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A method for basic n regulation of metal valence in carbide metal organic frameworks

A technology of metal-organic framework and metal carbide, which is applied in the field of material chemistry and catalytic reaction, can solve the problems of precious metal catalysts, such as easy agglomeration, price, inability to be widely used in large quantities, and high cost, to achieve good reaction rate and catalytic activity, and improve activity and efficiency , good modification effect

Active Publication Date: 2020-03-24
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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  • A method for basic n regulation of metal valence in carbide metal organic frameworks
  • A method for basic n regulation of metal valence in carbide metal organic frameworks
  • A method for basic n regulation of metal valence in carbide metal organic frameworks

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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 metals in carbonized metal-organic framework materials with basic N. First add 5~10wt.% alkaline nitrogen source into the copper acetate solution, use 500~1000W frequency ultrasonic field radiation to coordinate the N group with Cu in the solution, and then add the trimesic acid solution dropwise to continue the reaction. 1 to 3 hours to obtain the nitrogen-modified N‑MOF precursor material; then place the N‑MOF in a high-temperature tube furnace, heat it to 600 to 800°C in a nitrogen atmosphere and keep it for 4 to 6 hours to obtain Cu / CuO x / C(x<1) component is the main CN‑MOF catalyst. The basic nitrogen source used in the present invention has a basicity coefficient (pKb) in the range of 3 to 9. The high-energy cavitation generated by ultrasound is used to bond the basic nitrogen and copper elements, thereby regulating the metal in the metal oxide generated after carbonization. valence state, ultimately improving the activity and service life of the resulting catalyst.

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 Patents(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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