Microcrystalline Cellulose Sol-Gel Sorbents for High pH Stability

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Solution Overview

Problem

Silica-based liquid chromatography (LC) stationary phases suffer from limited pH stability, low thermal stability, and adsorption issues with basic compounds due to unreacted silanol groups, leading to irreproducible results and limited high-temperature applications.

Innovation Solution

Microcrystalline cellulose particles with sol-gel sorbent coating technology are used to create SPE sorbents and LC stationary phases, providing expanded pH stability (1-13) and high thermal stability (up to 350°C), eliminating acidic Si—OH bonds and enabling high-temperature liquid chromatography with water as the mobile phase.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If silica-based stationary phases are used, then good mechanical strength and high surface area are achieved, but pH stability is limited (maximum stable pH range of 2-9)

Engineering Contradiction:
Improvemechanical strengthVSAvoidpH stability
Core Design Contradiction:
StrengthVSStability of the object's composition

Solution Approach 1:

The patent changes the fundamental material parameter from silica to microcrystalline cellulose, which inherently has different chemical stability properties. Cellulose substrates with sol-gel coated stationary phases achieve stable operation across pH 1-13, resolving the pH stability limitation of silica phases while maintaining mechanical integrity through the cellulose support structure.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite structure combining microcrystalline cellulose particles with sol-gel coated stationary phases. This composite approach integrates the mechanical strength and surface area benefits of cellulose supports with the chemical stability provided by the sol-gel coating, achieving both mechanical and chemical stability across wide pH ranges.

Inventive Principle:
Principle #40Composite materials

2Area of stationary object

If silica-based stationary phases are used, then high surface area is achieved, but thermal stability is low (maximum operating temperature about 60°C)

Engineering Contradiction:
Improvesurface areaVSAvoidthermal stability
Core Design Contradiction:
Area of stationary objectVSTemperature

Solution Approach 1:

The patent changes the material composition from silica to microcrystalline cellulose-based sol-gel systems, fundamentally altering the thermal stability parameter. The sol-gel coated cellulose stationary phases maintain stable chromatographic performance at temperatures up to 350°C, enabling high-temperature liquid chromatography while preserving high surface area for efficient separations.

Inventive Principle:
Principle #35Parameter changes

3Strength

If silica substrate is used, then good mechanical strength is achieved, but unreacted silanol groups cause adsorption issues with basic compounds

Engineering Contradiction:
Improvemechanical strengthVSAvoidadsorption of basic compounds
Core Design Contradiction:
StrengthVSObject-generated harmful factors

Solution Approach 1:

The patent extracts and eliminates the problematic silanol groups from the stationary phase composition by using microcrystalline cellulose as the substrate instead of silica. The cellulose-based sol-gel system does not generate the same harmful silanol groups that cause unwanted adsorption of basic compounds, thereby removing this harmful factor while maintaining mechanical strength through the cellulose support.

Inventive Principle:
Principle #2Taking out (Extraction)

4Productivity

If conventional silica LC stationary phases are used, then column efficiency is achieved at room temperature, but column-to-column irreproducibility occurs

Engineering Contradiction:
Improvecolumn efficiencyVSAvoidcolumn-to-column reproducibility
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent changes the material composition from conventional silica to microcrystalline cellulose with sol-gel coating, which provides more consistent and reproducible column performance. The standardized cellulose substrate and sol-gel coating process eliminate the variability in silanol group content that causes column-to-column irreproducibility, while maintaining high column efficiency through the preserved surface area and pore structure.

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 solution offers improved stability and selectivity, allowing for efficient separation of compounds across a wide pH range and high temperatures, reducing the need for organic solvents and enhancing column efficiency and detection sensitivity.

Implementation Method 1

sol-gel sorbent coating technology as the polymer/sorbent immobilization technology

Methodology Applied
Scientific EffectSol-gel process: Sol

Implementation Method 2

The silica surface contains both silanols (Si—OH) and siloxanes (Si—O—Si) bonds as shown in FIG. 1. Silanol groups are strong adsorption sites

Methodology Applied
Scientific EffectAdsorption: Adsorption

Data Source

PatentUS20220016600A1Microcrystalline cellulose particle supported sol-gel sorbents
Publication Date: 2022.01.20 FLORIDA INTERNATIONAL UNIVERSITY
  • US20220016600A1 patent drawing
  • US20220016600A1 patent drawing
  • US20220016600A1 patent drawing

AI summary

Solid phase extraction (SPE) sorbents and liquid chromatography (LC) stationary phases are provided, as well as methods of fabricating the same. The SPE sorbents and LC stationary phases can use microcrystalline cellulose particles as the substrate and sol-gel sorbent coating technology as the polymer/sorbent immobilization technology. The SPE sorbents and LC stationary phases are stable in a pH range of 1-13 and at a temperature of up to 350 ° C.