Method for preparation of perfectly spherical particles of silic

Details Method for preparation of perfectly spherical particles of silic Method for preparation of perfectly spherical particles of silic

1976-07-23

1978-08-01

Cooper, Jack

Chemistry of inorganic compounds

Silicon or compound thereof

Oxygen containing

252317, 252448, 252451, C01B 3316

Patent

active

041043634

ABSTRACT:
The invention relates to a method for preparation of perfectly spherical particles of silicagel with controlled particle size and controlled pore diameter, which are suitable as packings for high-speed liquid chromatography and gel permeation chromatography. Free liquid silicic acid is obtained by acidifying of solutions of alkaline metal silicates in organic solvents by organic acids miscible with water in the presence of higher amine as an emulsifier and polymerized to hydrogel in the form of spherical particles. These are isolated and partially hardened by heating above 100.degree. C in a neutral organic medium, e.g. amyl acetate or dibutyl sebacate, to remove a part of water by distillation, then subjected to hydrothermal processing with water under pressure at a temperature above 150.degree. C and eventually stabilized. Chromatographic beds of silicagel particles prepared in this way may be used both with aqueous and organic eluants and exhibit very low spreading of zones and high separation efficiency comparable with commercial styrene-divinyl-benzene gels.

REFERENCES:
patent: 1772055 (1930-08-01), Miller et al.
patent: 2395524 (1946-02-01), Weiser et al.
patent: 2474910 (1949-07-01), Pierce et al.
patent: 2782869 (1957-02-01), Gray
patent: 3321276 (1967-05-01), Burzynski et al.
patent: 3647709 (1972-03-01), Hill
patent: 3819811 (1974-06-01), Aboutboul et al.

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