Graphitic Carbon HPLC for Polyolefin Copolymer Separation

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Solution Overview

Problem

Current HPLC methods for analyzing polyolefin polymers suffer from limited separation efficiency, particularly for amorphous polymers, and require lengthy analysis times, which are not adequately addressed by existing techniques like TREF and CRYSTAF.

Innovation Solution

The use of a graphitic carbon stationary phase in HPLC systems for polyolefin polymer analysis, allowing for improved separation efficiency by varying retention factors based on monomer to comonomer ratios in copolymers, and enabling differentiation between atactic, isotactic, and syndiotactic polypropylene.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If traditional silica-based HPLC methods are used for polyolefin polymer analysis, then the analysis can be performed, but the separation efficiency is limited

Engineering Contradiction:
Improveseparation efficiencyVSAvoidanalysis accuracy
Core Design Contradiction:
Measurement precisionVSReliability

Solution Approach 1:

The patent changes the chemical composition parameter of the stationary phase from traditional silica-based materials to graphitic carbon, fundamentally altering the interaction mechanisms with polyolefin polymers. This parameter change enables significantly improved separation efficiency while maintaining analysis reliability through the unique properties of graphitic carbon surfaces.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs graphitic carbon as a composite stationary phase material that combines the benefits of carbon's chemical inertness with graphitic structure's unique surface properties. This composite approach allows for enhanced polymer separation efficiency while providing a stable and reliable analysis platform for polyolefin copolymers.

Inventive Principle:
Principle #40Composite materials

2Measurement precision

If TREF or CRYSTAF methods are used for polyolefin polymer analysis, then chemical composition distribution can be analyzed, but the analysis time is relatively long

Engineering Contradiction:
Improvechemical composition analysisVSAvoidanalysis time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent replaces the thermal fractionation mechanism of TREF and CRYSTAF with a chromatographic separation mechanism using graphitic carbon HPLC. This substitution eliminates the need for temperature cycling and crystallization processes, dramatically reducing analysis time while maintaining the ability to analyze chemical composition distribution and polymer tacticity.

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

3Productivity

If conventional HPLC stationary phases are used, then analysis speed can be maintained, but separation efficiency remains limited

Engineering Contradiction:
Improveanalysis speedVSAvoidseparation efficiency
Core Design Contradiction:
ProductivityVSMeasurement precision

Solution Approach 1:

The patent changes the stationary phase material parameter to graphitic carbon, which fundamentally improves the separation efficiency for polyolefin copolymers. This parameter change enables the system to achieve both high analysis speed and high separation efficiency simultaneously, resolving the trade-off between productivity and measurement precision.

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

This approach significantly enhances separation efficiency and reduces analysis time, providing a more precise determination of monomer to comonomer ratios and polymer tacticity, outperforming traditional silica-based methods.

Implementation Method 1

introducing a solution of the polyolefin polymer into a liquid mobile phase flowing through a liquid chromatography stationary phase, the liquid chromatography stationary phase comprising graphitic carbon, the polyolefin polymer emerging from the liquid chromatography stationary phase with a retention factor greater than zero

Methodology Applied
Scientific EffectAdsorption: Adsorption

Data Source

PatentEP2754474B1Chromatography of polyolefin copolymers
Publication Date: 2017.04.19 DOW GLOBAL TECHNOLOGIES LLC
  • EP2754474B1 patent drawingFigure 1
  • EP2754474B1 patent drawingFigure 2
  • EP2754474B1 patent drawingFigure 3

AI summary

The present invention relates to an apparatus for determining the monomer to comonomer ratio of a copolymer wherein the apparatus comprises a high temperature liquid chromatography unit equipped with a graphitic carbon liquid chromatography column, a pump, a polymer solution, and a means for an additional fractionation by size exclusion chromatography or asymmetric flow field flow fractionation, added after the fractionation by the graphitic column.