Amino functionalized ionic liquid/hydrotalcite-like compound composite material, and preparation method and application thereof
An amino-functionalized, ionic liquid technology, used in chemical instruments and methods, adsorption water/sewage treatment, water/sludge/sewage treatment, etc.
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Embodiment 1
[0033] (a) Preparation of amino-functionalized ionic liquid 1-methyl-3-aminoethylimidazolium tetrafluoroborate
[0034] Under ice-bath conditions, pipette 20 mL of N-methylimidazole (10.3 g, 0.25 mol) into a round-bottomed flask, and add equimolar 2-bromoethylamine hydrobromide (51.22 g, 0.25 mol) under constant stirring It was slowly added dropwise into absolute ethanol (20 mL) equal to the volume of N-methylimidazole, and the reaction solution was stirred at 50° C. for 24 hours, and protected by nitrogen gas during the reaction. After the reaction, remove the solvent and unreacted volatile substances by rotary evaporation, dissolve the product with a small amount of water, then add 250 mL of 1 mol / L potassium hydroxide solution to reduce the protected amino group, and remove most of the water in the resulting solution by distillation under reduced pressure Then vacuum-dry at 60°C to constant weight, dissolve the product with ethanol-tetrahydrofuran mixed solvent with a volum...
Embodiment 2
[0038] (a) Preparation of amino-functionalized ionic liquid 1-methyl-3-aminoethylimidazolium tetrafluoroborate
[0039] Adopt the method and the condition synthesis of step (a) among the embodiment 1;
[0040] (b) Preparation of amino-functionalized ionic liquid / hydrotalcite-like composites
[0041] Divalent metal salt Zn(NO 3 ) 2 and trivalent metal salt Al(NO 3 ) 3 Prepare a mixed salt solution at a molar ratio of 2:1, the total metal ion concentration is 0.6 mol / L, and then the ionic liquid is 1-methyl-3-aminoethylimidazolium tetrafluoroborate and divalent metal salt Zn(NO 3 ) 2 Add the molar ratio of 0.5:2 into the mixed salt solution, titrate the above mixed solution and the sodium hydroxide solution with a molar concentration of 2 mol / L at the same time, control the pH between 9.0 and 10.0, stir vigorously, and age at 80 °C for 8 Hour. The obtained slurry was suction-filtered, the filter cake was washed 4 times with distilled water, and dried at 60° C. for 24 hou...
Embodiment 3
[0043] (a) Preparation of amino-functionalized ionic liquid 1-methyl-3-aminoethylimidazolium tetrafluoroborate
[0044] Adopt the method and the condition synthesis of step (a) among the embodiment 1;
[0045] (b) Preparation of amino-functionalized ionic liquid / hydrotalcite-like composites
[0046] Divalent metal salt Zn(NO 3 ) 2 and trivalent metal salt Al(NO 3 ) 3 Prepare a mixed salt solution at a molar ratio of 2:1, the total metal ion concentration is 0.6 mol / L, and then the ionic liquid is 1-methyl-3-aminoethylimidazolium tetrafluoroborate and divalent metal salt Zn(NO 3 ) 2 The molar ratio of 0.8:2 was added to the mixed salt solution, and the above mixed solution and the ammonia solution with a molar concentration of 4 mol / L were titrated simultaneously to control the pH between 9.0 and 10.0, vigorously stirred, and aged at 50°C for 18 hours. The obtained slurry was suction-filtered, the filter cake was washed 4 times with distilled water, and dried at 60° C. f...
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