Silica gel chromatographic filler and its preparation method and application
A silica gel chromatography and silica gel technology, applied in chemical instruments and methods, analytical materials, material separation, etc., can solve problems such as poor reproducibility, low stability of HILIC chromatography packing, and unsatisfactory lifespan, achieving good results and easy scale The effect of chemical production and good stability
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[0043] The preparation method of this silica gel chromatographic filler is set forth in detail below:
[0044] Firstly, the silica gel is activated and pretreated to obtain activated silica gel with silanol groups on the surface. The silica gel is preferably fully porous spherical silica gel, more preferably ultra-high purity fully porous spherical silica gel for chromatography. The particle size of the raw silica gel used for activation is preferably 3-20 μm, and the pore size is preferably The specific surface area is preferably 200-400m 2 / g. But the present invention is not limited thereto, and can be adjusted according to actual needs.
[0045] In some embodiments, the silica gel activation pretreatment process includes: adding an aqueous solution of hydrofluoric acid with a mass concentration of 0.04-0.08% to the silica gel, and refluxing to prepare the activated silica gel; the mass of the silica gel and hydrogen The volume ratio of the hydrofluoric acid aqueous so...
Embodiment 1
[0055] This example is used to illustrate the preparation of the silica gel chromatography filler of the present invention.
[0056] figure 1 It is a schematic diagram of the method for preparing silica gel chromatography filler in Example 1. Concrete preparation method comprises the following steps:
[0057] (1) Add 100 g of silica gel (5 μm, purchased from DAISO, Japan) into a 2 L glass reaction vessel, add 1000 mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 1000mL of hydrofluoric acid aqueous solution with a mass ratio of 0.08%, stir for 24 hours, wash with distilled water until neutral, finally add 1000mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;
[0058] (2) Add 400mL of acetone solution, 30.0g of 1,3-propane sultone, and 25.0g of 4-aminobutyltrimethoxysilane to a 1L glass reaction vessel in sequence, and stir for 14 hours at room temperature at 25°C; After the reaction, put the q...
Embodiment 2
[0064] This example is used to illustrate the preparation of the silica gel chromatography filler of the present invention.
[0065] (1) Add 100 g of silica gel (5 μm, purchased from DAISO, Japan) into a 2 L glass reaction vessel, add 1000 mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 1000mL of hydrofluoric acid aqueous solution with a mass ratio of 0.08%, stir for 24 hours, wash with distilled water until neutral, finally add 1000mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;
[0066] (2) Add 400mL of acetone solution, 30.0g of 1,3-propane sultone, and 25.0g of 3-aminopropylisopropyldiethoxysilane to a 1L glass material reaction vessel in sequence, at room temperature at 25°C Stir the reaction for 14 hours; after the reaction, put the qualitative filter paper into the Buchner funnel to filter under reduced pressure, and collect the filter cake to obtain the sulfamic acid silane;
[0067]...
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