Epoxy-Amine Monolith for Chromatography Back Pressure Reduction

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Solution Overview

Problem

Conventional organic polymer monoliths for chromatographic use suffer from issues such as high back pressure at high flow rates, morphological changes due to compressibility, and difficulty in forming in columns with diameters of 1 mm or more, resulting in a small specific surface area and particle-aggregation-type monoliths with poor performance.

Innovation Solution

A monolith separation medium is developed with a skeletal phase composed of an addition polymer of a bi- or higher-functional epoxy compound and a bi- or higher-functional amine compound, specifically using 1,3-bis(N,N′-diglycidylaminomethyl)cyclohexane and a bi- or higher-functional amine, which undergoes polymerization at elevated temperatures to form a stable, co-continuous structure with interconnected pores, reducing shrinkage and allowing easy column filling.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional organic polymer monoliths are formed using hydrophobic monomer components and poor solvents, then gel formation occurs due to particle aggregation, but this results in a particle-aggregation-type monolith with large pore tortuosity factor and small specific surface area

Engineering Contradiction:
Improvemonolith formationVSAvoidmonolith structure uniformity
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent changes the chemical composition parameters by using hydrophilic monomer components instead of hydrophobic ones, and by adjusting the solvent system to include water-soluble porogens. This parameter change prevents particle aggregation and enables the formation of a uniform skeletal structure with controlled pore distribution, resolving the contradiction between ease of manufacture and structural precision.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs composite material design by combining hydrophilic monomers with water-soluble porogens in a specific ratio range (5:95 to 45:55 by weight). This composite approach creates a synergistic effect where the hydrophilic monomer forms the skeletal structure while the water-soluble porogen creates uniform pores, achieving both ease of manufacture and high structural precision simultaneously.

Inventive Principle:
Principle #40Composite materials

2Adaptability or versatility

If conventional organic polymer monoliths are used in columns with inner diameter of 1 mm or more, then they can be formed, but they peel off from the column tubes due to compressibility

Engineering Contradiction:
Improvecolumn size adaptabilityVSAvoidmonolith stability
Core Design Contradiction:
Adaptability or versatilityVSReliability

Solution Approach 1:

The patent modifies the physical parameters of the monolith by adjusting the monomer-to-porogen ratio and selecting specific hydrophilic monomers that form more compliant polymers. This changes the compressibility parameter, allowing the monolith to adapt to column tubes of various sizes (including 1 mm or more inner diameter) without peeling, thus improving both adaptability and reliability.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If conventional organic polymer monoliths are used at high flow rates, then separation can be performed, but back pressure increases due to large pore tortuosity factor

Engineering Contradiction:
Improveflow rateVSAvoidback pressure
Core Design Contradiction:
ProductivityVSStress or pressure

Solution Approach 1:

The patent changes the pore structure parameters by using water-soluble porogens that create more open and less tortuous pore networks. This parameter change reduces the pore tortuosity factor, allowing high flow rates to be maintained with lower back pressure, thus resolving the contradiction between productivity and pressure.

Inventive Principle:
Principle #35Parameter changes

4Ease of manufacture

If conventional organic polymer monoliths are used, then they can be formed, but they have morphological change due to compressibility

Engineering Contradiction:
Improvemonolith formationVSAvoidmorphological stability
Core Design Contradiction:
Ease of manufactureVSStability of the object's composition

Solution Approach 1:

The patent adjusts the polymer composition parameters by selecting hydrophilic monomers that form polymers with appropriate glass transition temperatures and cross-linking densities. This parameter change improves morphological stability, preventing compression-induced deformation while maintaining ease of manufacture in standard column formats.

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 resulting monolith separation medium achieves a high-performance, non-particle-aggregation-type co-continuous structure with reduced shrinkage and increased organic content, suitable for various-sized columns, offering improved chromatographic performance and stability compared to conventional monoliths.

Implementation Method 1

heating the solution to obtain a polymer

Methodology Applied
Scientific EffectPolymerization: Photopolymerisation

Implementation Method 2

stably cross-linking the polymer before a non-particle-aggregation-type co-continuous structure of the polymer and the porogen transits to a particle aggregation structure

Methodology Applied
Scientific EffectCross-linking: Chemical Bonding

Implementation Method 3

spinodally decomposing the porogen and the polymer

Methodology Applied
Scientific EffectSpinodal decomposition: Phase Change

Implementation Method 4

addition polymer of a bi- or higher-functional epoxy compound and a bi- or higher-functional amine compound

Methodology Applied
Scientific EffectAddition reaction: Chemical Bonding

Data Source

PatentUS8217094B2Monolith separation medium for chromatographic use and method of producing the same
Publication Date: 2012.07.10 SHIMADZU CORP
  • US8217094B2 patent drawing
  • US8217094B2 patent drawing
  • US8217094B2 patent drawing

AI summary

A monolith separation medium comprising a skeletal phase and continuous pores forming a three-dimensional network structure, which has a functional group enabling the introduction of a new functional group on the surface of the skeletal phase. The skeletal phase has an average diameter of a submicron to micrometer size and is in a co-continuous structure of the non-particle-aggregation type. It is composed of an addition polymer of 1,3-bis(N,N′-diglycidylaminomethyl)cyclohexane as an epoxy compound with a bifunctional or higher amine compound, is rich in organic matters and is free from any aromatic-origin carbon atom. Thus, it is an organic polymer monolith separation medium of the non-particle-aggregation type.