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Method for regulating valence state of metal in carbonized metal-organic framework material through alkaline N

A metal-organic framework and metal carbide technology, which is applied in the field of material chemistry and catalytic reaction, can solve the problems of being expensive, not being widely used in large quantities, and the price of precious metal catalysts being easy to agglomerate, so as to achieve good modification, good reaction rate and catalytic activity. The effect of improving activity and efficiency

Active Publication Date: 2018-04-06
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims at the problem that the existing noble metal catalysts are easy to agglomerate and expensive and cannot be widely used in large quantities, and provides a method for basic N to regulate the valence state of metal oxides in carbonized metal-organic framework materials. The present invention adopts The basic nitrogen source with a basicity coefficient (pKb) in the range of 3 to 9, and then use the high-energy cavitation generated by ultrasound to bond basic nitrogen and copper elements, thereby regulating the valence state of the metal in the metal oxide formed after carbonization , ultimately improving the activity and service life of the resulting catalyst

Method used

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  • Method for regulating valence state of metal in carbonized metal-organic framework material through alkaline N
  • Method for regulating valence state of metal in carbonized metal-organic framework material through alkaline N
  • Method for regulating valence state of metal in carbonized metal-organic framework material through alkaline N

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Embodiment 1

[0042] A method for regulating the valence state of a metal in a metal organic framework material by basic N, comprising the following steps,

[0043] (1) Preparation of metal-organic framework material MOF: Dissolve 0.5448g of anhydrous copper acetate in 24ml of water, and then dissolve 0.6300g of trimesic acid (the mass ratio of copper acetate and trimesic acid is 1:1.16) solution one by one Add dropwise into the anhydrous copper acetate solution, stir at 1000rpm until the mutual solubility is uniform, and the metal organic framework material MOF can be obtained; then the MOF is soaked in the ethanol solution, filtered and placed in a vacuum oven at 100°C for vacuum drying. Degree <100Pa;

[0044] (2) Carbonization of MOF: 0.3g of MOF was placed in a tube furnace under N 2 Carbonization in the atmosphere, the specific parameters of carbonization: N 2 The flow rate is 80mL / min, the heating rate is 10°C / min, the carbonization temperature is 600°C, and the carbonization time ...

Embodiment 2

[0046] A method for regulating the valence state of a metal in a metal organic framework material by basic N, comprising the following steps,

[0047] (1) Preparation of basic N-modified metal-organic framework N-MOF-1: Add 0.05874g (5wt.%) dopamine (alkalinity coefficient pKb is around 3) to 24mL, 0.5448g of anhydrous copper acetate aqueous solution In the process, stir at 1000 rpm for 0.5h, then irradiate and react under a 500W ultrasonic field for 0.5h; then add 0.6300g of trimesic acid (the mass ratio of copper acetate and trimesic acid is 1:1.16) solution one by one Add it dropwise, and continue to stir until it dissolves evenly to obtain a basic nitrogen-modified metal-organic framework material N-MOF-1; soak N-MOF-1 in ethanol solution, filter and place it in a vacuum oven at 120°C Carry out vacuum drying, vacuum degree <100Pa;

[0048] (2) Carbonization of N-MOF-1: 0.3g of N-MOF-1 was placed in a tube furnace, 2 Carbonization in the atmosphere, the specific parameter...

Embodiment 3

[0050] A method for regulating the valence state of a metal in a metal organic framework material by basic N, comprising the following steps,

[0051] (1) Preparation of basic N-modified metal-organic framework N-MOF-2: 0.3695g (10wt.%) melamine (alkalinity coefficient pKb around 9) was added to 24mL of 0.5448g anhydrous copper acetate aqueous solution , stirred at 1000 rpm for 1 h, then irradiated and reacted for 1 h under a 1000 W ultrasonic field; then 3.1500 g of trimesic acid (the mass ratio of copper acetate and trimesic acid is 1:5.78) solution was added dropwise , continue to stir until the mutual dissolution is uniform, and obtain the nitrogen-modified metal-organic framework material N-MOF-2 material; soak the N-MOF-2 in an ethanol solution, filter it, and place it in a vacuum drying oven at 120°C for vacuum drying. Vacuum <100Pa;

[0052] (2) Carbonization of N-MOF-2: put 0.3g of N-MOF-2 in a tube furnace, 2 Carbonization in the atmosphere, the specific parameters...

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Abstract

The invention discloses a method for regulating the valence state of metal in a carbonized metal-organic framework material through alkaline N. Firstly, 5wt.%-10wt.% of an alkaline N source are addedto a copper acetate solution, an N group and Cu in the solution are coordinated by use of ultrasonic field radiation at the frequency of 500-1,000 W, a trimesic acid solution is dropwise added to thesolution, the reaction is sustained for 1-3 h, and an N-modified N-MOF precursor material is obtained; the N-MOF precursor material is put in a high-temperature tube furnace, heated to 600-800 DEG C in the N atmosphere and kept for 4-6 h, and a CN-MOF catalyst with Cu / CuOx / C(x<1) is obtained. The alkalinity coefficient (pKb) of the alkaline N source is in the range of 3-9, alkaline N and copper elements are bonded under the high-energy cavitation action produced by ultrasonic, so that the valence state of metal in a metal oxide produced after carbonization is regulated, and finally, the activity of the obtained catalyst is improved and the service life of the catalyst is prolonged.

Description

technical field [0001] The invention belongs to the field of material chemistry and catalytic reaction, and in particular relates to heteroatom modification of porous metal organic framework materials, a catalyst and a preparation method thereof. Background technique [0002] In recent years, with the continuous development of our country, the pollution of nitro compounds to the environment has become increasingly serious, which has aroused widespread concern in the society. Among them, p-nitrophenol (4-NP) and nitroaromatic compounds are highly toxic and difficult to degrade in nature, so the treatment of wastewater containing nitroaromatic compounds is a worldwide technical problem. The reduction product of p-nitrophenol, p-aminophenol, has low toxicity and is easy to degrade, and it is also a synthetic intermediate of analgesic and antipyretic. The transformation of p-nitrophenol into p-aminophenol not only realizes the degradation of p-nitrophenol, but also effectively ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J23/72B01J27/24B01J37/34B01J37/06B01J37/08B01J35/10
CPCB01J23/72B01J27/24B01J31/1691B01J31/2213B01J37/06B01J37/082B01J37/086B01J37/343B01J35/613B01J35/615
Inventor 赵祯霞孙晓丹胡鹏周凯彬赵钟兴
Owner GUANGXI UNIV
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