Organic Acid Thermal Treatment of Purified FDCA for Spherical Particles

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Solution Overview

Problem

Existing purification processes for 2,5-furandicarboxylic acid (FDCA) fail to adequately remove impurities such as 2-furancarboxylic acid (FCA) and mono alkyl esters, leading to undesirable mechanical and physical properties like plate-like shapes, fines, and agglomeration, which hinder efficient handling and polymerization.

Innovation Solution

A thermal treatment process is introduced, involving mixing purified FDCA with a treatment solvent at elevated temperatures to achieve a controlled dissolution of FDCA, followed by cooling to precipitate improved particle shapes and sizes, enhancing purity and mechanical properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If comprehensive purification processes (hydrogenation, oxidation, distillation, recrystallization) are applied to crude FDCA, then the purity of FDCA is improved, but the mechanical and physical properties of the particles deteriorate (plate-like shapes, fines, agglomeration)

Engineering Contradiction:
Improvepurity of FDCAVSAvoidmechanical properties of particles
Core Design Contradiction:
Manufacturing precisionVSStrength

Solution Approach 1:

The patent applies parameter changes by controlling the dissolution temperature (100-200°C) and the composition of the aqueous medium (pH, ionic strength, specific ions like Ca²⁺, Mg²⁺, Na⁺, K⁺, Cl⁻, SO₄²⁻, PO₄³⁻) to achieve controlled dissolution and subsequent precipitation. This transforms the particle morphology from plate-like to spherical shapes with reduced fines and improved mechanical strength, while maintaining high purity levels.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes phase transitions by dissolving purified FDCA at elevated temperatures and then cooling the solution to induce precipitation. This phase change process (solid→liquid→solid) enables the formation of spherical particles with improved mechanical properties and reduced agglomeration, while the controlled dissolution-precipitation cycle maintains high purity.

Inventive Principle:
Principle #36Phase transitions

2Manufacturing precision

If conventional purification methods are used, then 5-formyl-2-furancarboxylic acid (FFCA) is effectively removed, but other impurities (2-furancarboxylic acid FCA, mono alkyl esters) remain in significant amounts

Engineering Contradiction:
Improveremoval of FFCAVSAvoidamount of remaining impurities
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent employs parameter changes by adjusting the dissolution temperature and aqueous medium composition to selectively dissolve FDCA while leaving impurities like FCA and mono alkyl esters in the solid phase or in the mother liquor. The specific pH, ionic strength, and ion composition are optimized to enhance the solubility difference between FDCA and impurities, enabling their separation upon cooling and filtration.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If solid FDCA particles are obtained with conventional processes, then the product can be isolated, but the particles exhibit undesirable properties (fines, agglomerates, poor flowability) that complicate handling and storage

Engineering Contradiction:
Improveisolation of solid productVSAvoidhandling and storage properties
Core Design Contradiction:
Ease of manufactureVSEase of operation

Solution Approach 1:

The patent applies parameter changes by controlling the dissolution temperature (100-200°C), cooling rate, and aqueous medium composition to generate spherical particles with uniform size distribution and reduced fines. These morphological changes significantly improve flowability, reduce agglomeration, and enhance handling properties while maintaining ease of isolation through filtration or centrifugation.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent explicitly applies spheroidality by inducing the formation of spherical particles through controlled dissolution and precipitation. The spherical morphology reduces particle interlocking, improves flowability, minimizes agglomeration, and enhances handling and storage properties compared to plate-like particles, while the process remains simple and integrated into the purification sequence.

Inventive Principle:
Principle #14Spheroidality (Curvature)

4Manufacturing precision

If thermal treatment at elevated temperatures is applied, then particle morphology and purity are improved, but energy consumption increases

Engineering Contradiction:
Improveparticle morphology and purityVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The patent optimizes the dissolution temperature range (100-200°C) to achieve the desired particle morphology and purity improvement while minimizing energy consumption. The process utilizes moderate temperature elevation rather than extreme heating, and the aqueous medium composition is optimized to enhance solubility at these moderate temperatures, reducing the thermal energy requirement compared to conventional high-temperature treatments.

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

The process significantly reduces FCA and FDCA-Me impurities, resulting in spherical particles with favorable size distribution, improving handling and polymerization efficiency, while being resource-efficient and safe.

Implementation Method 1

mixing purified FDCA with a treatment solvent at elevated temperatures to achieve a controlled dissolution of FDCA

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 2

cooling to precipitate improved particle shapes and sizes

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 3

A thermal treatment process is introduced, involving mixing purified FDCA with a treatment solvent at elevated temperatures

Methodology Applied
Scientific EffectHeating: Heating

Data Source

PatentUS12365660B2Organic acid and thermal treatment of purified 2,5-furandicarboxylic acid
Publication Date: 2025.07.22 FURANIX TECH BV
  • US12365660B2 patent drawing
  • US12365660B2 patent drawing

AI summary

Thermal treatment of purified FDCA for producing a carboxylic acid composition, the process including the steps of providing or producing a thermal treatment composition including a purified carboxylic acid composition and an organic acid containing treatment solvent composition; subjecting the thermal treatment composition to an elevated temperature, where the FDCA is partially dissolved, and cooling the treated composition and separating at least a portion of the FDCA from the treated composition to obtain a carboxylic acid composition.