Cross-linking agent modified XAD-4 resin and method for preparing same
A technology of XAD-4 and cross-linking agent, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of small adsorption capacity and increased operation complexity, and achieve narrow pore size distribution, improved adsorption capacity, and improved pore size. structure effect
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Embodiment 1
[0031] Add 9.5g of XAD-4 resin to a 250mL three-necked flask equipped with a mechanical stirrer, a reflux condenser and a thermometer, dissolve 7.9g of DCX with 50mL of anhydrous 1,2-dichloroethane and add it to the three-necked flask, and mix the solution Swell in an ice-water bath at 0-5°C for 12 hours. Under medium-speed stirring, 11 mL of anhydrous tin tetrachloride was added to the three-necked flask and kept for 2 hours; the temperature was raised to 60°C for 8 hours, and then the temperature was raised to 80°C for 4 hours. Terminate the reaction with absolute ethanol, pour out the solution, alternately wash 3 times with 1% hydrochloric acid aqueous solution and absolute ethanol, transfer the resin to a Soxhlet extractor, extract the resin with absolute ethanol for 8 hours, and vacuum-dry spare. The specific surface area of the resin is 841.7m 2 / g, pore volume 0.7686cm 3 / g, pore size distribution 1~8.8nm, average pore size 3.65nm.
Embodiment 2
[0033] Dissolve 18.10g of BCMBP in 120mL of 1,2-dichloroethane, add it into a 250mL three-neck flask, then add 15.0g of XAD-4 resin into the three-necked flask, and swell at 0~5°C for 24 hours. Start the mechanical stirring, quickly add 18mL of anhydrous tin tetrachloride to the three-necked bottle, and keep it for 3 hours; then raise the temperature of the mixed solution to 60°C for 10 hours, then raise the temperature to 85°C for 4 hours. The reaction was terminated with acetone, the solution was poured out, and washed three times alternately with 1% aqueous hydrochloric acid and absolute ethanol until the solution was clear. Transfer the resin to a Soxhlet extractor, extract the resin with absolute ethanol for 12 hours, and dry it in vacuum for later use. The specific surface area of the resin is 1228m 2 / g, pore volume 1.068cm 3 / g, pore size distribution 1~8.6nm, average pore size 3.43nm.
Embodiment 3
[0035]Add 10.0g of XAD-4 resin to a 250mL three-necked flask equipped with a mechanical stirrer, reflux condenser and thermometer, dissolve 13.20g of DPB with 60mL of 1,2-dichloroethane and add it to the three-necked flask, and the mixed solution is at 0~ Swell in an ice-water bath at 5°C for 12 hours. Under medium-speed stirring, add 10.8 mL of anhydrous tin tetrachloride to the three-necked flask in an ice-water bath and keep it for 2 hours; raise the temperature to 65°C and keep it for 8 hours, then raise the temperature to 80°C and keep it for 4 hours. Terminate the reaction with absolute ethanol, pour out the solution, alternately wash 3 times with 1% hydrochloric acid aqueous solution and absolute ethanol, transfer the resin to a Soxhlet extractor, extract the resin with absolute ethanol for 8 hours, and vacuum-dry spare. The specific surface area of the resin is 721.1m 2 / g, pore volume 0.6274cm 3 / g, pore size distribution 1~9.0nm, average pore size 3.88nm.
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