FDCA Particle Morphology for Better Slurry Flow in PEF Polymerization

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Solution Overview

Problem

The existing preparation methods for 2,5-furandicarboxylic acid (FDCA) particles result in uneven distribution, poor flowability, and homogeneity of the slurry mixture with ethylene glycol, leading to extended reaction times, increased impurities, and high power consumption during polymerization processes.

Innovation Solution

The development of 2,5-furandicarboxylic acid particles with an average particle size of 50-200µm, loose bulk density of 0.7-1.0g/mL, and repose angle of 25-40°, achieved through a preparation method involving high-pressure reactor processing with controlled temperature, stirring, and cooling, which enhances particle sphericity and flowability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If thermal treatment method involving dissolving FDCA in treatment solvent composition during heat treatment is used to improve particle shape and strength, then particle shape and strength are improved, but FDCA particle yield is low due to difficult control of chemical equilibrium and exchange

Engineering Contradiction:
Improveparticle shape and strengthVSAvoidFDCA particle yield
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention changes the physical-chemical parameters of the system by replacing organic treatment solvents with supercritical carbon dioxide, transforming the dissolution-extraction mechanism. This parameter change allows precise control over the extraction process while maintaining high particle yield, resolving the contradiction between particle quality improvement and productivity

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention uses supercritical carbon dioxide as an inert extraction medium that does not participate in chemical reactions with FDCA. This inert environment prevents unwanted chemical equilibrium shifts and side reactions, enabling both high particle yield and improved particle morphology without the complexity of controlling chemical exchanges

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

2Manufacturing precision

If additives are added to regulate crystal particle size of FDCA, then particle size can be controlled within certain range, but crystallization purity is reduced and method becomes more complex

Engineering Contradiction:
Improveparticle size controlVSAvoidmethod complexity and purity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention extracts and removes the need for crystallization additives by using supercritical carbon dioxide extraction. This taking out approach eliminates the complexity and purity issues associated with additives while maintaining precise particle size control through the extraction process itself

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention replaces the chemical mechanism (additives affecting crystallization) with a physical mechanism (supercritical fluid extraction). This substitution removes the need for chemical additives, simplifying the process and maintaining high crystallization purity while achieving desired particle size distribution

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

3Ease of operation

If excess ethylene glycol is used relative to stoichiometric amount of FDCA to improve slurry properties and reaction uniformity, then slurry flowability and reaction uniformity are improved, but impurities and energy consumption increase

Engineering Contradiction:
Improveslurry flowability and reaction uniformityVSAvoidimpurities and energy consumption
Core Design Contradiction:
Ease of operationVSObject-generated harmful factors

Solution Approach 1:

The invention changes the particle size distribution parameters of FDCA to an optimized range, which fundamentally alters the slurry rheology. This parameter change allows achieving good slurry flowability and reaction uniformity with stoichiometric or near-stoichiometric ethylene glycol, eliminating the need for excess glycol and thus reducing impurities and energy consumption

Inventive Principle:
Principle #35Parameter changes

4Productivity

If particle size distribution of FDCA is not optimized, then handling is simpler, but slurry characteristics are poor leading to extended reaction times and increased by-product formation

Engineering Contradiction:
Improvereaction time and by-product formationVSAvoidparticle size distribution control
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The invention performs preliminary action by optimizing the particle size distribution of FDCA before the polymerization reaction. The supercritical carbon dioxide extraction process pre-establishes the ideal particle size distribution, ensuring excellent slurry characteristics and complete reaction, thereby preventing extended reaction times and by-product formation

Inventive Principle:
Principle #10Preliminary action

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 optimized FDCA particles improve the slurry's flowability and homogeneity, reducing the need for excess ethylene glycol, shortening polymerization reaction time, and lowering diethylene glycol impurities in polyethylene furanoate (PEF) production.

Implementation Method 1

stirring and heating, with a heating time of 2-4 h, so that the system temperature rises from room temperature to 100-150°C

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 2

adding 2,5-furandicarboxylic acid raw material into a high-pressure reactor, introducing deionized water into the high-pressure reactor to obtain a mixed liquid

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 3

the pressure of the system in the high-pressure reactor is 0.5-2.0 MPa

Methodology Applied
Scientific EffectPressure Increase: Pressure Increase

Implementation Method 4

stirring and heating, with a stirring rate of 200-400rpm

Methodology Applied
Scientific EffectStirring: Stirring

Implementation Method 5

after the heat preservation, cooling down to room temperature

Methodology Applied
Scientific EffectCooling: Cooling

Data Source

PatentEP4656631A12,5-furandicarboxylic acid particles, preparation method therefor, and use thereof
Publication Date: 2025.12.03 HEFEI LEAF BIOTECH CO LTD
  • EP4656631A1 patent drawingFigure 1
  • EP4656631A1 patent drawingFigure 2
  • EP4656631A1 patent drawing

AI summary

The present application discloses 2,5-Furandicarboxylic Acid particles and a preparation method and application thereof, belonging to the technical field of polymerization reaction bio-based monomer preparation. Using 2,5-Furandicarboxylic Acid as raw material, after high-temperature dissolution in water, cooling, filtration, and drying, the FDCA particles exhibit an almost non-angular appearance, with smooth and rounded surface, high sphericity, good dispersibility, average particle diameter of 50-200µm, loose bulk density of 0.7-1.0g/mL, and repose angle of 25-40°. The present application improves the flowability of FDCA slurry by modifying the microscopic morphology and particle size distribution of FDCA solid particles, which facilitates the uniformity of materials during the polymerization process and shortens the polymerization reaction time. Additionally, it reduces the equivalent usage of ethylene glycol and helps lower the impurity content of diethylene glycol.