A kind of spiral polymer functionalized silica microsphere chiral stationary phase and its preparation and application
A technology of chiral stationary phase and silica gel microspheres, which is applied in the direction of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., and can solve the problems of inability to separate and identify chiral compounds, backwardness, and differences in distribution and metabolism And other issues
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[0026] Preparation of hand -fixed phase:
[0027] 1) Activation of silicon microspheres: Take 1.0G silicon microspheres (2.9-3.2 μm) scattered in 30 mL hydrochloric acid solution (3mol L (3mol L) under the action of ultrasound. -1 ) In the middle of 110 ° C, the reflux reaction was 12h. Use the sand core funnel to filter the silicon pipe, and use ultra -pure water and methanol to wash silicon balls in turn, and then dry it in a vacuum drying box of 80 ° C for 24h;
[0028] 2) Silicon microsphere surface connection: Take step 1) 1.0g in the 1.0G has been activated to the 30ml dry toluene under ultrasound, add 0.6g of Silicidine O- The base) -N- (triangular oxyxyxanel propylene) amino methyl acid ester, 100 μL water-free triamine, and reaches the reaction of 24h at 120 ° C through nitrogen protection. After the reaction is over, stir and cool to room temperature, and then use toluene and methanol to wash the silicon balls in turn, and dry it in a vacuum drying box at 100 ° C for 24h...
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