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A catalyst for selective hydrogenation of aromatic nitro compounds and preparation method thereof

A compound and catalyst technology, which is applied in the field of catalysts and preparations for selective hydrogenation of aromatic nitro compounds, can solve the problems of difficult to realize catalyst reuse, limit the practical application of catalysts, increase the cost of catalyst preparation, etc., and achieve excellent catalytic performance. Reduced weight, easy separation, and easy operation

Inactive Publication Date: 2019-01-22
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, there have been quite a few reports on the selective hydrogenation of substituted aromatic amines. The heterogeneous catalysts reported in the literature are mainly divided into two categories: 1) noble metal catalysts, such as supported gold (WO2007116111-A1; Journal of Catalysis, 265( 2009), 19; Green Chem., 14(2012), 3164) and platinum catalysts (WO2009071727; CN201210468132.8; Journal of Catalysis, 321(2015), 7), etc. These noble metal catalysts are expensive and require additives to control selectivity, and there are problems such as metal residues in the product, which greatly limits the practical application of this type of catalyst
2) Base metal catalysts, literature (Chem.Com., 48(2012), 7982) utilizes citric acid-stabilized iron nanoparticle catalysts to achieve selective hydrogenation of substituted nitro compounds in water. Since the iron catalyst does not use a carrier, Therefore, it is difficult to realize the reuse of catalyst
Although both catalysts have high selectivity, expensive organic nitrogen-containing ligands (1,10-phenanthroline) are used in the catalyst preparation process, which undoubtedly increases the cost of catalyst preparation.
In addition, this preparation method is only suitable for carbon-based supports, and other supports have low activity

Method used

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  • A catalyst for selective hydrogenation of aromatic nitro compounds and preparation method thereof
  • A catalyst for selective hydrogenation of aromatic nitro compounds and preparation method thereof
  • A catalyst for selective hydrogenation of aromatic nitro compounds and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1. Catalyst based on Co and nanographitic carbon

[0036] Take 20ml of distilled water, add 1.875g of tartaric acid under stirring, then add 1.819g of Co(NO3 ) 2 ·6H 2 O, then add 60ml glycerin aqueous solution (glycerin: water = 4:1, volume ratio) and 5.0g polyethylene glycol PEG 6000, finally add 0.5g nano-graphite carbon, after stirring evenly, place in a hydrothermal kettle at 150°C for 13h After drying the obtained solid, it was transferred to a tube furnace for calcination at 800° C. for 2.0 h under argon to obtain a carbon-coated Co catalyst dispersed on nano-graphitic carbon, with a Co content of 29.2 wt%.

[0037] figure 1 The X-ray diffraction pattern of the carbon-coated cobalt-based catalyst shows that the active metal cobalt is in a reduced state.

Embodiment 2

[0038] Example 2. Catalysts based on Ni and nanographitic carbon

[0039] Take 20ml of distilled water, add 1.875g of tartaric acid under stirring, then add 1.818g of Ni(NO 3 ) 2 ·6H 2 O, then add 60ml glycerin aqueous solution (glycerin: water = 4:1, volume ratio) and 5.0g polyethylene glycol PEG 6000, finally add 0.5g nano-graphite carbon, after stirring evenly, place in a hydrothermal kettle at 150°C for 13h , after the obtained solid was dried, it was transferred to a tube furnace and calcined at 800° C. for 2.0 h under argon to obtain a carbon layer-coated Ni catalyst dispersed on nano-graphitic carbon, and the Ni content was 28.0 wt%.

[0040] figure 2 The transmission electron microscope image of the cobalt-based catalyst coated with the carbon layer shows that the active metal cobalt nanoparticles are coated with a carbon layer of about 2-5nm.

Embodiment 3

[0041] Example 3. Catalysts based on Cu and nanographitic carbon

[0042] Take 20ml of distilled water, add 1.875g of tartaric acid under stirring, then add 1.51g of Cu(NO 3 ) 2 ·3H 2 O, then add 60ml glycerin aqueous solution (glycerin: water = 4:1, volume ratio) and 5.0g polyethylene glycol PEG 6000, finally add 0.5g nano-graphite carbon, after stirring evenly, place in a hydrothermal kettle at 150°C for 13h , after the obtained solid was dried, it was transferred to a tube furnace for calcination at 800° C. for 2.0 h under argon to obtain a carbon layer-coated Cu catalyst dispersed on nano-graphitic carbon, with a Cu content of 30.1 wt%.

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Abstract

The invention relates to a catalyst for selective hydrogenation reaction of an aromatic nitrocompound and a preparation method of the catalyst. The catalyst consists of a catalyst carrier and active metal coated with carbon, wherein the catalyst carrier includes a carbon-base carrier, SiO2, TiO2 or Al2O3; the active metal is selected from Co, Fe, Ni or Cu and other poor and noble metals. The catalyst is prepared by adopting a Pechini type sol-gel process which comprises the steps of dispersing an active metal precursor to water containing a coordination compound, adding a polyhydric alcohol solution and a macromolecule auxiliary, then adding the carrier, stirring for dispersion, carrying out hydrothermal reaction, separating out solid on the lower layer, and calcining in the inert atmosphere to obtain the catalyst in which carbon coats the active metal. Compared with the prior art, the catalyst can realize the hydrogenation reaction of a substituted aromatic nitrocompound in the mild condition; substrate conversion rate and production selectivity are high; the catalyst has recyclable economy and good application prospect.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular to a catalyst for selective hydrogenation of aromatic nitro compounds and a preparation method thereof. Background technique [0002] Functionalized aromatic amines are a class of important chemical raw materials transformed from substituted aromatic nitro compounds, which are widely used in the synthesis of pharmaceuticals, dyes, polymers, pesticides, spices and surfactants, biomass fuels, etc. Chemical Products. The hydrogenation of nitro compounds to prepare aromatic amines is a common catalytic hydrogenation reaction, which can be realized by many commercial catalysts, such as Pd / C, Pt / C or Raney Ni, etc., and these catalysts are selective in the hydrogenation reaction of substituted nitro compounds. lower. Therefore, the key to successfully realize the selective hydrogenation of substituted aromatic nitro compounds to prepare functional aromatic amines lies in the design o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/75B01J23/755B01J23/72C07B43/04C07C209/36C07C211/46C07C211/52C07C211/51C07C213/02C07C215/76C07C217/84C07C225/22C07C221/00C07C237/30C07C231/12C07C229/60C07C227/04C07C255/58C07C253/30C07D215/40
CPCY02P20/584
Inventor 陈兵峰袁国卿李峰波黄志军
Owner INST OF CHEM CHINESE ACAD OF SCI