Hypercrosslinked porous polycarbazole for fast and efficient removal of organic micropollutants from water
Description
This dataset contains the experimental and characterization data supporting the research article on the removal of organic micropollutants from water using hypercrosslinked porous polycarbazole. The dataset have characterization of adsorbents such as FT-IR spectrum, solid 13C NMR spectra, nitrogen adsorption desorption isotherms,organic micropollutants adsorption performance data, effects of experimental parameters, adsorption kinetics, adsorption isotherms, and regeneration/reusability results of the adsorbent. These data support the results, discussion, reproducibility, and conclusions presented in the associated manuscript.
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Synthesis of 1,3,5-tris(carbazole)benzenemethanone) (TCZP) The synthesis is based on reported literature.1 Carbazole (3.00 g, 17.97 mmol) and NaH (1.29 g, 53.91 mmol) were added to a two-neck flask, and then dry tetrahydrofuran (THF) (240 mL) was injected at 0 °C. The mixture was stirred at room temperature for 45 min. The resulting mixture was added to 1,3,5-benzenetricarbonyltrichloride (1.6 g, 6 mmol) in dry THF (150 mL) at 0 °C. After being stirred at 0 °C for 10 min and further stirred for 2 hrs at room temperature, the reaction was quenched with water. After the solvent was removed by rotary evaporation, the residue was purified by flash column chromatography (silica gel, petroleumether/CH2Cl2 = 4:1, 3:1, and 1:1) to give BTCZM as a white solid. After flash column chromatographic purification and then vacuum drying at 50 °C for 12 h, a white solid of 3.21 g with 81% yield was obtained. The FT-IR shows a strong absorption peak at about 1687 cm–1, which is attributed to the amide carbonyl functional group. Synthesis of tricarbazolephenone–hypercrosslinked polymer The synthesis of tricarbazolephenone–hypercrosslinked polymer (TCZP-HCP) is based on reported literature.2 Under a nitrogen atmosphere, benzene-1,3,5-triyltris((9H-carbazol-9-yl)methanone) (0.23 mmol, 0.15 g) was dispersed in CH2Cl2 (20 mL) for 30 min, and then anhydrous FeCl3 (9.6 mmol, 1.2816 g) was added to the solution; the stirred mixture is evacuated for two cycles with nitrogen refilling; the mixture was allowed to react at 20 °C, 30 °C, 40 °C, and 60 °C for 4 , 8 , 24 hours, respectively under vigorously stirring. After cooling to room temperature, the solid product was quenched by using 20 mL of HCl−H2O (v/v = 2:1), washed several times with deionized water and methanol, further purified by Soxhlet extractor with each methanol and THF 24 h. After purification is over the solid was freeze dried to give a dark yellow powder with 66% yield.
Institutions
- University of South AfricaGauteng, Pretoria