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Nanometer size chemical modified materials and uses

a chemical modification and nanometer technology, applied in the field of nanometer size chemical modification materials and uses, can solve the problems of high surface coverage and high hydrolytic stability of stationary phases, remain virtually unexplored in the field of separation, use of poss grafted, etc., to improve hydrolytic stability, increase hydrophobicity, and high ligand coverage

Inactive Publication Date: 2012-08-16
DIONEX CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0006]POSS-containing stationary phase materials for chromatography exhibit several benefits compared to those prepared by conventional methods using sitylating reagents, e.g., improved hydrolytic stability, increased hydrophobicity, high ligand coverage and unique selectivity (increased shape selectivity, increase hydrophobic selectivity). In addition, the commercial availability of a range of useful POSS compounds at economical costs makes them a viable approach for developing novel stationary phases. However, until the present inventions, POSS-based materials were not used as surface modifying agents for stationary supports for chromatography,
[0009]A particular advantage provided by POSS is that a single molecule can provide up to five times the surface coverage relative to that provided by comparable silane coupling agents applied in the hypothetical monolayer fashion where R=cyclohexyl. Thus, POSS bonded phases have high ligand density, which leads to better hydrolytic stability and higher hydrophobic retention than similar stationary phases prepared by silylation.

Problems solved by technology

While sitylating reagents with diverse functional groups are commercially available, making stationary phases with high surface coverage and high hydrolytic stability remains challenging.
Although POSS compounds are well-characterized and widely used, they remain virtually unexploited in the field of separations.
One report describes the use of a POSS cross-linker used in an inorganic-organic hybrid monolithic column, however, these workers do not describe the use of a POSS grafted to a solid support as a stationary phase for chromatography.

Method used

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  • Nanometer size chemical modified materials and uses
  • Nanometer size chemical modified materials and uses
  • Nanometer size chemical modified materials and uses

Examples

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Effect test

example 1

[0171]1) Functionalization-General Conditions

General Synthetic Procedure of Making T7-POSS Bonded Phases 42-49

[0172]A selected T7R7(OH)3-POSS compound is dissolved in an appropriate high boiling point solvent in a round bottom flask. A suitable quantity of silica gel is dispersed in this solution. After reflux for 24 to 96 hours, the reaction mixture is filtered. The cake is then washed with sufficient quantity of a suitable solvent in which the POSS compound can be dissolved. The resulting material is dried in a vacuum oven at 60° C. for 12 hours.

[0173]Alternatively, a T7R7(OH)3-POSS compound is dissolved in an appropriate low boiling point solvent in a round bottom flask. Then a suitable quantity of silica gel is dispersed in this solution. After carefully removing all volatiles on a rotovap under reduced pressure, the resulting substance is heated at 160° C. for 12 hours. Then the reaction mixture is filtered and the cake is washed with sufficient quantity of a suitable solvent i...

example 2

Synthesis of iso-Butyl-T7 POSS Phase (43)

[0177]10 g Trisilanolisobutyl POSS (3) is dissolved in 100 mL of decane in a 200-mL round bottom flask. 10 g of raw silica gel (5.0 μm; specific surface area, 300 m2 / g; mean pore size, 120 Å; pore volume, 1.00 mL / g) is dispersed in this solution. After reflux for 72 hours, the reaction mixture is filtered. The cake is then washed with sufficient quantity of heptane. The resulting material is dried in a vacuum oven at 60° C. for 12 hours. The elemental analysis yields a carbon content of 7.01%, which corresponds to a ligand density of 3.88 μmol / m2.

example 3

Synthesis of iso-Octyl-T7 POSS Phase (44)

[0178]10 g Trisilanolisobutyl POSS (4) is dissolved in 100 mL of decane in a 200-mL round bottom flask. 10 g of raw silica gel (5.0 μm; specific surface area, 300 m2 / g; mean pore size, 120 Å; pore volume, 1.00 mL / g) is dispersed in this solution. After reflux for 72 hours, the reaction mixture is filtered. The cake is then washed with sufficient quantity of heptane. The resulting material is dried in a vacuum oven at 60° C. for 12 hours. The elemental analysis yields a carbon content of 9.37%, which corresponds to a ligand density of 3.85 μmol / m2.

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Abstract

There are provided ligand compositions and stationary phases comprising a polyhedral oligomeric silsequioxane moiety. Also provided are chromatographic devices comprising the stationary phases, and methods of making and using the ligands, stationary phases and chromatographic devices of the invention.

Description

CROSS-REFERENCE TO RELATED APPLICATION(S)[0001]This application is a nonprovisional application of and claims priority of U.S. Provisional Application No. 61 / 442,752, filed on Feb. 14, 2011.BACKGROUND OF THE INVENTION[0002]For liquid chromatography applications, selectivity and hydrolytic stability of the stationary phase are the most important aspects. Silylating reagents have been widely used for modifying solid supports, including silica gel, for liquid chromatography and many other applications. While sitylating reagents with diverse functional groups are commercially available, making stationary phases with high surface coverage and high hydrolytic stability remains challenging.[0003]Polyhedral oligomeric silsequioxanes (POSS) are a class of nanometer size compounds with high symmetry, good chemical and thermal stability, and ready commercial availability. They find use as nanometer-scale building blocks to improve the properties of a broad range of materials including medical ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01D15/08C08F236/20C07F7/21B01J20/286
CPCB01J20/286B01J20/287B01J20/289C07F7/21B01J20/3246B01J20/3257B01J2220/54B01J20/3219G01N1/405
Inventor LIU, XIAODONGPOHL, CHRISTOPHER A.
Owner DIONEX CORP
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