Preparation method of thermosensitive ion imprinting gel
An ion imprinting, temperature-sensitive technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc. Effect of Sensitive Temperature Response Characteristics
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[0016] A method for preparing a temperature-sensitive ion imprinted gel, the process comprising the following steps:
[0017] (1) Ligand synthesis
[0018] Take 5-30mmol of chloromethylstyrene and 20-50mmol of amine compounds, add them to 50-200mL of solvent and stir for 5-12h, after the reaction, evaporate the solvent to obtain ligand solid, and then wash , recrystallization, filtration, and drying to finally obtain a white powder of pure ligand;
[0019] (2) Synthesis of complexes
[0020] Dissolve the ligand obtained above in 200mL of methanol to make a ligand solution; take 2 to 5 mmol of the molecular formula as M(ClO 4 ) n ?6H 2 The metal perchlorate salt of O is dissolved in 100-200 mL of acetonitrile to make a metal perchlorate solution, where M is a metal ion; the ligand solution and the metal perchlorate solution are mixed to obtain a concentrated solution of the complex, Add ether 5 to 20 times its volume to the concentrated solution of the complex, mix to prod...
Embodiment 1
[0027] Take 10mmol of chloromethylstyrene and 40mmol of ethylenediamine and dissolve them in 200mL of dichloromethane respectively, add the chloromethylstyrene solution into the ethylenediamine solution dropwise within 30min under stirring, react for 5h, and use rotary evaporation The dichloromethane was evaporated to obtain a ligand solid, and then the ligand solid was dissolved in 200ml of CH 3 OH, then add 5 times the amount of ether of the solution volume to form a white precipitate, which is separated by filtration and dried under reduced pressure to obtain a pure white powder of the ligand. The reaction that occurs in this step is:
[0028] ;
[0029] Dissolve the ligand obtained above in 200mL methanol, take 2mmol Cu(ClO 4 ) 2 ?6H 2O was dissolved in 200mL of acetonitrile, and the two solutions were mixed to obtain a concentrated solution of the complex, and then 5 times the volume of the mixed solution was added to the ether to obtain the precipitate of the comple...
Embodiment 2
[0033] Take 5mmol of chloromethylstyrene and 20mmol of diethylenetriamine and dissolve them in 50mL of dichloromethane respectively, add the chloromethylstyrene solution dropwise to the diethylenetriamine solution within 30min under stirring, react for 8h, and use Rotary evaporator evaporates dichloromethane to obtain ligand solid, then the ligand solid is dissolved in 200ml of CH 3 OH, then add 5 times the volume of the solution of ether to form a white precipitate, which is separated by filtration and dried under reduced pressure to obtain a white powder of pure ligand;
[0034] Dissolve the ligand obtained above in 200mL methanol, take 3mmol Cu(ClO 4 ) 2 ?6H 2 O was dissolved in 100mL of acetonitrile, and the two solutions were mixed to obtain a concentrated solution of the complex, and then 5 times the volume of the mixed solution was added to the ether to obtain the precipitate of the complex, which was filtered and vacuum-dried at 50°C for 1 hour to obtain the complex ...
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