Multi-capillary Lining Manufacturing via Controlled Hydrolysis

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Solution Overview

Problem

Existing methods for manufacturing multicapillary packings for chromatography face challenges in producing conduits fine enough for certain applications without introducing cracks and fissures.

Innovation Solution

A method involving the assembly of ablative preforms into a bundle, followed by the creation of a gel through hydrolysis of an organometallic precursor, and finally ablating the preforms to form conduits within the gel, while controlling the amount of water used to minimize defects.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If ablative preforms are used to create fine conduits in chromatography packings, then the required conduit fineness is achieved, but cracks and fissures appear in the packing structure

Engineering Contradiction:
Improveconduit finenessVSAvoidstructural integrity
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent changes the water-to-precursor ratio parameter from conventional high ratios to a specific low ratio range (0.5-2 times stoichiometric amount). This parameter change modifies the gelation kinetics and pore structure formation, enabling fine conduits to be created without generating cracks and fissures that normally appear when using ablative preforms for fine conduit fabrication.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite gel structure by combining organometallic precursor with controlled water amounts to form a homogeneous gel matrix that can accommodate ablative preforms. This composite approach allows the gel to maintain structural integrity while being processed to create fine conduits, resolving the contradiction between conduit fineness and structural integrity.

Inventive Principle:
Principle #40Composite materials

2Stability of the object's composition

If conventional sol-gel process is used with high water content, then complete hydrolysis of organometallic precursor is achieved, but cracks and fissures are generated in the gel structure

Engineering Contradiction:
Improvehydrolysis completenessVSAvoidgel structural integrity
Core Design Contradiction:
Stability of the object's compositionVSReliability

Solution Approach 1:

The patent fundamentally changes the water content parameter from conventional high levels to a precisely controlled low level (0.5-2 times stoichiometric amount). This parameter change achieves complete hydrolysis of the organometallic precursor while preventing the excessive pore formation and structural stress that cause cracks and fissures in conventional high-water sol-gel processes.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent applies partial hydrolysis control by limiting water to exactly what is needed (0.5-2 times stoichiometric amount) rather than using excess water. This controlled partial action achieves sufficient hydrolysis for complete precursor conversion while avoiding the excessive pore formation and structural degradation that occur with conventional excess water approaches.

Inventive Principle:
Principle #16Partial or excessive action

3Reliability

If monolithic structure is prepared without defects, then packing reliability is improved, but the manufacturing process becomes more difficult

Engineering Contradiction:
Improvepacking reliabilityVSAvoidprocess difficulty
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent simplifies the manufacturing process by changing the water-to-precursor ratio parameter to a low range (0.5-2 times stoichiometric amount). This single parameter change simultaneously achieves complete precursor hydrolysis and prevents crack formation, making it easier to manufacture defect-free monolithic structures compared to conventional methods that require complex process control to avoid defects.

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 method effectively produces multicapillary packings with minimal cracking and fissures, achieving high silica density and mechanical strength, thus enhancing the packing's performance in chromatography applications.

Implementation Method 1

creating a gel between the ablative preforms of the bundle by hydrolysis of an organometallic precursor in the presence of an amount of water not exceeding ten times the stoichiometric amount required for complete hydrolysis

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

ablation of the preforms, preferably by pyrolysis, oxidation, vaporization, melting and draining, mechanical extraction or chemical etching

Methodology Applied
Scientific EffectPyrolysis: Pyrolysis

Data Source

PatentEP4175746B1Method for manufacturing a multi-capillary lining
Publication Date: 2025.05.28 SEPARATIVE
  • EP4175746B1 patent drawingFigure 1
  • EP4175746B1 patent drawingFigure 2
  • EP4175746B1 patent drawing

AI summary

The present disclosure relates to a method for manufacturing multi-capillary lining that can serve as a chromatographic column, and to the multi-capillary packing obtained by such a method.