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Hydrotalcite-like nanosheet@ZIF-67 composite material modified electrode as well as preparation method and detection application thereof

A technology of composite materials and modified electrodes, applied in the direction of material electrochemical variables, etc., can solve the problems of limiting the depth development of LDH, achieve the effect of simple preparation method and avoid cumbersome steps

Active Publication Date: 2018-12-28
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the LDHNS in the exfoliated state is easy to aggregate and return to the bulk state of LDH in the aqueous medium, and can only be used in the form of colloidal solution, which greatly limits the in-depth development of LDH in the field of electrochemistry.

Method used

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  • Hydrotalcite-like nanosheet@ZIF-67 composite material modified electrode as well as preparation method and detection application thereof
  • Hydrotalcite-like nanosheet@ZIF-67 composite material modified electrode as well as preparation method and detection application thereof
  • Hydrotalcite-like nanosheet@ZIF-67 composite material modified electrode as well as preparation method and detection application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (a) Preparation of CoAl-LDHNS

[0029] The divalent metal salt Co(NO 3 ) 2 ·6H 2 O and trivalent metal salt Al(NO 3 ) 3 ·9H 2 O is dissolved in a certain volume of formamide in a certain molar ratio, the total metal ion concentration is 0.03mol / L, and then titrated with an appropriate amount of 0.1mol / L NaOH solution, the pH of the solution is adjusted to 8.5, and the obtained CoAl-LDHNS CoAl-LDHNS is obtained after centrifugal washing of the colloidal solution for use;

[0030] (b) Preparation of CoAl-LDHNS@ZIF-67

[0031] Weigh 1.83g of CoAl-LDHNS obtained in step (a), place it in a beaker containing a certain volume of formamide, ultrasonicate for 4h to obtain dispersion A, then weigh 0.75g of dimethylimidazole and dissolve it in the same volume of formamide The solution B is obtained from the solution. Under stirring, the solution B is dropped into the above dispersion A at a constant speed. The reaction solution is reacted in a water bath at 50℃ for 24h, then aged at roo...

Embodiment 2

[0033] (a) Preparation of CoAl-LDHNS

[0034] Prepare according to the method and conditions of step (a) in Example 1;

[0035] (b) Preparation of CoAl-LDHNS@ZIF-67

[0036] Prepare according to the method and conditions of step (b) in Example 1;

[0037] (c) Preparation of CoAl-LDHNS@ZIF-67 composite material modified GCE

[0038] Polish the base electrode into a mirror surface, then ultrasonically clean it with ultrapure water, and dry it at room temperature to obtain a processed GCE; ultrasonically disperse the CoAl-LDHNS@ZIF-67 composite material prepared in step (b) in deionized water, Prepare a dispersion with a concentration of 1mg / mL, take 5μL of the dispersion and apply dropwise to the surface of the GCE treated in step (c), and dry it naturally at room temperature to obtain CoAl-LDHNS@ZIF-67 composite film modified GCE, which is marked as CoAl- LDHNS@ZIF-67 / GCE;

Embodiment 3

[0040] (a) Preparation of CoAl-LDHNS

[0041] Prepare according to the method and conditions of step (a) in Example 1;

[0042] (b) Preparation of CoAl-LDHNS@ZIF-67

[0043] Prepare according to the method and conditions of step (b) in Example 1;

[0044] (c) Preparation of CoAl-LDHNS@ZIF-67 / GCE

[0045] Polish the base electrode into a mirror surface, then ultrasonically clean it with ultrapure water, and dry it at room temperature to obtain a processed GCE; ultrasonically disperse the CoAl-LDHNS@ZIF-67 composite material prepared in step (b) in deionized water, Prepare a dispersion with a concentration of 1 mg / mL, take 8 μL of the dispersion and apply dropwise to the surface of the GCE treated in step (c), and dry it naturally at room temperature to obtain CoAl-LDHNS@ZIF-67 / GCE;

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Abstract

The invention discloses a hydrotalcite-like nanosheet@ZIF-67 composite material modified electrode, a preparation method thereof and application thereof to simultaneous detection of naphthol isomer. The preparation method comprises the following steps: growing ZIF-67 in situ on a hydrotalcite-like nanosheet stripped from formamide to prepare a cobalt-aluminum hydrotalcite nanosheet@ZIF-67 compound; and preparing a corresponding modified glassy carbon electrode from the compound. The obtained modified electrode plays a synergistic role between the hydrotalcite-like nanosheet and the ZIF-67, andrealizes high-sensitivity simultaneous detection of the naphthol isomer, wherein the linear range of alpha-naphthol detection is 3x10<->7 to 1.5x10<-4>mol / L, and the detection limit is 62nmol / L; andthe linear range of beta-naphthol detection is 3x10<->7 to 1.5x10<-4>mol / L, and the detection limit is 94 nmol / L. The modified electrode has the advantages of simple preparation method, easy control of conditions, wide linear range of detection, low detection limit, and high stability and high sensitivity of the detection method.

Description

Technical field: [0001] The invention relates to a ZIF-67 modified electrode grown in situ on Co-Al ELDH; the invention also relates to a preparation method of the modified electrode and its application in electrochemical sensing and detection. Background technique: [0002] Naphthol is an important organic chemical raw material and dye intermediate in chemical production in today's society. It is widely used in organic dyes, organic pigments, pesticides and medicine. Naphthol has two isomers, namely α-naphthol and β-naphthol. Because the two often coexist in the environmental system and have high toxicity at low concentrations, it is particularly important to establish a stable and sensitive detection method. At present, the methods for detecting such substances mainly include high performance liquid chromatography, gas chromatography, spectrophotometry, fluorescence, electrochemiluminescence, etc. However, these methods have disadvantages such as complicated operating conditio...

Claims

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Application Information

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IPC IPC(8): G01N27/30G01N27/48
CPCG01N27/30G01N27/48
Inventor 詹天荣李智康敬霞
Owner QINGDAO UNIV OF SCI & TECH
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