Phenols electrochemical sensor based on ionic liquid-graphene oxide sensitive membrane
A technology of ionic liquid and graphene, applied in the field of electroanalytical chemistry, can solve the problems of cumbersome operation, time-consuming, lack of high sensitivity and selectivity, etc., and achieve simple operation process, simple instrument requirements, good conductivity and enrichment effect of ability
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[0037] Example 1
[0038] A new type of ionic liquid 4-hydroxy-1-methyl-1-(3-pyrrolylpropyl)-piperidine bromide salt, and its synthesis method is as follows:
[0039] Weigh 4-hydroxy-N-methylpiperidine (0.4549g, 3mmol) in a 50mL three-necked flask, add 15mL toluene as a solvent, and add 1-(3-bromopropyl)pyrrole (0.5640g, 3.3mmol) dropwise Put it in a three-necked flask, place it in an oil bath at 80°C, and stir for 15 hours under nitrogen protection to form a yellow oily insoluble body. Cool to room temperature, separate the toluene layer, add water to dissolve the yellow oily liquid, and extract with ether. The water layer was evaporated to dryness to obtain a yellow oily liquid, that is, the product of the present invention 4-hydroxy-1-methyl-1-(3-pyrrolpropyl)-piperidine bromide ionic liquid 0.8510g (yield 93.9%), 1 H NMR (D 2 O) δ: 6.76 (d, 2H), 6.11 (d, 2H), 3.98 (t, 2H), 3.89 (d, 1H) 3.38 (t, 2H), 3.20 (d, 2H), 3.12 (d, 2H) ), 2.92 (s, 3H), 2.16 (t, 2H), 1.96 (d, 2H), 1.74 ...
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[0041] Example 2
[0042] A carboxylated graphene oxide-ionic liquid composite nano material, and its preparation method is as follows:
[0043] (1) Combine 10mg graphene oxide (GO), 0.5g sodium hydroxide solid (NaOH) and 0.5g chloroacetic acid (ClCH 2 COOH) was dissolved in 10 mL of water, sonicated uniformly, and stirred on a magnetic stirrer for 2 hours. After centrifugal separation, the solid was washed with water to neutrality, and dried under vacuum at 60°C to obtain 9.5 mg of carboxylated graphene oxide, which was recorded as GO-COOH. Add all the obtained carboxylated graphene oxide to 10mL0.01mol·L -1 In NaOH solution, the reaction was stirred on a magnetic stirrer for 2 hours, centrifuged, the solid was washed with water to neutrality, and dried under vacuum at 60°C to obtain 9.0 mg of carboxylated graphene oxide in an alkalized form, which was recorded as GO-COONa.
[0044] The graphene oxide used has no special requirements;
[0045] Specifically, the graphene oxide in thi...
Example Embodiment
[0050] Example 3
[0051] Such as Figure 4 As shown, a carboxylated graphene oxide-ionic liquid composite nano-material modified electrode includes an insulating layer 1, a glassy carbon substrate 3, an electrode lead 4 electrically connected to the glassy carbon substrate 3, and the surface of the glassy carbon substrate 3 is coated with carboxylation Graphene oxide-ionic liquid nano-composite nano-material film 2. The preparation method of the carboxylated graphene oxide-ionic liquid modified electrode includes the following steps in sequence:
[0052] (1) Pretreatment of glassy carbon electrode: first polish the glassy carbon electrode (3 mm in diameter) with alumina polishing powder with a particle size of 0.3 micron and 0.05 micron, rinse with water, and then use nitric acid solution (65wt% Nitric acid and water equal volume mixed solution), ethanol solution (95wt% ethanol and water equal volume mixed solution) and water are ultrasonically cleaned on the glassy carbon electr...
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