Preparation method of carbamate chromatographic filler with ion exchange characteristic
A carbamate, ion exchange technology, applied in the direction of anion exchanger materials, cation exchange materials, organic cation exchangers, etc., can solve problems such as the need for catalysts, high temperature, substrate alcohol steric hindrance sensitivity, etc., to reduce The effect of high silanol activity, high conversion and yield, and low reagent usage
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Embodiment 1
[0030] Example 1: Preparation of urethane-embedded octadecyl-bonded silica gel with cation exchange function
[0031] Step A: 18.94 g of octadecanol was dissolved in 100 mL of toluene, heated to 60 °C under mechanical stirring, and 11.35 g of N,N'-carbonyldiimidazole was rapidly added into it in small batches, and completed in 5 min, keeping the temperature below The reaction was changed for 1 hour, and then 15.50 g of 3-aminopropyltriethoxysilane was added dropwise, and the reaction was continued for 2 hours without changing the temperature.
[0032] Step B: Mix 50.0 g of activated silica gel (average diameter 5 μm, specific surface area 350 m2 g-1) with 150 mL of toluene, stir mechanically to form a slurry, and then add N-trimethoxysilylpropyl oxamide monomethyl ester 5 g was added to the reaction solution prepared in step A, heated to reflux under mechanical stirring for 24 hours, then vacuum filtered while hot, washed with boiling toluene, ethanol, 75% ethanol and methanol...
Embodiment 2
[0035] Example 2: Preparation of carbamate-embedded triaconyl-bonded silica gel with anion exchange function
[0036] Step A: 9.22 g of n-triacontanol was dissolved in 40 mL of acetonitrile, heated to 80°C under mechanical stirring, and 3.40 g of N,N'-carbonyldiimidazole was rapidly put into it in small batches, completed in 5 min, and the temperature was maintained. The reaction was kept unchanged for 1 hour, and then 3.78 g of 3-aminopropyltrimethoxysilane was added dropwise, and the reaction was continued for 2 hours without changing the temperature.
[0037] Step B: Mix 20.0 g of activated silica gel (average diameter 5 μm, specific surface area 350 m2 g-1) with 60 mL of toluene, stir mechanically to form a slurry, and then add 4 g of N-trimethoxysilylpropylethylenediamine It was added to the reaction solution obtained in step A, heated to reflux for 48 hours under mechanical stirring, then vacuum filtered while hot, washed with boiling acetonitrile, ethanol, 75% ethanol a...
Embodiment 3
[0040] Example 3: Preparation of bis-carbamate-embedded hexyl bidentate-bonded silica gel with anion exchange function
[0041] Step A: 11.83 g of 1,6-hexanediol was heated to 60°C under mechanical stirring in 100 mL of toluene, and 16.2 g of N,N'-carbonyldiimidazole was rapidly added into it in small batches, and completed in 5 minutes. , keep the temperature unchanged for 1 hour, then drop 35.8 g of 3-aminopropyltrimethoxysilane, and continue the reaction for 2 hours without changing the temperature.
[0042] Step B: Mix 70.0 g of activated silica gel (average diameter 10 μm, specific surface area 350 m2 g-1) with 250 mL of toluene, stir mechanically to form a slurry, and then add N-trimethoxysilylpropyl diethylenetriamine 5 g was added to the reaction solution prepared in step A, heated to reflux for 24 hours under mechanical stirring, then vacuum filtered while hot, washed with boiling toluene, ethanol, 75% ethanol and methanol in turn, and vacuum dried for 5 hours.
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