Ultraporous sol gel monoliths

• US 7,595,350 B2
• Filed: 09/11/2008
• Issued: 09/29/2009
• Est. Priority Date: 12/20/2004
• Status: Active Grant

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Varian Incorporated (Agilent Technologies, Inc.)
• Inventors: Xu, Dengfeng
• Primary Examiner(s): Kugel; Timothy J.
• Application Number:
  US12/209,061
• Publication Number:
  US 20090008327A1
• Time in Patent Office: 383 Days
• Field of Search: 516/110, 516/111, 516/100, 210/656, 436/161
• US Class Current: 516/111
• CPC Class Codes: B01D 15/26 characterised by the separation mechanism
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28047 Gels
• CPC Class Codes: B01J 20/28057 Surface area, e.g. B.E.T specific surface area
• CPC Class Codes: B01J 20/28069 Pore volume, e.g. total pore volume, mesopore volume, micropore volume
• CPC Class Codes: B01J 20/282 Porous sorbents ion exchange B01J39/00 - B01J41/00
• CPC Class Codes: B01J 20/286 Phases chemically bonded to a substrate, e.g. to silica or to polymers
• CPC Class Codes: B01J 20/291 Gel sorbents
• CPC Class Codes: B01J 21/08 Silica
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: B01J 2220/82 Shaped bodies, e.g. monoliths, plugs, tubes, continuous beds
• CPC Class Codes: B01J 35/56 Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
• CPC Class Codes: C04B 2111/00793 as filters or diaphragms
• CPC Class Codes: C04B 2111/0081 as catalysts or catalyst carriers
• CPC Class Codes: C04B 2111/00836 for medical or dental applications
• CPC Class Codes: C04B 2111/00844 for electronic applications
• CPC Class Codes: C04B 35/515 based on non-oxide ceramics
• CPC Class Codes: C04B 35/553 based on fluorides
• CPC Class Codes: C04B 38/0045 by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
• CPC Class Codes: C04B 38/0054 the pores being microsized or nanosized
• CPC Class Codes: C04B 38/0074 : expressed as porosity percentage

Abstract

Ultraporous sol gel monoliths and methods for preparing the same are provided, having superior flow characteristics for chromatography and analytical chemistry applications. The methods for forming an ultra porous sol-gel monolith include (a) forming a solution comprising a porogen, a matrix dissolving catalyst and a sol gel precursor; (b) allowing the solution to form a gel; and (c) drying the gel at an elevated temperature. The ultraporous sol gel monoliths are characterized by a porosity of up to about 97%, a BET surface area of at least about 50 m²/g and substantially no micropores.

Claims

1. A method of separating a mixture of analytes, comprising applying the mixture of analytes to a sol gel monolith having a total porosity of up to about 97% with substantially no pores having diameters less than about 2.0 nm;

and eluting the analytes using a mobile phase.

2. The method of claim 1, wherein the method of separating is thin layer chromatography, high performance liquid chromatography, reversed phase chromatography, normal phase chromatography, ion chromatography, ion pair chromatography, reverse phase ion pair chromatography, ion exchange chromatography, affinity chromatography, hydrophobic interaction chromatography, size exclusion chromatography, chiral recognition chromatography, perfusion chromatography, electrochromatography, partition chromatography, microcolumn liquid chromatography, capillary chromatography, capillary zone electrophoresis (CZE), nano-LC, open tubular liquid chromatography (OTLC), capillary electrochromatography (CEC), liquid-solid chromatography, preparative chromatography, hydrophilic interaction chromatography, supercritical fluid chromatography, precipitation liquid chromatography, bonded phase chromatography, fast liquid chromatography, flash chromatography, liquid chromatography-mass spectrometry, gas chromatography, microfluidics based separations, chip based separations, or solid phase extraction separations.