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Superficially porous materials comprising a substantially nonporous core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations

a technology of substantially nonporous core and particle size distribution, which is applied in the field of superficially porous materials comprising a substantially nonporous core having narrow particle size distribution, and the process for the preparation thereof, can solve the problems of low yield of narrow distribution, insufficient particle size (1-2 m) for effective use, and insufficient chromatographic enhancement of pore geometry. to achieve the effect of preventing fine generation, aggregation and agglomeration

Inactive Publication Date: 2013-05-09
WATERS TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The invention is a material that is better than conventional silica particles when exposed to high pH mobile phases. It can also be combined with other chemicals to improve its stability. The patent text also describes methods for preventing fines (small particles) from generating, aggregating, and agglomerating during certain chemical reactions. This can be achieved by adding ethanol solutions of alkoxysilane or organoalkoxysilanes at a slow and constant rate. Another method involves adding a secondary solution containing ethanol, water, and ammonium hydroxide in a similar manner.

Problems solved by technology

These particles do not have sufficient size (1-2 μm) for effective use in UPLC, nor do they contain chromatographically enhanced pore geometry.
Other surfactant-templated approaches, can yield low yields of narrow distribution, fully porous particles, however these approaches have not been used to prepare monodisperse, spherical superficially porous particles having chromatographically enhanced pore geometry.
The AMT process, as shown in FIG. 8, results in bumpy surface features and variation of the porous layer thickness.
Since hybrid materials are not thermally stable above 600° C., this approach is not applicable to the formation of hybrid superficially porous particles.
While the description of monodisperse superficially porous silica particles has been noted in the literature, these particles do not display chromatographically enhanced pore geometry and desirable pore diameters for many chromatographic applications.

Method used

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  • Superficially porous materials comprising a substantially nonporous core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations
  • Superficially porous materials comprising a substantially nonporous core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations
  • Superficially porous materials comprising a substantially nonporous core having narrow particle size distribution; process for the preparation thereof; and use thereof for chromatographic separations

Examples

Experimental program
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Effect test

example 1

[0518]Nonporous hybrid particles were formed following a modification of a reported process {Choi, J. Y.; Kim, C. H.; Kim, D. K. J. Am. Ceram. Soc., 1998, 81, 1184-1188. Seog, I. S; Kim, C. H. J. Mat. Sci., 1993, 28, 3277-3282}. To a clean 40 mL vial was added a stir bar, water (26 mL) and 14.8 M NH4OH (4.3 mL). This solution was then heated to 60° C. with stirring (600 rpm) in a water bath before one or more alkoxysilanes, including phenyltriethoxysilane (PTES, Gelest, Morrisville, Pa.), 1,8-bis(triethoxysilyl)octane (BTEO, Gelest, Morrisville, Pa.), 1,2-bis(triethoxysilyl)ethane (BTEE, Gelest, Morrisville, Pa.), 1,2-bis(methyldiethoxysilyl)ethane (BMDEE, Gelest, Morrisville, Pa.), vinyltriethoxysilane (VTES, Gelest, Morrisville, Pa.), or mercaptopropyltrimethoxysilane (MPTMS, Lancaster Chemical, Lancaster UK) were added (3 mL total). The reaction was sealed, and returned to the 60° C. water bath for 2 h. The reaction was further continued for 24 h at 25° C. The particles were isol...

example 2

[0519]Nonporous hybrid particles were formed following a modification of a reported process {U.S. Pat. Nos. 4,983,369 and 4,911,903}. To a clean Nalgene bottle (125 mL) was added a stir bar, water (14 mL), ethanol (80 mL), and NH4OH (7 mL, 14.8 M). One or more alkoxysilanes, including tetraethoxysilane (TEOS, Gelest, Morrisville, Pa.), phenyltriethoxysilane (PTES, Gelest, Morrisville, Pa.), or mercaptopropyltrimethoxysilane (MPTMS, Lancaster Chemical, Lancaster UK) were added with stirring (600 rpm, 4 mL, 25° C.). The reaction was sealed and the onset of turbidity was monitored. The formation of spherical particles was further monitored over 24 h by light microscopy. The particles were purified and isolated by repeated centrifugation from ethanol (3×100 mL) and water (3×100 mL). The particles were air dried for 12 h and then vacuum dried (70° C., 30 mm Hg) for 12 h. Carbon content was determined by combustion analysis. Average particle size was determined by SEM.

TABLE 2SilanesPartic...

example 3

[0520]Product 2c was thermally treated in an air muffled oven at 700° C. for 3 h. The resulting nonporous silica product (3a) had no organic content.

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Abstract

Novel chromatographic materials for chromatographic separations, columns, kits, and methods for preparation and separations with a superficially porous material comprising a substantially nonporous core and one or more layers of a porous shell material surrounding the core. The material of the invention is comprised of superficially porous particles and a narrow particle size distrution. The material of the invention is comprised of a superficially porous monolith, the substantially nonporous core material is silica; silica coated with an inorganic / organic hybrid surrounding material; a magnetic core material; a magnetic core material coated with silica; a high thermal conductivity core material; a high thermal conductivity core material coated with silica; a composite material; an inorganic / organic hybrid surrounding material; a composite material coated with silica; a magnetic core material coated with an inorganic / organic hybrid surrounding material; or a high thermal conductivity core material coated with an inorganic / organic hybrid surrounding material.

Description

RELATED APPLICATION[0001]This application claims the benefit of U.S. provisional application Ser. No. 61 / 367,797, filed Jul. 26, 2011, the entire disclosure of which is incorporate herein by this reference.BACKGROUND OF THE INVENTION[0002]Superficially porous particles (also called pellicular, fused-core, or core-shell particles) were routinely used as chromatographic sorbents in the 1970's. These earlier superficially porous materials had thin porous layers, prepared from the adsorption of silica sols to the surface of ill-defined, polydisperse, nonporous silica cores (>20 μm). The process of spray coating or passing a solution of sols through a bed of particles was commonly used. Kirkland extensively explored the use of superficially porous particles throughout this time and helped develop the Zipax brand of superficially porous materials in the 1970's. A review of Kirkland's career was provided by Unger (Journal of Chromatography A, 1060 (2004) 1).[0003]Superficially porous pa...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01J20/28B01J20/32
CPCB01J20/28054Y10T428/2991B01D15/20B01J20/283B01J20/285B01J20/3291B01J20/28071B01J20/286B01J20/3204B01J20/3219B01J20/3236B01J20/3257B01J20/3289B01J20/3293B01J20/28004B01J20/28057B01J20/3214
Inventor WYNDHAM, KEVIN D.MURIITHI, BEATRICE W.MORRIS, MICHAEL F.LAWRENCE, NICOLE L.
Owner WATERS TECH CORP
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