Spray Oxidation of HMF to FDCA via Pressure-Controlled Cooling

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current methods for producing 2,5-furandicarboxylic acid (FDCA) from hexoses like fructose and glucose face challenges such as low conversion rates, side reactions leading to by-products, and catalyst deactivation due to self-polymerization and degradation of hydroxymethylfurfural (HMF) at elevated temperatures, along with difficulties in recycling and disposing of acidic catalysts.

Innovation Solution

A process involving a catalytically effective combination of cobalt, manganese, and bromide components is used to oxidize a sprayable feed containing a crude dehydration product of a natural hexose, where the exothermic temperature rise is controlled by selecting and managing the reactor pressure, allowing for high yields of FDCA without the need for HMF isolation or derivatization, and utilizing acetic acid as a solvent that vaporizes to provide evaporative cooling.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Speed

If HMF is oxidized at elevated temperatures to produce FDCA, then the reaction rate improves, but catalyst deactivation occurs due to self-polymerization and degradation of HMF

Engineering Contradiction:
Improvereaction rateVSAvoidcatalyst stability
Core Design Contradiction:
SpeedVSReliability

Solution Approach 1:

The patent changes the physical state parameter of the reaction system by using spray oxidation to create a aerosol dispersion of HMF droplets in the gas phase, rather than conducting the reaction in liquid phase. This parameter change allows the oxidation to proceed at elevated temperatures (200-400°C) without the catalyst deactivation problems associated with liquid phase reactions, as the HMF does not undergo self-polymerization in the spray oxidation environment

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent replaces the traditional liquid phase oxidation mechanism with a gas phase spray oxidation mechanism. Instead of using liquid catalysts or dissolved oxygen in liquid medium, the invention uses a spray nozzle to atomize the HMF-containing liquid into fine droplets that are suspended in a gas phase oxidant atmosphere, fundamentally changing the reaction mechanism to avoid catalyst deactivation

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

2Ease of manufacture

If acid-based dehydration methods are used to produce HMF from hexoses, then the conversion process is established, but low conversion rates and formation of by-products occur

Engineering Contradiction:
Improveprocess establishmentVSAvoidconversion rate
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

The patent modifies the dehydration process parameters by using organic acid catalysts (such as sulfonic acids) in organic solvents or neat conditions, rather than traditional aqueous mineral acids. This parameter change in catalyst type and reaction medium improves HMF conversion rates and selectivity while reducing by-product formation compared to conventional acid-based methods

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs strong oxidants including molecular oxygen from air, ozone, hydrogen peroxide, or peracetic acid in the oxidation step. These strong oxidants accelerate the conversion of HMF to FDCA, improving productivity and conversion rates while maintaining the benefits of the spray oxidation approach

Inventive Principle:
Principle #38Strong oxidants (Accelerated oxidation)

3Ease of manufacture

If inorganic acids are used for HMF production, then the catalyst is inexpensive, but recycling and disposal become difficult

Engineering Contradiction:
Improvecatalyst costVSAvoidcatalyst recycling
Core Design Contradiction:
Ease of manufactureVSEase of operation

Solution Approach 1:

The patent employs organic acid catalysts that can be easily separated and regenerated through simple processes such as distillation or extraction. These catalysts, while potentially more expensive than inorganic acids, offer the advantage of being recoverable and reusable multiple times, eliminating the disposal problems associated with inorganic acids and reducing overall process costs through catalyst longevity

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

4Ease of operation

If solid acid resins are used as catalysts, then catalyst recycling is improved, but deactivating humin polymers form on the resin surface

Engineering Contradiction:
Improvecatalyst recyclingVSAvoidcatalyst activity
Core Design Contradiction:
Ease of operationVSReliability

Solution Approach 1:

The patent uses homogeneous organic acid catalysts in the spray oxidation process, which are easily separated from the product stream through condensation and phase separation. These catalysts do not suffer from the humin polymer deposition problems that plague solid acid resins, maintaining their catalytic activity over multiple cycles and eliminating the need for complex resin regeneration procedures

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

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 unexpectedly high yields of FDCA, minimizing yield losses and degradation, and allows for the recovery of FDCA as a substantially pure solid product, overcoming previous limitations in commercial-scale production.

Implementation Method 1

utilizing acetic acid as a solvent that vaporizes to provide evaporative cooling

Methodology Applied
Scientific EffectEvaporative cooling: Evaporation

Implementation Method 2

a catalytically effective combination of cobalt, manganese and bromide components for catalyzing the oxidation of the furanic substrate

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 3

reacting the furanic substrate and the oxidant in the presence of the cobalt, manganese and bromide components to form 2,5-furandicarboxylic acid

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 4

limiting the exothermic temperature rise due to the reaction, through a selection and control of the operating pressure within the reactor vessel

Methodology Applied
Scientific EffectPressure control: Pressure Increase

Data Source

PatentEP2750789B1Spray oxidation process for producing 2,5-furandicarboxylic acid from hydroxymethylfurfural
Publication Date: 2018.07.11 ARCHER DANIELS MIDLAND CO
  • EP2750789B1 patent drawingFigure 1
  • EP2750789B1 patent drawing

AI summary

A process is provided for carrying out an oxidation on a sprayable feed including a furanic substrate to be oxidized and a catalytically effective combination of cobalt, manganese, and bromide components for catalyzing the oxidation of the furanic substrate, which process comprises spraying the feed into a reactor vessel as a mist, supplying an oxidant, reacting the furanic substrate and the oxidant, and managing the exothermic temperature rise due to the reaction through a selection and control of the operating pressure within the reactor vessel. A crude dehydration product from the dehydration of fructose, glucose or both, including 5-hydroxymethylfurfural, can be directly oxidized by the process to produce 2,5-furandicarboxylic acid in surprisingly increased yields.