Graphitic Carbon Chromatography for Polyolefin Separation

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Solution Overview

Problem

Current HPLC methods for analyzing polyolefin polymers suffer from limited separation efficiency and long analysis times, particularly when dealing with amorphous polyolefin polymers, as existing techniques like TREF and CRYSTAF are inadequate for these materials.

Innovation Solution

A method and apparatus for one-dimensional chromatography using a liquid chromatography stationary phase comprising graphitic carbon, with the introduction of a temperature and/or solvent gradient to enhance separation efficiency, specifically employing a temperature gradient device and solvent gradient device in conjunction with a stationary phase containing graphitic carbon and inert fillers like glass spheres.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If traditional HPLC methods with silica or zeolite stationary phases are used for polyolefin polymer analysis, then analysis can be performed, but separation efficiency is limited

Engineering Contradiction:
Improveseparation efficiencyVSAvoidanalysis capability for amorphous polymers
Core Design Contradiction:
Measurement precisionVSReliability

Solution Approach 1:

The patent changes the stationary phase material from silica or zeolite to graphitic carbon, fundamentally altering the surface chemistry and interaction mechanisms. This parameter change enables effective separation of polyolefin polymers including amorphous types by providing appropriate adsorption characteristics that match the polymer properties

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses graphitic carbon as a composite stationary phase material that combines specific structural properties (layered graphite structure) with chromatographic functionality. This composite approach creates a stationary phase with enhanced separation capabilities for polyolefin polymers compared to traditional single-material phases

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 analysis time is relatively long

Engineering Contradiction:
Improvechemical composition distribution 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 stationary phase. This substitution allows separation based on chemical composition distribution to occur through adsorption-desorption processes rather than slow crystallization- melting cycles, significantly reducing analysis time while maintaining analytical capability

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

Solution Approach 2:

The patent changes the fundamental separation mechanism from thermal fractionation to chromatographic adsorption by using graphitic carbon stationary phase. This parameter change in the separation mechanism enables faster analysis while preserving the ability to analyze chemical composition distribution and expand capability to amorphous polymers

Inventive Principle:
Principle #35Parameter changes

3Measurement precision

If graphitic carbon stationary phase is used with temperature gradient, then separation efficiency is improved, but device complexity increases

Engineering Contradiction:
Improveseparation efficiencyVSAvoidtemperature gradient device
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent employs a temperature gradient device that serves multiple functions: controlling polymer solubility during injection, optimizing adsorption equilibrium on the graphitic carbon stationary phase, and enhancing separation efficiency. This multi-functional approach justifies the added device complexity by providing several benefits within a single system component

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 improves separation efficiency and reduces analysis time for polyolefin polymers, enabling more precise analysis of polyolefin polymers by varying the retention factor based on monomer to co-monomer ratios, offering a faster and more efficient method compared to traditional techniques like TREF and CRYSTAF.

Implementation Method 1

liquid chromatography stationary phase comprising graphitic carbon

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 2

graphitic carbon stationary phase

Methodology Applied
Scientific EffectPi-pi interactions:

Implementation Method 3

wherein the solution introduced into the liquid chromatography stationary phase is subjected to a temperature gradient

Methodology Applied
Scientific EffectTemperature gradient: Temperature Gradient

Implementation Method 4

wherein the solution is subjected to a solvent gradient and a temperature gradient

Methodology Applied
Scientific EffectSolvent gradient:

Data Source

PatentEP2516033B1Chromatography of polyolefin polymers using a graphitic carbon stationary phase
Publication Date: 2017.07.05 DOW GLOBAL TECHNOLOGIES LLC

AI summary

The invention provides a method for one-dimensional chromatography of a polyolefin polymer, comprising introducing a solution of the polyolefin polymer into a liquid flowing through a liquid chromatography stationary phase, the liquid chromatography stationary phase comprising graphitic carbon, and wherein the polyolefin polymer emerging from the liquid chromatography stationary phase has a retention factor greater than zero, and wherein the solution introduced into the liquid chromatography stationary phase is subjected to a temperature gradient, and/or the solution is subjected to a solvent gradient. The invention also provides a method for multi-dimensional chromatography of a polyolefin polymer, comprising introducing a solution of the polyolefin polymer into a liquid flowing through a first liquid chromatography stationary phase or a field flow fractionation device, and subsequently flowing the solution through a second liquid chromatography stationary phase, the second liquid chromatography stationary phase comprising graphitic carbon, and wherein the polyolefin polymer emerging from the liquid chromatography stationary phase has a retention factor greater than zero. The invention also provides an apparatus for polyolefin polymer chromatography, comprising a liquid chromatography stationary phase, the liquid chromatography stationary phase comprising graphitic carbon and at least one inert filler.