Porous inorganic/organic hybrid particles for chromatographic separations and process for its preparation
First Claim
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1. A method of preparation of spherical, porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, comprising the steps ofa) prepolymerizing a mixture of one or more organoalkoxysilanes and a tetraalkoxysilane to produce a polyorganoalkoxysiloxane;
- b) preparing an aqueous suspension of said polyorganoalkoxysiloxane, said suspension further comprising a surfactant or combination of surfactants,c) gelling said aqueous suspension in the presence of a base catalyst so as to produce porous particles; and
d) modifying the pore structure of said porous particles by subjecting said porous particles to hydrothermal treatmentthereby preparing spherical porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry in which all pores of a diameter of about <
34 Å
contribute less than about 110 m2/g to the specific surface area of the particle.
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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 that offer more efficient chromatographic separations than that known in the art.
89 Citations
49 Claims
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1. A method of preparation of spherical, porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, comprising the steps of
a) prepolymerizing a mixture of one or more organoalkoxysilanes and a tetraalkoxysilane to produce a polyorganoalkoxysiloxane; -
b) preparing an aqueous suspension of said polyorganoalkoxysiloxane, said suspension further comprising a surfactant or combination of surfactants, c) gelling said aqueous suspension in the presence of a base catalyst so as to produce porous particles; and d) modifying the pore structure of said porous particles by subjecting said porous particles to hydrothermal treatment thereby preparing spherical porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry in which all pores of a diameter of about <
34 Å
contribute less than about 110 m2/g to the specific surface area of the particle.- View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30)
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31. A method of preparation of spherical, porous particles of hybrid silica having a chromatographically-enhancing pore geometry, comprising the steps of
a) prepolymerizing a mixture of one or more organoalkoxysilanes and a tetraalkoxysilane in the presence of an acid catalyst to produce a polyorganoalkoxysiloxane; -
b) preparing an aqueous suspension of said polyorganoalkoxysiloxane, said suspension further comprising a surfactant or combination of surfactants, and gelling in the presence of a base catalyst so as to produce porous particles; and c) modifying the pore structure of said porous particles by hydrothermal treatment, thereby preparing porous particles of hybrid silica having a chromatographically-enhancing pore geometry in which all pores of a diameter of about <
34 Å
contribute less than about 110 m2/g to the specific surface area of the particle.- View Dependent Claims (32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48)
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49. A method of preparation of spherical, porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry, comprising the steps of
a) prepolymerizing a mixture of one or more organoalkoxysilanes and a tetraalkoxysilane to produce a polyorganoalkoxysiloxane; -
b) preparing an aqueous suspension of said polyorganoalkoxysiloxane, said suspension further comprising a surfactant or combination of surfactants, c) gelling said aqueous suspension in the presence of a base catalyst so as to produce porous particles; and d) modifying the pore structure of said porous particles by subjecting said porous particles to hydrothermal treatment thereby preparing spherical porous inorganic/organic hybrid particles having a chromatographically-enhancing pore geometry in which; all pores of a diameter of about <
34 Å
contribute less than about 110 m2/g to the specific surface area of the particle;said particles have a specific surface area of about 75 to 600 m2/g; and said particles have an average pore diameter of about 100 to 300 Å
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Specification