Preparation method of polymerization degree-controllable cellulose-based heavy metal ion absorbent
A heavy metal ion, cellulose-based technology, applied in chemical instruments and methods, adsorption water/sewage treatment, water/sludge/sewage treatment, etc., to achieve high solution stability, reduce reagent consumption, and solve the effect of heavy metal residues
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Embodiment 1
[0030] 1. Pass the bagasse cellulose through a 80-mesh sieve, take 1g (0.0062mol) of bagasse cellulose, add 50ml of N,N-dimethylacetamide, and then add 5g (0.1180mol) of anhydrous lithium chloride. After processing in a microwave digestion apparatus at a temperature of 130°C for 20 minutes, stir at room temperature for 3 hours to obtain a fully dissolved transparent solution;
[0031] 2. Transfer the solution in step 1 to an ice bath (10°C), stir and add 3.5g of 2-bromoisobutyryl bromide, and then continue stirring for 60 minutes. When the reaction temperature reaches 70°C, fill with nitrogen and add 1.50ml of three Ethylamine, keep the pH neutral, and react at a constant temperature of 70°C for 10 hours;
[0032] 3. Pour the reaction solution of step 2 into a mixed solution of methanol and deionized water with a volume ratio of 1:1 to wash the precipitate. The temperature of the precipitation reaction solution is 35°C, and then alternately wash with deionized water and methan...
Embodiment 2
[0037] 1. Pass the bagasse cellulose through a 60-mesh sieve, take 1g (0.0062mol) bagasse cellulose, add 40ml N, N-dimethylformamide, then add 4g (0.1180mol) anhydrous lithium chloride, at 400W power, 80 After processing in a microwave digestion apparatus at a temperature of ℃ for 30 minutes, stir at room temperature for 3 hours to obtain a fully dissolved transparent solution;
[0038] 2. Transfer the solution in step 1 to an ice bath (6°C), stir and add 2.5g of 2-bromoisobutyryl bromide, then continue to stir for 40min, when the reaction temperature reaches 50°C, fill with nitrogen and add 1ml of triethyl Amines, keep the pH neutral, and react at a constant temperature of 50°C for 8 hours;
[0039] 3. Pour the reaction solution in step 2 into a mixed solution of methanol and deionized water with a volume ratio of 1:1 to wash the precipitate. The temperature of the precipitation reaction solution is 25°C, and then alternately wash with deionized water and methanol for 5 times...
Embodiment 3
[0044] 1. Pass bagasse cellulose through a 80-mesh sieve, take 1g (0.0062mol) bagasse cellulose, add 45ml N, N-hexamethylphosphoric triamide, then add 4.5g (0.1180mol) anhydrous lithium chloride, in 600W Power and temperature of 100°C in a microwave digestion apparatus for 10 minutes, then stirred at room temperature for 2 hours to obtain a fully dissolved transparent solution;
[0045] 2. Transfer the solution in step 1 to an ice bath (4°C), stir and add 3g of 2-bromoisobutyryl bromide, and then continue stirring for 50 minutes. When the reaction temperature reaches 65°C, fill with nitrogen and add 1.23ml of triethyl Amines, keep the pH at neutral, and react at a constant temperature of 60°C for 9 hours;
[0046] 3. Pour the reaction solution in step 2 into a mixed solution of methanol and deionized water with a volume ratio of 1:1 to wash the precipitate. The temperature of the precipitation reaction solution is 30°C, and then alternately wash it with deionized water and met...
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