Preparation method of porous organic-inorganic hybrid silica microspheres

Abstract

The invention relates to a porous organic-inorganic hybridization silicon microsphere preparation method. The method comprises the following steps of (1) subjecting polyethyl silicate-40 and organosiloxane to hydrolytic polycondensation through acid catalysis to obtain hybridized pre-polymers; (2) building an emulsion system with the prepared pre-polymers serving as the dispersion phase, water-alcohol serving as the continuous phase and triton100-sodium lauryl sulfate serving as the emulsifying agent, performing further hydrolytic condensation on the pre-polymers in the alkaline condition and performing emulsion droplet curing to form balls to obtain organic-inorganic hybridization porous spherical silicon; (3) reaming the prepared hybridized silicon microspheres. The particle sizes of the prepared hybridized silicon microspheres range from microns to hundreds of microns, and the particle sizes are controllable.

Description

[0001] Technical field: [0002] The invention relates to a preparation method of silica gel microspheres, and further relates to a preparation method of porous organic-inorganic hybrid silica gel microspheres. [0003] Background technique: [0004] As a new type of material, organic-inorganic hybrid silica gel has a good application prospect in the field of adsorption and separation due to its unique physical and chemical properties, which has attracted extensive attention of researchers. As a chromatographic packing, the control of its morphology, particle size and pore structure is very important. The preparation methods of spherical silica mainly include spray drying method, polymer-induced colloidal aggregation method, sol-gel method and so on. At present, the preparation methods of organic-inorganic hybrid silica are mainly based on the sol-gel method for functional modification, including grafting method, co-condensation method, and periodic mesoporous silicone PMOs. ...

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Problems solved by technology

However, in most of the reported synthesis methods of organic-inorganic hybrid spherical silica, the spherical shape and pore structure of the material are difficult to meet the requirements of chromatographic stationary phase, and the prepared hybrid silica has a particle size of less than 3 μm and poor microsphere morphology. And it has a microporous structure, which limits the application of hybrid silica gel materials in chromatographic analysis

In 2006, C.Li et al. prepared phenyl hybrid ethyl bridged mesoporous organic silica gel by co-condensation method, and the phenyl content on the surface of the microspheres was 2.5 μmol / m 2 , the particle size distribution is 2-8μm, and the specific surface area is 601m 2 / g, but the average pore size is only 2.9nm, and the spherical shape of the microspheres is poor, and the surface is not smooth

In 2011, B.Di et al also prepared 3-8 μm aminopropyl hybrid ethyl bridging mesoporous organic silica gel by co-condensation method, with a specific surface area of ​​765m 2 / g, the average pore diameter is 4.09nm, the pore volume is 0.585cc / g, the surface amino coverage is 0.32mmol / g, about 0.4μmol / m 2 , although a higher specific surface area has been obtained, there is still a certain gap between the microsphere pore structure parameters and the silica gel matrix chromatography packing parameters and the microspheres are not round.

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