Preparation method for silica gel-loaded aminomethylpyridine chelating resin for deep copper removal
An aminomethylpyridine, chelating resin technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of low nucleophilic substitution reaction efficiency, low functional group loading, low halogen group loading efficiency, etc., To achieve the effect of simple and economical synthesis route, fast adsorption speed and good mechanical strength
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Embodiment 1
[0033] Embodiment 1 adopts different aprotic solvents to prepare silica gel-loaded aminomethylpyridine chelating resin
[0034] (1) Take 30g of chromatographically packed silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.
[0035] (2) Mix 20ml of 2-aminomethylpyridine, 30ml of triethylamine and 30ml of aprotic solvent into a three-necked bottle and heat up to 50-90°C. Then, under mechanical stirring, use a constant pressure dropping funnel to add a mixture of 50ml 3-chloropropyltrimethoxysilane coupling agent and 30ml aprotic solvent drop by drop, keep the temperature at 50-90°C, and reflux in a nitrogen atmosphere for 6- 18h. After the reaction, the triethylamine hydrochloride crystals were remo...
Embodiment 2
[0039] Embodiment 2 adopts different inert organic solvents to prepare silica gel-loaded aminomethylpyridine chelating resin
[0040] (1) Take 30g of chromatographically packed silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.
[0041] (2) 20ml of 2-aminomethylpyridine, 30ml of triethylamine and 30ml of dimethyl sulfoxide were evenly mixed and added into the three-necked flask, and the temperature was raised to 90°C. Then, under mechanical stirring, a mixture of 50ml of 3-chloropropyltrimethoxysilane coupling agent and 30ml of aprotic solvent was added dropwise with a constant pressure dropping funnel, and the temperature was kept at 90°C, and the nitrogen atmosphere was refluxed for 18h. After t...
Embodiment 3
[0045] Embodiment 3 adopts different organic bases to prepare silica gel-loaded aminomethylpyridine chelating resin
[0046] (1) Take 30g of chromatographically packed silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.
[0047] (2) 20ml of 2-aminomethylpyridine, 30ml of triethylamine and 30ml of dimethyl sulfoxide were evenly mixed and added into the three-necked flask, and the temperature was raised to 90°C. Then, under mechanical stirring, a mixture of 50ml of 3-chloropropyltrimethoxysilane coupling agent and 30ml of aprotic solvent was added dropwise with a constant pressure dropping funnel, and the temperature was kept at 90°C, and the nitrogen atmosphere was refluxed for 18h. After the reacti...
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