Carboxyl grafting method of polystyrene
A polystyrene and cross-linked polystyrene technology, applied in the field of cation exchange resins, can solve the problems of multiple separation process steps of catalysts and small molecular products, miscibility, and difficulty in reusing catalysts and solvents.
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Embodiment 1
[0033] 2.5 g of uncrosslinked polystyrene, 15 g of anhydrous aluminum trichloride, 50 ml of o-dichlorobenzene, and 2.5 ml of γ-butyrolactone were respectively added to a 100 mL flask. Heat in a water bath, keep the temperature at 45°C, and react for 5 hours under stirring conditions. After the reaction, quickly pour into 10% hydrochloric acid ice water solution under stirring conditions. At this time, the mixed solution becomes strongly acidic, and the obtained solution is grass green. , and then wash the resulting reaction mixture with saturated NaCl solution until the solution is nearly neutral. Anhydrous CaCl 2 After drying, the dried liquid was distilled under reduced pressure to remove the solvent—o-dichlorobenzene, to obtain a viscous liquid, which was dried in an oven at 100° C. to obtain 2 g of a yellow-brown solid. The surface of the solid sample contains carboxyl groups, and the results of infrared spectroscopy (FT-IR) analysis confirm the presence of carboxyl group...
Embodiment 2
[0035] Add 2.5g of cross-linked polystyrene, 30mL of o-dichlorobenzene, 10g of anhydrous aluminum trichloride into a 50mL three-necked bottle, stir, the solution turns yellow, put in a water bath at 20-32°C, drop 2.5mL of γ-butyrolactone , stirred for 4 hours and poured into hydrochloric acid-ice water solution, the cross-linked polystyrene in the system was still solid, suction filtered (washed with a small amount of alcohol solution), washed with deionized water until neutral, collected solid matter, dried to obtain Solid sample 2.3 grams.
Embodiment 3
[0037]Add 10g of cross-linked polystyrene, 120mL of o-dichlorobenzene, and 30g of anhydrous aluminum trichloride into a 250mL three-necked bottle, stir, and the solution turns yellow. In a water bath at 20-32°C, add 10mL of γ-butyrolactone dropwise, continuously Stir, the reaction solution gradually turns reddish-brown, pour it into hydrochloric acid-ice aqueous solution after 4 hours, the cross-linked polystyrene in the system is still solid, suction filter (washing with a small amount of ethanol solution), wash with deionized water until neutral , collected the solid matter and dried to obtain 8.9 grams of solid sample. The surface of the solid sample contains carboxyl groups, and the results of infrared spectroscopy (FT-IR) analysis confirm the presence of carboxyl groups in the sample (1705cm -1 ) is consistent with the carbonyl peak of the control sample 4-phenylbutyric acid; in addition, the content of the carboxyl group on the surface of the sample can be determined by ...
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