Preparation method of humic acid bonded silica gel
A technology of bonding silica gel and humic acid, which is applied in the field of analytical chemistry, can solve the problems of small surface coverage, cumbersome preparation steps, unstable humic acid-modified silica gel stationary phase, etc., and achieve the effect of stable performance and simple method
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Embodiment 1
[0019] Embodiment 1: Preparation of humic acid bonded silica gel stationary phase
[0020] (1) Preparation of amino-bonded silica gel (APTS): Take 2.5g of vacuum-dried silica gel in a 100ml three-necked flask, add 50mL of anhydrous toluene and 0.25g of 3-aminopropyltrimethoxysilane, stir magnetically, and N 2 Heated to reflux in an oil bath at 100°C in an atmosphere, reacted for 24 hours, cooled, filtered with suction, washed with toluene and acetone in turn, and dried in vacuum at 60°C for 5 hours before use.
[0021] (2) Synthesis of the acid chloride compound (HAC) of humic acid: take humic acid (average molecular weight is 6000, China Pharmaceutical Group, Shanghai, China) solid 0.5g in a 50mL round bottom flask, add thionyl chloride 5mL, oil Heat the bath under reflux and stir to react for 24 hours. Distill under reduced pressure to distill off all the thionyl chloride and other low-boiling point reaction products. The remaining solid is the acid chloride compound of hum...
Embodiment 2
[0024] (1) Preparation of amino-bonded silica gel (APTS): Take 10.0 g of vacuum-dried chromatographic silica gel in a 250 mL three-neck flask, add 100 mL of anhydrous toluene and 0.1 g of 3-aminopropyltrimethoxysilane, and magnetically stir , at N 2 Heated to reflux in an oil bath at 120°C in an atmosphere, reacted for 12 hours, cooled, filtered with suction, washed with toluene and acetone in turn, and dried in vacuum at 60°C for 5 hours before use.
[0025] (2) Synthesis of the acid chloride compound (HAC) of humic acid: get humic acid (molecular weight is 40000, Alfa Aesar company, the U.S.) solid 2.0g in 50mL round bottom flask, add thionyl chloride 20mL, N2 In the atmosphere, the oil bath was heated to reflux and stirred for 24 hours, and then distilled under reduced pressure to distill off all the thionyl chloride and other low-boiling point reaction products. The remaining solid was the acid chloride compound of humic acid, which was dissolved by adding 100mL of DMF and ...
Embodiment 3
[0028] (1) Preparation of bonded silica gel (APTS): Take 2.0 g of vacuum-dried silica gel in a 250 mL three-necked flask, add 30 mL of treated anhydrous toluene and 1.0 g of 3-aminopropyltrimethoxysilane, and magnetically Stirring, in N 2 Heated to reflux in an oil bath at 100°C in an atmosphere, reacted for 24 hours, cooled, filtered with suction, washed with toluene and acetone in turn, and dried in vacuum at 120°C for 5 hours before use.
[0029] (2) Extraction of humic acid: Add 50 g of sodium humate (Shenyang Tianji Materials Co., Ltd.) into 500 mL of 0.2 mol / L HCl solution and stir, then let stand and pour off the supernatant. After washing the precipitate to neutrality, add it to 500mL 0.5mol / L NaOH solution, shake it properly for 24 hours, let it stand overnight, and centrifuge to separate the soy sauce-like solution, which is the sodium humate solution, and then add the concentration of 0.1mol / L (50-200ml) of hydrochloric acid is used for acid analysis, and after the...
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