Amino metal organic framework material containing active metal component as well as preparation method and application of amino metal organic framework material

An active metal, metal amide technology, applied in the preparation of amino compounds, the preparation of organic compounds, the preparation of amino hydroxy compounds, etc., can solve the problems of high catalyst cost, complex preparation process, low metal dispersion, etc. Highly dispersed, simple and controllable preparation method

Active Publication Date: 2015-04-22
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these catalysts have good catalytic performance, they have disadvantages such as low metal dispersion, high catalyst cost, and complicated preparation process.

Method used

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  • Amino metal organic framework material containing active metal component as well as preparation method and application of amino metal organic framework material
  • Amino metal organic framework material containing active metal component as well as preparation method and application of amino metal organic framework material
  • Amino metal organic framework material containing active metal component as well as preparation method and application of amino metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In this implementation, the active metal component is Pd, and the amino metal organic framework material is NH 2 -UiO-66, the amino metal organic framework material containing the active metal component is denoted as Pd / NH 2 -UiO-66, where Pd mass accounts for NH 2 - 0.2 to 10 wt% of the mass of UiO-66.

[0030] The Pd / NH 2 - The preparation method of UiO-66 material is as follows:

[0031] (1) Prepare 0.2~10wt% Pd / NH 2 -UiO-66:

[0032] NH 2 - The preparation method of UiO-66 is as described in the literature: Nanoscale, 2013, 5, 9374-9382.

[0033] The NH 2 -UiO-66 has good thermal stability and water stability, and the specific surface has reached 950m 2 g -1 above. the NH 2 -UiO-66 powder is vacuum-dried in a vacuum oven at 150°C for more than 12 hours.

[0034] (2) Weigh 2-110 mg of palladium acetate, disperse in 45 ml of acetone, and ultrasonicate for 5 minutes until uniformly dispersed to obtain the first solution. At the same time, 0.5 g of activate...

Embodiment 2

[0041] In this example, the active metal component is Pd, and the amino metal organic framework material is NH 2- MIL-53, the amino metal organic framework material containing the active metal component is denoted as Pd / NH 2 -MIL-53 with Pd mass accounting for NH 2 - 0.2 to 10 wt% of the mass of MIL-53.

[0042] The Pd / NH 2 - The preparation method of MIL-53 material is as follows:

[0043] (1) Preparation of Pd / NH 2 -MIL-53:

[0044] NH 2 - The preparation method of MIL-53 powder is as described in the literature: Inorganic Chemistry, 2009, 48, 3057-3064.

[0045] The NH 2 -MIL-53 has a high specific surface area and pore size, and has good thermal stability and water stability. the NH 2 - MIL-53 powder is vacuum-dried in a vacuum oven at 150°C for more than 12 hours.

[0046] (2) Accurately weigh 3 to 150 mg of palladium acetylacetonate, disperse it in 50 ml of acetone, and sonicate until it is evenly dispersed to obtain the first solution; at the same time, 0.5 g ...

Embodiment 3

[0051] In this implementation, the active metal component is Pd, and the amino metal organic framework material is NH 2 -MIL-101, the amino metal organic framework material containing the active metal component is denoted as Pd / NH 2 -MIL-101 where Pd mass accounts for NH 2 - 0.2 to 10 wt% of the mass of MIL-101.

[0052] The Pd / NH 2 - The preparation method of MIL-101 material is as follows:

[0053] (1) Preparation of NH 2 -MIL-101 powder

[0054] NH 2 - The preparation method of MIL-101 powder is as described in the literature: RSC Advances, 2012, 2, 6417-6419.

[0055] The NH 2 -MIL-101 powder has good thermal stability and water stability, and the specific surface area reaches 2500m 2 g -1 above. the NH 2 - MIL-101 powder is vacuum dried at 150°C to remove NH 2 - Moisture in the pores of MIL-101.

[0056] (2) Weigh 3 to 150 mg of palladium acetylacetonate, disperse it in 50 ml of acetone, and sonicate until it is uniformly dispersed to obtain the first solutio...

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PUM

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Abstract

The invention provides an amino metal organic framework material containing an active metal component. The amino metal organic framework material is used as a carrier; and the active metal component is dispersed in the carrier, wherein the weight of the active metal component is 0.05-15% of that of the amino MOFs material. According to the invention, a mixed solution is formed from the carrier and an active metal precursor containing a carbanyl group; amino in the MOFs material is reacted with the carbanyl group in the active metal precursor, so that the active metal precursor is connected to the MOFs material; then, the material is prepared through a reduction method; uniform dispersion of the active metal component in the MOFs material is realized; when the material is used as the catalyst, the catalytic effect is obvious because of high dispersion of the active component, for example, the amino metal organic framework material is used in a process for preparing aromatic amine by hydrogenation reduction of an aromatic nitro compound, etc.

Description

technical field [0001] The invention relates to a material composed of a carrier and an active metal component, in particular to an amino metal organic framework material containing an active metal component, its preparation method and application. Background technique [0002] Aromatic nitro compounds are common pollutants in industrial wastewater. Aromatic amine is an important chemical intermediate, which is widely used in pharmaceutical, plastic, printing and dyeing, cosmetics production and other industries. Therefore, people try to use aromatic nitro compounds to prepare aromatic amines. At present, there are mainly iron powder reduction method, electrolytic reduction method and catalytic hydrogenation method. Among them, the catalytic hydrogenation process reduces production and has little pollution, so it is favored by people. [0003] The key to the process of catalytic hydrogenation reduction of aromatic nitro compounds to prepare aromatic amines is the hydrogena...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C215/76C07C213/02C07C211/46C07C209/36C02F1/70
Inventor 陈亮陶凯孔春龙
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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