Micro-channel Reactor for Continuous HMF Synthesis

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Solution Overview

Problem

Current technologies for synthesizing 5-hydroxymethylfurfural (HMF) from glucose suffer from low selectivity, high by-product formation, and poor catalyst stability, along with an inability to precisely control residence time in batch reactors.

Innovation Solution

A method utilizing a micro-channel reactor with FeCl3 and HCl as homogeneous catalysts in the aqueous phase and methyl butyl ketone as the organic phase for in-situ HMF extraction, allowing for continuous synthesis of HMF with improved selectivity and yield.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Loss of time

If batch reactor is used for HMF synthesis from glucose, then the reaction process is simple to operate, but the residence time cannot be precisely controlled and the reaction time is long (tens of hours)

Engineering Contradiction:
Improvereaction timeVSAvoidoperation simplicity
Core Design Contradiction:
Loss of timeVSEase of operation

Solution Approach 1:

The patent replaces the traditional batch reactor mechanical system with a micro-channel reactor system that uses continuous flow and precise pumping to control residence time. The micro-channel reactor enables precise control of reaction parameters through its small scale and continuous operation mode, reducing reaction time from tens of hours to significantly shorter durations while maintaining operational control through automated flow systems.

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

Solution Approach 2:

The patent changes key reaction parameters by transitioning from batch to continuous flow operation in a micro-channel reactor. This enables precise control of residence time, temperature, and catalyst concentration, allowing the reaction to be optimized for faster HMF production while maintaining selectivity and reducing by-products through controlled continuous processing.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional catalysts are used for HMF synthesis, then the catalyst system is simple, but the HMF selectivity is low and by-products are high

Engineering Contradiction:
ImproveHMF selectivityVSAvoidcatalyst system complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent employs a composite catalyst system combining FeCl3 and HCl in the aqueous phase, which works synergistically to enhance HMF selectivity. This composite catalyst approach allows for precise control of the dehydration reaction of fructose intermediates, achieving high HMF selectivity and minimizing by-product formation through the combined catalytic effects of the iron salt and strong acid.

Inventive Principle:
Principle #40Composite materials

Solution Approach 2:

The patent uses methyl butyl ketone as an intermediary organic phase that extracts HMF in-situ during the reaction. This intermediary phase selectively extracts HMF from the aqueous reaction mixture, preventing further degradation and side reactions, thereby enhancing HMF selectivity and yield while simplifying the overall process by combining reaction and extraction in one system.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If long reaction time is used in batch reactor, then complete conversion is achieved, but HMF selectivity decreases and by-products increase

Engineering Contradiction:
ImproveHMF selectivityVSAvoidreaction efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent implements continuous extraction of HMF into the organic phase (methyl butyl ketone) during the reaction process. This continuous removal of HMF from the aqueous phase prevents over-reaction and degradation, maintaining high HMF selectivity throughout the reaction. The continuous operation also enables steady-state conditions that improve productivity compared to batch processing.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent extracts HMF in-situ into the organic phase (methyl butyl ketone) during the reaction, removing the product from the reaction environment. This extraction prevents further degradation of HMF to by-products like levulinic acid and formic acid, maintaining high selectivity. The dual-phase system allows the reaction to proceed efficiently while continuously removing the desired product.

Inventive Principle:
Principle #2Taking out (Extraction)

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 method significantly reduces reaction time to less than 30 minutes, enhances HMF selectivity, minimizes by-product formation, and provides a stable and controllable continuous operation, resulting in high yield and improved process efficiency.

Implementation Method 1

FeCl3 and HCl are used as homogeneous catalysts in the aqueous phase

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 2

methyl butyl ketone is used as the organic phase for in-situ HMF extraction

Methodology Applied
Scientific EffectLiquid-liquid extraction: Liquid-Liquid Extraction

Data Source

PatentUS12234214B2Method for continuously synthesizing 5-hydroxymethylfurfural by using micro-channel reactor
Publication Date: 2025.02.25 CHINA CONSTRUCTION INDUSTRIAL & ENERGY ENGINEERING GROUP CO LTD
  • US12234214B2 patent drawing

AI summary

The present discloses relates to a method for continuously synthesizing 5-hydroxymethylfurfural by using a micro-channel reactor, which belongs to the technical field of micro-chemical engineering. The method includes: separately conveying an aqueous glucose solution, which contains FeCl3 and HCl, and methyl butyl ketone to a T-shaped micro-mixer, the T-shaped micro-mixer being in communication with a capillary tube; then enabling an aqueous glucose solution phase and a methyl butyl ketone phase to flow in the capillary tube in a segmented flow manner while performing an HMF synthesis reaction; and collecting a reaction product flowing out of the capillary tube, wherein HMF generated by the reaction is present in an organic phase of the reaction product. The method is easy to operate, has a controllable process, high product yield, a low by-product amount and a short synthesis period, and is a green method for efficient and continuous synthesis of HMF.