Method for rapidly preparing metal-organic framework (MOF) compound having controllable structure by using electrochemical method

A metal-organic framework and electrochemical technology, which is applied in the field of rapid preparation of structure-controllable metal-organic framework compounds by electrochemical methods, can solve the problems of single metal-organic framework morphology and uncontrollable synthesis process, and achieve short synthesis time and smooth synthesis process. The effect of simplicity and broad application prospects

Inactive Publication Date: 2017-09-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the problems that the metal-organic frameworks prepared in the prior art have a single shape and the synthesis process is uncontrollable, a variety of metal-orga...

Method used

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  • Method for rapidly preparing metal-organic framework (MOF) compound having controllable structure by using electrochemical method
  • Method for rapidly preparing metal-organic framework (MOF) compound having controllable structure by using electrochemical method
  • Method for rapidly preparing metal-organic framework (MOF) compound having controllable structure by using electrochemical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Synthesis of ZIF-67 nanomaterials on the surface of FTO:

[0021] a: Ultrasonic the conductive substrate FTO with absolute ethanol, acetone and deionized water respectively for 10 minutes to remove impurities on the surface;

[0022] b: Prepare 1mg / mL cobalt nitrate (Co(NO 3 ) 2 ), 0.5mg / mL1,2-dimethylimidazole, methanol mixed solution 50mL as the electrolyte solution;

[0023] c: In the electrolyte solution prepared in step b, FTO is used as the working electrode, the saturated calomel electrode is used as the reference electrode, and the platinum wire is used as the counter electrode, and ZIF-67 is directly grown on the FTO by the constant potential method, and the electrochemically synthesized potential Set to -0.9V, the synthesis time is 200s, and the synthesis temperature is 25°C.

Embodiment 2

[0025] Synthesis of ZIF-67 nanomaterials on CoAl-LDH@Ni foam:

[0026] a: Ultrasonic the conductive substrate Ni foam with absolute ethanol, acetone and deionized water respectively for 10 minutes to remove impurities on the surface;

[0027] b: Soak the Ni foam obtained in step a in 1 mg / mL cobalt nitrate (Co(NO 3 ) 2 ) and 1mg / mL aluminum nitrate (Al(NO 3 ) 3 ) and 1mg / mL urea in a high-temperature and high-pressure reactor, put the reactor in an oven, and react at 110°C for 24 hours to obtain CoAl-LDH grown on Ni foam, that is, CoAl-LDH@Ni foam.

[0028] c: prepare 1mg / mL cobalt nitrate (Co(NO 3 ) 2 ), 50mL of a mixed solution of 0.5mg / mL1,2-dimethylimidazole and methanol was used as the electrolyte solution;

[0029] d: In the electrolyte solution prepared in step c, CoAl-LDH@Ni foam was used as the working electrode, the saturated calomel electrode was used as the reference electrode, and the platinum wire was used as the counter electrode, and CoAl-LDH@FTO was dire...

Embodiment 3

[0031] Synthesis of ZIF-8 nanomaterials on ZnO@Ni foil:

[0032] a: Ultrasonic the conductive substrate Ni foil with absolute ethanol, acetone and deionized water respectively for 10 minutes to remove impurities on the surface;

[0033] b: Soak the Ni foil obtained in step a in 100 mL of absolute ethanol containing 0.06M zinc acetate, and calcinate at 350°C for 30 minutes. Put the calcined Ni foil into a high-temperature and high-pressure reactor containing 0.06M zinc nitrate and 0.06M hexamethylenetetramine (HMT), react at 100°C for 24 hours, wash it with deionized water and ethanol, Dry at room temperature to obtain ZnO nanorod arrays grown on Ni foil, that is, ZnO@Nifoil.

[0034] c: prepare 1mg / mL zinc nitrate (Zn(NO 3 ) 2 ), 0.5mg / mL1,2-dimethylimidazole, methanol mixed solution 50mL as the electrolyte solution;

[0035] d: In the electrolyte solution prepared in step c, ZnO@Ni foil was used as the working electrode, the saturated calomel electrode was used as the ref...

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Abstract

The invention relates to a method for rapidly preparing a metal-organic framework (MOF) compound having a controllable structure by using an electrochemical method. After the method is adopted, an MOF material can be electrically synthesized on a variety of macroscopic and microcosmic conductive substrates by means of a simple and rapid one-step electrical synthesis method. Furthermore, the directional growth of multiple MOFs materials can be realized on different types of macroscopic and microcosmic conductive substrates by regulating and controlling the types, concentrations, proportions, electrical synthesis voltages, time and the like of organic ligands and metal ions in an electrolyte solution; the particle sizes and morphologies of the MOFs materials can be artificially regulated and controlled. The electrochemical synthesis method has the advantages of short synthesis time and simple operation process, synthesis can be completed under the condition of room temperature, and a condition for subsequent extensive preparation and industrial application is provided. In addition, the prepared novel MOFs thin-film material has a very wide application prospect in the aspects of electrolytic water oxygen evolution reaction (OER), supercapacitor electrode materials (SCs), lithium ion battery electrode materials, biosensing and the like.

Description

technical field [0001] The invention belongs to the field of synthesis of metal organic framework materials, and in particular relates to a method for rapidly preparing structure-controllable metal organic framework compounds by an electrochemical method. Background technique [0002] Metal-organic frameworks (MOFs), also known as metal-organic coordination polymers (MOCP), are an inorganic-organic complex assembled by metal ions and organic ligands through coordination. Hybrid functional materials. Metal ions and multidentate organic ligands containing nitrogen and oxygen (mostly aromatic polyalkali or polyacids) self-assemble into materials with special pore structures, in which metal ions serve as nodes of the skeleton structure, and organic ligands become links between these The bridging group of the node. This metal-organic framework material can be complexed with various metal ions through different organic ligands, so as to design and control the pore structure in t...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 邵明飞杨绮慧栗振华卫敏
Owner BEIJING UNIV OF CHEM TECH
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