Porous inorganic/organic hybrid particles for chromatographic separations and process for its preparation
AssigneeWaters Investments Limited
InventorsZhiping Jiang, Raymond P. Fisk
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Abstract
Novel material for chromatographic separations, processes for its preparation, and separations devices containing the chromatographic material. In particular, the disclosure describes porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, which desirably may be surface modified, and which offer more efficient chromatographic separations than that known in the art.
Claims96
A porous inorganic/organic hybrid material, comprising porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry.
A method of preparation of porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, comprising the steps of
- forming porous inorganic/organic hybrid particles;
- and
- modifying the pore structure of said porous particles, forming inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry.
A separations device having a stationary phase comprising porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry.
A chromatographic column having improved life, comprising
- a) a column having a cylindrical interior for accepting a packing material, and
- b) a packed chromatographic bed comprising porous particles of hybrid silica of the formula SiO2/(R2pR4qSiOt)n, wherein R2 and R4 are independently C1-C18 alkyl or aryl moiety, p and q are 0, 1 or 2, provided that p+q=1 or 2, and that when p+q=1, t=1.5, and when p+q=2, t=1;
- and n is a number from 0.1 to 1, said porous hybrid silica chromatographic matrix having a chromatographically-enhancing pore geometry and average pore diameters of from about 100 to 300 Å, and said porous particles of hybrid silica have been surface modified.
A method of preparation of porous particles of hybrid silica having a chromatographically-enhancing pore geometry, comprising the steps of
- a) prepolymerizing a mixture of an organotrialkoxysilane and a tetraalkoxysilane in the presence of an acid catalyst to produce a polyalkyloxysiloxane;
- b) preparing an aqueous suspension of said polyalkyloxysiloxane, said suspension further comprising a surfactant, and gelling in the presence of an base catalyst so as to produce porous particles;
- and
- c) modifying the pore structure of said porous particles by hydrothermal treatment.
The method of claim 70 wherein the molar ratio of said organotrialkoxysilane and tetraalkoxysilane is from about 0.5:1 to 0.2:1.
Porous particles of hybrid silica having a chromatographically-enhancing pore geometry, produced by the process of
- a) prepolymerizing a mixture of an organotrialkoxysilane and a tetraalkoxysilane in the presence of an acid catalyst to produce a polyalkyloxysiloxane;
- b) preparing an aqueous suspension of said polyalkyloxysiloxane, said suspension further comprising a surfactant, and gelling in the presence of an base catalyst so as to produce porous particles;
- and
- c) modifying the pore structure of said porous particles by hydrothermal treatment, forming hybrid silica particles having a chromatographically-enhancing pore geometry.
Dependencies are inferred from the claim text.