Polyether-Free Silica Stationary Phase for Hydrocarbon Separation

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Solution Overview

Problem

Chromatography columns, particularly MEMS columns, face challenges in achieving sufficient separation performance for light hydrocarbons with low retention times, leading to inaccurate monitoring of hydrocarbons and other components in mud gases during oil and gas drilling, due to residual polyethers in traditional silica-based stationary phases.

Innovation Solution

A silica-based stationary phase substantially free of polyethers is developed, using a sol-gel process that involves washing with an acid to remove polyethers, followed by neutralization and drying, resulting in a monolithic structure with enhanced separation capabilities for alkanes and other substances.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional silica-based stationary phase is used in chromatography column, then the column can be manufactured with standard sol-gel process, but residual polyethers in the stationary phase cause poor separation performance for light hydrocarbons

Engineering Contradiction:
Improveseparation performanceVSAvoidresidual polyethers
Core Design Contradiction:
Manufacturing precisionVSObject-generated harmful factors

Solution Approach 1:

The patent applies the extraction principle by removing residual polyethers from the silica-based stationary phase through acid washing. The sol-gel process incorporates polyethers as structure-directing agents, but these must be removed post-synthesis to achieve good separation performance. The acid treatment extracts the harmful polyether residues while preserving the silica structure, directly resolving the contradiction between manufacturing ease and separation performance.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent changes the chemical parameters of the stationary phase by controlling the silica network structure and removing polyether components. This involves adjusting the sol-gel process parameters and applying acid treatment to transform the stationary phase from polyether-containing to polyether-free, thereby improving separation performance for light hydrocarbons without compromising manufacturability.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If polyethers are removed from stationary phase to improve separation, then retention factors and resolution improve, but additional washing and neutralization steps are required

Engineering Contradiction:
Improveretention factor and resolutionVSAvoidnumber of processing steps
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies preliminary action by incorporating polyethers during the sol-gel synthesis process itself, rather than attempting to remove them from pre-formed stationary phases. The polyethers are present from the beginning to direct the gel structure formation, and their removal is then performed as a controlled post-synthesis treatment. This approach simplifies the overall process compared to alternative methods that would require more extensive purification steps.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes the chemical composition parameters of the stationary phase by systematically removing polyether components through acid washing followed by neutralization. This parameter change transforms the stationary phase from containing polyether residues to being substantially free of polyethers, achieving improved retention factors and resolution for light hydrocarbon separation.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If acid washing is performed to remove polyethers, then separation performance improves, but the stationary phase requires neutralization and additional drying time

Engineering Contradiction:
Improveseparation capabilityVSAvoidprocessing time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent changes the chemical state of the stationary phase through controlled acid washing, neutralization, and drying parameters. By optimizing these parameter changes, the process achieves substantial polyether removal and improved separation capability. The time investment in these steps is justified by the significant improvement in retention factors and resolution for light hydrocarbon analysis.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent converts the potentially harmful effect of extended processing time into a benefit by using the acid washing and neutralization steps to thoroughly remove polyether residues. The additional time invested in these purification steps directly translates to improved separation performance and more reliable analytical results, making the time expenditure worthwhile.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

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 silica-based stationary phase significantly improves the separation of hydrocarbons and other substances, enhancing retention factors and resolution, particularly for C1-C2 components, enabling continuous and accurate monitoring of mud gases during drilling operations.

Implementation Method 1

washing with an acid to substantially remove the polyethers from the polymerized sol-gel

Methodology Applied
Scientific EffectAcid washing:

Implementation Method 2

washing with a basic neutralization solvent

Methodology Applied
Scientific EffectNeutralization:

Implementation Method 3

drying the inside of the neutralized chromatography column to form a silica-based stationary phase substantially free of the polyethers

Methodology Applied
Scientific EffectDrying:

Data Source

PatentUS11491465B2Silica-based stationary phase for a chromatography column and methods for producing the same
Publication Date: 2022.11.08 GEOSERVICES EQUIP SAS
  • US11491465B2 patent drawing
  • US11491465B2 patent drawing
  • US11491465B2 patent drawing

AI summary

A silica-based stationary phase for chromatography columns and the methods of preparing such. More particularly, but not by way of limitation, a silica-based stationary phase that is substantially free of polyethers (e.g., polymer glycols). Also, a chromatography column comprising a silica-based stationary phase substantially free of polyethers (e.g., polymer glycols) within its channels as either a thin-film coating and/or a monolith and/or a monolithic coating. More particularly, a micro-electro-mechanical system (MEMS) chromatograph comprising a silica-based monolith substantially free of polyethers (e.g., polymer glycols) as the stationary phase within the micro-channels of the column.