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Nitrogen-doped porous cobalt-carbon material and preparation method and application thereof

A technology of nitrogen doping and carbon materials, which is applied in the preparation of hydrocarbon ammoxidation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of unfavorable catalyst recycling, potential safety hazards, harsh reaction conditions, etc., and achieve effective Good for environmental protection, wide application range, and mild reaction conditions

Inactive Publication Date: 2019-10-08
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, there are some disadvantages in the above methods. For example, homogeneous catalysis is not conducive to the recycling of catalysts; strong oxidants, alkalis and ligands are often added in the reaction, and the reaction conditions are harsh; when using heterogeneous catalysis, high temperature and high pressure oxygen are required. If it is carried out under certain conditions, it will cause side reactions and have potential safety hazards
In addition, the use of organic solvents will pollute the environment, which is not conducive to environmental protection.

Method used

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  • Nitrogen-doped porous cobalt-carbon material and preparation method and application thereof
  • Nitrogen-doped porous cobalt-carbon material and preparation method and application thereof
  • Nitrogen-doped porous cobalt-carbon material and preparation method and application thereof

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Embodiment 1

[0024] Example 1: Preparation of catalyst Co@NC

[0025] Add 2-methylimidazole (3.24g) and Co(NO 3 ) 2 ·6H 2 O (1.43g), stirred at room temperature for 24h, washed with methanol after the reaction and dried by centrifugation to obtain ZIF-67. Add ZIF-67 (400mg), Zn(NO 3 ) 2 ·6H 2 O (5.95g) and 2-methylimidazole (6.16g) were stirred at 35°C for 24h, washed with methanol and dried by centrifugation to obtain ZIF-67@ZIF-8. The obtained ZIF-67@ZIF-8 was calcined in a tube furnace at a heating rate of 5 °C / min at 900 °C for 3 h to obtain a nitrogen-doped porous cobalt-based nanocatalyst with a cobalt content of 3.4 wt.%. Its SEM and TEM images are as follows figure 1 and figure 2 shown.

[0026] Ammoxidation of Primary Alcohols

[0027]

[0028] Add 0.2mmol of primary alcohol compound, 14mg of Co@NC, and 1mL of water into the reaction vessel, and react at 50°C for 12h under normal pressure oxygen condition. After the reaction is completed and the temperature is lower...

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Abstract

The invention discloses a nitrogen-doped porous cobalt-based nano material and a preparation method and application thereof. The material is prepared by taking a ZIF-67@ZIF-8 composite material as a precursor through high-temperature calcination. The material is used as a catalyst, water is used as a solvent, atmospheric pressure oxygen is used as an oxidizing agent, ammonia water is used as a nitrogen source, and conversion from primary alcohol to nitrile compounds can be realized in a one-step method at the temperature of 50 DEG C. According to the invention, the nitrogen-doped porous cobalt-based nano material with large specific surface area and pore volume and good alkalinity and hydrophilicity is adopted as a catalyst, and the catalyst is simple to prepare and is efficient; reactionconditions are mild, and high-temperature and high-pressure conditions are not needed; alkali and strong oxidant do not need to be sued in reaction; water as a reaction solvent is also the unique by-product of the reaction; the substrate has a wide application range and can be applied to aromatic ring, fused ring and heterocyclic primary alcohol compounds; and the reaction can be carried out at high concentration, and the catalyst can be recycled after the reaction is finished, so that the industrial application is facilitated.

Description

technical field [0001] The invention belongs to the field of nanoporous material preparation, and in particular relates to a nitrogen-doped porous cobalt carbon material and a preparation method and application thereof. Background technique [0002] Nitrile compounds are multifunctional intermediates commonly used in organic synthesis, and they are important structural units of pesticides, dyes, drugs and various fine chemicals. Derivatives of nitrile compounds can also be used to construct amides, carboxylic acids and nitrogen-containing heterocyclic compounds. Therefore, the synthesis of nitrile compounds has received extensive attention from industry and academia. [0003] And the common method of synthesizing nitriles by alcohols mainly includes the following: (1) primary alcohol ammoxidation (Catal.Commun., 2019,19,51-56; J.Iran.Chem.Soc.2015,12,107-111; RSC.Adv.2014,4,54007-54017.); (2) Heterogeneous Phase-catalyzed ammoxidation of primary alcohols (Chem.Commun.2017...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C253/28C07C255/50C07C255/54C07C255/52C07C255/34C07D213/85
CPCB01J27/24C07C253/28C07D213/85C07C255/50C07C255/54C07C255/52C07C255/34Y02P20/584
Inventor 陆国平孙嘉霖孙康康
Owner NANJING UNIV OF SCI & TECH
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