Straw-based hydrogel adsorbent for efficiently removing heavy metal ions and preparation method thereof
A technology of hydrogel adsorbent and heavy metal ions, which is applied in the fields of alkali metal compounds, chemical instruments and methods, adsorption water/sewage treatment, etc., can solve the problems of straw-based adsorbent removal inconvenience, etc. Gentle, easily controlled effect
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Embodiment 1
[0042] The rice straw (RS) was crushed and cleaned by ultrasonic treatment with ethanol and acetone, and then dried in an oven.
[0043] Dip 20 g of dried rice straw into a modified solution containing 20 g of 2-bromoisobutyryl bromide, 40 g of triethylamine and 100 g of DMF; stir at room temperature for 12 hours to prepare 2-bromoisobutyryl bromide modified Modified straw (code named RS-Br).
[0044] Wash the RS-Br to remove residual reactants and dry it in an oven. Weigh 5g again and add in the Schlenk reaction flask that solvent DMF (25g) is housed, then add cross-linking agent DVB (1%, 60mg), then add styrene monomer (13mL), acrylonitrile (5mL), catalyst CuBr 2 (25.0mg, 0.11mmol) and the organic ligand PMDETA (29 μl), stirred thoroughly; after deoxygenation by nitrogen gas, 25mg reducing agent stannous isooctanoate was added, and reacted at 60°C for 48h to obtain straw-based hydrogel (RS-g -PSAN).
[0045] Add the above-prepared RS-g-PSAN to a solution containing 20mL D...
Embodiment 2
[0060] Wheat straw (WS) was crushed and cleaned by ultrasonic treatment with ethanol and acetone, and dried in an oven. Dip 20g of dried wheat straw (WS) into a modified solution consisting of 2-bromo-2-methylpropionyl bromide (40g), triethylamine (40g) and DMSO (100g), and stir at room temperature for 12h , and prepared 2-bromo-2-methylpropionyl bromide-modified modified straw (code named WS-Br). Wash the WS-Br to remove residual reactants and dry it in an oven. The dried 5g WS-Br was soaked into the solution containing acrylonitrile monomer (13mL), DMSO (30g), MBA (0.5%, 9mg), CuCl 2 (19mg, 0.11mmol) and bpy (29μl) Schlenk reaction flask, after purging nitrogen to remove oxygen, add 50mg reducing agent stannous isooctanoate, react at 60℃ for 40h, and obtain straw-based hydrogel (WS-g-PAN) .
[0061] Add the above-prepared WS-g-PAN to a container containing 20mL DMAC, 2g catalyst AlCl 3 ·6H 2 In a three-necked flask of O and 30 mL of diethylenetriamine, pass N 2 30min,...
Embodiment 3
[0064]The rice straw (RS) was pulverized, washed, and dried in an oven. 12 g of dried straw were immersed in a solution containing 2-bromo-2-methylpropionyl chloride (48 g), pyridine (36 g) and DMF (100 g). The solution was stirred at room temperature for 12 hours to prepare 2-bromo-2-methylpropionyl chloride modified straw, whose code name was RS-Cl. Wash RS-Cl to remove residual reactants, and dry in an oven. Immerse 2g of RS-Cl into a solution containing methacrylonitrile monomer (5mL), DMF (30g), HAM (1%, 0.4g), CuCl 2 (19.0mg, 0.11mmol) and TMPA (29μl) in a Schlenk reaction flask, after purging nitrogen to remove oxygen, add 30mg reducing agent stannous isooctanoate, react at 60°C for 12h, and obtain RS-g-PMAN modified straw.
[0065] Add the above-prepared RS-g-PMAN to the solution containing 20mL DMSO, 2g catalyst AlCl 3 ·6H 2 In the three-necked flask of O and 30mL triethylenetetramine, pass N 2 After 30 minutes, the reaction was continued in a 90°C water bath fo...
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