554-00-7Relevant articles and documents
Efficient and recyclable bimetallic Co–Cu catalysts for selective hydrogenation of halogenated nitroarenes
Lu, Xionggang,Ren, Jiaan,Sheng, Yao,Wang, Xueguang,Wu, Baoqin,Zou, Xiujing
, (2021/12/20)
Silica supported N-doped carbon layers encapsulating Co–Cu nanoparticles (Co1Cux@CN/SiO2) were prepared by a one-step impregnation of Co(NO3)2·6H2O, Cu(NO3)2·3H2O, urea and glucose, following in situ carbothermal reduction. Effects of Cu contents on the catalytic performance of the Co1Cux@CN/SiO2 catalysts were investigated for selective hydrogenation of p-chloronitrobenzene to p-chloroaniline. The Co1Cu0.30@CN/SiO2 with Cu/Co molar ratio of 0.30:1 presented much higher activity and stability than the monometallic Co@CN/SiO2 catalyst. The addition of Cu into Co1Cux@CN/SiO2 catalysts had favorable effects on the formation of highly active Co–N sites and N-doped carbon layer. The role of the N-doped carbon layer was to protect the Co from oxidation by air, and the Co1Cu0.30@CN/SiO2 could be reused for at least 12 cycles without decrease in catalytic efficiency. Mechanistic and in situ infrared studies revealed that the interaction effect between the Co and Cu atoms made the surface of Co highly electron rich, which decreased adsorption of halogen groups and resulting in the enhanced selectivity during chemoselective hydrogenation of halogenated nitroarenes for a wide scope of substrates.
Method for preparing dichloroaniline through chlorination
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Paragraph 0027-0040, (2021/02/13)
The invention relates to a method for preparing dichloroaniline by chlorination. The method comprises the following steps: adding o-chloroaniline into a solvent, and carrying out chlorination reactionat 0-80 DEG C for 2-12 hours; neutralizing the reaction solution with alkali until the pH value is 9-10, and separating the organic phase from the water phase to obtain an organic phase; and carryingout rectification separation on the organic phase to respectively obtain pure products 2,4-dichloroaniline and 2,6-dichloroaniline. According to the invention, the main raw material o-chloroaniline is easy to obtain and low in price, so that the method has relatively high economical efficiency; the method has the advantages of no need of special reagents or solvents, one-step chlorination reaction, mild reaction conditions, simple operation, less wastewater, simple treatment and environmental friendliness, and only generates a small amount of salt-containing wastewater in the neutralization step; and the total yield is greater than 90%, and the purity can reach 99.5% or above, which is higher than the purity of 99% of the product in the prior art.
In Situ Synthesized Silica-Supported Co@N-Doped Carbon as Highly Efficient and Reusable Catalysts for Selective Reduction of Halogenated Nitroaromatics
Sheng, Yao,Wang, Xueguang,Yue, Shengnan,Cheng, Gonglin,Zou, Xiujing,Lu, Xionggang
, p. 4632 - 4641 (2020/07/30)
Silica-supported Co@N-doped carbon (Co@CN/SiO2) catalysts were first prepared by a one-step impregnation with a mixed solution of cobalt nitrate, glucose and urea, followed by in situ carbonization and reduction. The Co@CN/SiO2 catalysts were investigated for the selective reduction of nitro aromatics to the corresponding anilines using hydrazine hydrate. The Co@CN/SiO2-500 carbonized at 500 °C exhibited the highest catalytic activity and excellent stability without any decay of activity after 6 cycles for the reduction of nitrobenzene. Both metallic Co atoms and Co?N species formed in the Co@CN/SiO2 catalysts were active, but the Co?N species were dominant active sites. The high activities of the Co@CN/SiO2 catalysts were attributed to the synergistic effect between the Co and N atoms, promoting heterolytic cleavage of hydrazine to form H+/H? pairs. Representative examples demonstrated that the Co@CN/SiO2-500 could completely transform various halogen-substituted nitro aromatics to the corresponding halogenated anilines with high TOFs and selectivity of '99.5 percent.
