem

Current photoelectrochemical cells (PECs) face inefficiencies due to kinetically unfavorable water oxidation as the anode reaction, which limits the production of valuable chemicals like 2,5-furandicarboxylic acid (FDCA) from 5-hydroxymethylfurfural (HMF), with previous methods requiring precious metals and high pressures/temperatures.

Innovation Solution

The use of TEMPO-mediated electrochemical and photoelectrochemical cells that oxidize HMF to FDCA or 2,5-diformylfuran (DFF) at ambient conditions without precious metal catalysts, utilizing a TEMPO mediator to promote oxidation and suppress water oxidation, allowing for high yields and selectivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If water oxidation is used as the anode reaction in PECs, then the circuit is completed and H+ is generated, but the reaction is kinetically unfavorable and limits the production of valuable chemicals

Engineering Contradiction:
Improveproduction rate of valuable chemicalsVSAvoidkinetic favorability of anode reaction
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent introduces an organic mediator (such as methyl viologen or anthraquinone derivatives) that acts as an intermediary between the semiconductor electrode and HMF. The mediator absorbs photogenerated holes and transfers them to HMF, enabling efficient oxidation while avoiding the kinetic limitations of direct water oxidation. This resolves the contradiction by providing an alternative electron transfer pathway that is both kinetically favorable and productive for chemical synthesis.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Productivity

If precious metal catalysts are used for HMF oxidation, then conversion efficiency improves, but device complexity and cost increase

Engineering Contradiction:
Improveconversion efficiency of HMFVSAvoidcatalyst system complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent replaces expensive precious metal catalysts with organic mediators that are cheaper, easier to synthesize, and can be used in solution phase. The organic mediators perform the catalytic function temporarily during the reaction cycle and can be regenerated, eliminating the need for complex precious metal catalyst systems while maintaining high conversion efficiency.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent substitutes the traditional heterogeneous catalysis mechanism (mechanical contact between solid catalyst and liquid reactant) with a solution-phase organic mediation mechanism. The organic mediator dissolves in the electrolyte and facilitates electron transfer through molecular interactions, replacing the need for solid precious metal catalysts and simplifying the overall system.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

3Productivity

If high pressure and temperature are applied for HMF oxidation, then reaction rate increases, but energy consumption and operational complexity increase

Engineering Contradiction:
Improvereaction rateVSAvoidenergy consumption
Core Design Contradiction:
ProductivityVSUse of energy by moving object

Solution Approach 1:

The patent changes the reaction conditions from high pressure and temperature to ambient or mild conditions by introducing the organic mediator. The mediator enables the oxidation reaction to proceed efficiently at lower temperatures and pressures by providing an alternative reaction pathway with lower activation energy, thus reducing energy consumption while maintaining high productivity.

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

Achieves nearly complete conversion of HMF to FDCA or DFF with high selectivity and Faradaic efficiency at ambient temperatures and pressures, replacing water oxidation and eliminating the need for precious metal catalysts, thus enhancing the efficiency and utility of PECs for solar fuel production.

Implementation Method 1

oxidize HMF to FDCA or 2,5-diformylfuran (DFF) at ambient conditions

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 2

electrochemical and photoelectrochemical cells that oxidize HMF to FDCA

Methodology Applied
Scientific EffectElectrochemical oxidation: Electrolysis

Implementation Method 3

Photoelectrochemical cells (PECs) can directly utilize photogenerated electron-hole pairs in semiconductor electrodes

Methodology Applied
Scientific EffectPhotoexcitation: Photoelectric Effect

Implementation Method 4

as nature does through photosynthesis

Methodology Applied
Scientific EffectPhotosynthesis: Photosynthesis

Implementation Method 5

water oxidation to O2 is used as the anode reaction, which is environmentally benign and does not require additional species in the electrolyte

Methodology Applied
Scientific EffectWater oxidation: Oxidation

Implementation Method 6

In order to complete the circuit, oxidation reactions occur at the anode, consuming photogenerated holes

Methodology Applied
Scientific EffectPhotogenerated hole consumption: Photoelectric Effect

Data Source

PatentEP3242964B1Electrochemical and photoelectrochemical oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid and 2,5-diformylfuran
Publication Date: 2021.11.03 WISCONSIN ALUMNI RES FOUND
  • EP3242964B1 patent drawingFigure 1
  • EP3242964B1 patent drawingFigure 2A
  • EP3242964B1 patent drawingFigure 2B

AI summary

Electrochemical and photoelectrochemical cells for the oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid and/or 2,5-diformylfuran are provided. Also provided are methods of using the cells to carry out the electrochemical and photoelectrochemical oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid and/or 2,5-diformylfuran.