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Carbon material coated nickel catalyst and method for preparing primary amine compound by using same

A technology of nickel catalyst and carbon material, which is applied in the field of carbon material wrapping nickel catalyst and preparing primary amine compounds by using the same, can solve the problems of unobtained performance materials and the like, and achieve the effects of high reaction selectivity, low cost and simple preparation method.

Inactive Publication Date: 2020-01-31
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, materials with satisfactory performance have not yet been obtained

Method used

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  • Carbon material coated nickel catalyst and method for preparing primary amine compound by using same
  • Carbon material coated nickel catalyst and method for preparing primary amine compound by using same
  • Carbon material coated nickel catalyst and method for preparing primary amine compound by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A nitrogen-doped carbon material comprising a cobalt catalyst prepared by:

[0035] 1) Using medical absorbent cotton as raw material, soak 0.5g of medical absorbent cotton in 0.1mol / LNi(NO 3 ) 2 solution, ultrasonic 10min to remove air bubbles, and then continue to soak at room temperature for 24h, and then impregnated Ni(NO 3 ) 2 The raw materials are taken out to obtain cotton-Ni(NO 3 ) 2 The composite was dried at 80 °C for 24 h.

[0036] 2) the dry sample that step 1) obtains in H 2 Under atmosphere, heat from room temperature to 400°C at a heating rate of 2°C / min, then calcinate at 400°C for 3 h, after the product is cooled, use 1% O 2 / N 2 Treat for 2 hours, take it out, and grind it into powder to obtain a catalyst whose active ingredient is nickel coated with carbon material, which is recorded as Ni / C catalyst.

[0037] The carbon material coated nickel catalyst prepared in this embodiment is scanned with a transmission electron microscope, and the resu...

Embodiment 2

[0039] Carry out X-ray diffraction analysis to the carbon material wrapped nickel catalyst prepared in embodiment 1, the X-ray diffraction pattern of gained is as follows figure 2 shown, from figure 2It can be seen that the three peaks at 2θ=44.4°, 51.9° and 76.5° are characteristic peaks of nickel nanoparticles, further indicating the existence of nickel nanoparticles.

Embodiment 3

[0041] The active ingredient prepared in Example 1 is that the nickel catalyst wrapped by carbon material is subjected to X-ray photoelectron spectroscopy analysis, and the valence state of nitrogen and carbon is characterized by XPS technology, and the X-ray photoelectron spectroscopy analysis of gained is as follows: image 3 shown.

[0042] XPS was used to examine the oxidation states of surface elements on Ni / C catalysts. XPS spectra confirmed the presence of Ni, C, N and O in the catalyst mainly ( image 3 a) elements. Such as image 3 As shown in b, the C1s XPS spectrum of the Ni / C catalyst shows a main peak at 284.6 eV, corresponding to sp 2 Hybrid graphitic carbon (C=C). Additionally, two other weak peaks with binding energies of 286.1 eV and 288.9 eV were attributed to C–O and O–C=O species, respectively. Such as image 3 As shown in c, the two fitting peaks are located at and The binding energies of the metals are respectively Ni 2p 3 / 2 and Ni 2p 1 / 2 . T...

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Abstract

The invention relates to the technical field of preparation of primary amine by catalyzing reduction of nitro compounds, in particular to a carbon material coated nickel material catalyst as an effective component and application thereof in catalyzing reduction of a nitro compound to prepare primary amine. The catalyst is prepared by the following method: taking medical absorbent cotton as a raw material, soaking the medical absorbent cotton in a Ni (NO3) 2 solution, ultrasonically removing bubbles, soaking the mixture at room temperature for 3-24 hours, drying a Cotton-Ni (NO3) 2 compound at60-120 DEG C, filling a dried sample into a tubular furnace, and heating; under a hydrogen atmosphere, raising the temperature to 300-600 DEG C at the heating rate of 1-5 DEG C / min, and keeping for 1-5 h; and finally, cooling the black product to room temperature in the hydrogen atmosphere. The preparation method of the catalyst is particularly simple and easy to operate, and the catalyst can be used for preparing the primary amine by catalytically reducing the nitro compound. By utilizing the catalyst, various nitro compounds can be catalytically reduced under the conditions of room temperature, low hydrogen pressure and environment-friendly solvent, the reaction is rapid, and the yield and the selectivity are high.

Description

technical field [0001] The invention relates to the technical field of catalysts and the preparation of primary amine compounds, and more specifically relates to a carbon material-wrapped nickel catalyst and a method for preparing primary amine compounds using the same. Background technique [0002] Amines are very important industrial intermediates and have been widely used as building blocks of pharmaceuticals, agrochemicals, pigments, dyes and fine chemicals. Therefore, there has been increasing interest in the synthesis of amines in recent years. Nitro compounds are easy to obtain, have good stability, and are the starting materials for the synthesis of primary amines. Traditionally, primary amines, such as sulfides, Fe, and Zn, have been synthesized by reducing nitro compounds using stoichiometric reducing agents. The use of a large number of chemical reducing agents leads to high cost of reduction of nitro compounds to primary amines. In addition, these methods rele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C209/36C07C211/46C07C211/47C07C213/02C07C217/84C07C215/76C07C211/52C07C253/30C07C255/58C07C221/00C07C225/22C07C211/06C07C211/35
CPCB01J23/755C07C209/36C07C213/02C07C253/30C07C221/00C07C209/365C07C2601/14B01J35/64B01J35/613B01J35/633C07C211/46C07C211/47C07C217/84C07C215/76C07C211/52C07C255/58C07C225/22C07C211/06C07C211/35
Inventor 刘冰唐庆杰袁紫亮
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES