Purifying PFPE Carboxylates via Batch Chromatography

Solution Overview

Problem

Current methods for purifying polydispersed perfluoropolyethers (PFPEs) carboxylates with high average functionality and molecular weight are inefficient and require multiple steps, especially when dealing with mixtures containing non-functional and functional PFPEs, as existing chromatographic techniques are not suitable for achieving high purity.

Innovation Solution

A batch chromatography process involving a mixture of non-functional and functional PFPEs with a solid phase and fluorinated organic solvent at ambient conditions, followed by separation and optional washing steps, effectively increases the average functionality of PFPE carboxylates by adsorbing higher functionality species and desorbing them with a mixture of alcohol and fluorinated solvent.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional chromatographic techniques are used to purify PFPE carboxylates, then separation of functional and non-functional species is attempted, but the process requires multiple steps and is inefficient for polydispersed mixtures with high molecular weight

Engineering Contradiction:
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The invention changes the chemical parameters of the system by introducing a basic substance (amine or ammonia) to react with PFPE carboxylates, transforming them into salts with different solubility characteristics. This parameter change enables single-step purification by filtration, dramatically improving productivity while reducing process complexity compared to conventional multi-step chromatographic methods

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention extracts functional PFPE carboxylates from polydispersed mixtures by converting them into insoluble salts through reaction with basic substances. The salts are then separated by filtration, effectively taking out the functional species from non-functional PFPEs in a single operation, thereby improving purification efficiency without requiring complex multi-step processes

Inventive Principle:
Principle #2Taking out (Extraction)

2Manufacturing precision

If multiple purification steps are used to achieve high purity PFPE carboxylates, then separation precision improves, but processing time and operational complexity increase

Engineering Contradiction:
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention segments the purification process into two distinct operations: (1) reaction of PFPE carboxylates with basic substances to form salts, and (2) filtration to separate salts from non-functional PFPEs. This segmentation achieves high purity in a single step, eliminating the need for multiple sequential purification steps and thereby reducing processing time while maintaining manufacturing precision

Inventive Principle:
Principle #1Segmentation

3Manufacturing precision

If conventional separation methods are applied to polydispersed PFPE mixtures, then some separation is achieved, but the methods are not suitable for achieving high functionality and purity simultaneously

Engineering Contradiction:
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The invention creates a composite system combining PFPE carboxylates with basic substances (amines or ammonia) to form salt complexes. This composite approach exploits the differential solubility and reactivity of functional versus non-functional species, enabling simultaneous achievement of high functionality and purity in polydispersed mixtures through a single filtration step, greatly simplifying the manufacturing process

Inventive Principle:
Principle #40Composite materials

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 process conveniently achieves high average functionality and molecular weight PFPE carboxylates, even with polydispersed mixtures, allowing for efficient purification and recovery of functional groups, particularly suitable for industrial-scale applications.

Implementation Method 1

contacting a mixture (M) of non-functional PFPEs and functional PFPEs carboxylates with high number average molecular weight, said mixture (M) having functionality (F), with a solid phase and a fluorinated organic solvent at ambient conditions to obtain a suspension (S) of a solid phase having adsorbed onto it a mixture (M1) of functional PFPE carboxylates with functionality (F1) higher than (F)

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 2

adding the solid phase with a mixture of an alcohol and a fluorinated organic solvent to obtain a suspension (S2) of the solid phase in a liquid phase, said liquid phase having mixture (M1) therein dissolved

Methodology Applied
Scientific EffectDesorption: Desorption

Data Source

PatentEP2914358B1Process for the purification of (PER)fluoropolyethers with carboxylate end groups
Publication Date: 2017.03.08
  • EP2914358B1 patent drawing
  • EP2914358B1 patent drawing
  • EP2914358B1 patent drawing

AI summary

The invention relates to a batch chromatography process the purification of (per)fluoropolyether (PFPE) carboxylates, in particular to a process for increasing the average functionality of PFPE carboxylates mixtures.