Nickel-based crystalline state frame material and preparation and application in methanol oxidation thereof

A crystalline, organic framework technology, applied in the field of metal organic framework materials and their preparation, can solve the problems of slow metal platinum catalysts, easy to be poisoned, etc.

Active Publication Date: 2018-12-28
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the development of methanol fuel cells is limited by the slow reaction kinetics of methanol reaction ...

Method used

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  • Nickel-based crystalline state frame material and preparation and application in methanol oxidation thereof
  • Nickel-based crystalline state frame material and preparation and application in methanol oxidation thereof
  • Nickel-based crystalline state frame material and preparation and application in methanol oxidation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 0.025mmol 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine, 0.025mmol 1,2-bis(4-pyridyl)ethylene, 0.1mmol Ni(ClO 4 ) 2 , 5ml of N,N-dimethylacetamide (DMA), 0.3ml of deionized water, 0.5ml of fluoroboric acid, ultrasonic for 15min and put into a stainless steel reaction kettle lined with polytetrafluoroethylene, and react at a constant temperature of 120°C for 24h, And cooling down to room temperature at a constant rate of 2-3° C. / h to obtain a green hexahedral block crystal and a porous crystalline metal organic framework material with a porosity of 79.5%. Namely Ni.MOF. (The general chemical formula is: {(Ni 3 (μ 3 -O) 3 (TATAB) 2 (dpe) 3 )·3H 2 O·1DMA} n , n is positive infinity, and n only represents the structural characteristics of crystalline materials constructed by the repeated appearance of the smallest unit, which is a general formula).

Embodiment 2

[0027] Weigh 4mg of the porous crystalline MOF sample collected in Example 1 into a 4ml sample tube, add 0.2ml of naphthol, 0.8ml of absolute ethanol and 1ml of deionized water, and apply it on glassy carbon after ultrasonication for 30min on the electrode. Methanol Oxidation (MOR) performance of the test material, after scanning through CV until it is stable, the test is as follows: Figure 6 .

Embodiment 3

[0029] 2 mg of superconducting Ketjen black (KB) was placed in an agate mortar, 8 mg of the porous crystalline metal-organic framework material synthesized in Example 1 was placed therein, ground clockwise for 5 min, the ground sample was placed in a 10 mL beaker and Add 2 mL of ethanol, sonicate in an ultrasonic instrument for 20 min, put it in a vacuum drying oven at 80°C for 10 h, take it out, grind it with agate for 5 min, and collect the sample.

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Abstract

The invention discloses a nickel-based crystalline state frame material and a preparation method and application thereof. The preparation method comprises the specific steps that a macroporous Ni.MOFis newly synthesized through a hydrothermal method, the macroporous Ni.MOF is taken as an anodic catalyst material of methanol oxidation, and the application of the macroporous Ni.MOF in the methanoloxidation is explored. According to the nickel-based crystalline state frame material and the preparation method and application thereof, organic ligand 2,4,6-tris(4-carboxyl phenyl)-1,3,5-triazine, 1,2,-di(4-pyridyl) ethylene and nickelous perchlorate are self-assembled in a mixed solution of N,N-dimethylacetamide, water and fluoboric acid to obtain a porous metal organic framework material, thesynthetic materials are assembled into a three-electrode system for the methanol oxidation test, and through data analysis, the material has excellent methanol oxidation activity.

Description

technical field [0001] The invention relates to a metal-organic framework material formed with trimesic acid derivatives as the main ligand, 1,2-bis(4-pyridyl)ethylene as the auxiliary ligand, and transition metal nickel as the metal center and a preparation method thereof. The prepared catalyst electrode material test shows that it has excellent performance for methanol oxidation (MOR). Background technique [0002] MOFs is the abbreviation of metal organic framework compound (English name Metal orgaic Framework), which is a kind of periodic network structure formed by self-assembly of inorganic metal centers (metal ions or metal clusters) and bridging organic ligands. crystalline porous materials. MOFs is an organic-inorganic hybrid material, also known as a coordination polymer, which is different from both inorganic porous materials and general organic complexes, and has both the rigidity of inorganic materials and the flexibility of organic materials. Moreover, due to...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/16B01J31/22B01J35/00
CPCB01J31/1691B01J31/2243B01J35/0033C08G83/008
Inventor 李东升田军武吴亚盘赵君吴涛张健张其春卜贤辉
Owner CHINA THREE GORGES UNIV
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