- Tailoring supported palladium sulfide catalysts through H 2-assisted sulfidation with H2S
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Supported palladium sulfide catalysts are of great interest in selective hydrogenation reactions. In this work, "Pd4S", "Pd3S", "Pd16S7" and "PdS" supported on activated carbon were selectively synthesized by tailoring the H2-assisted sulfidation of Pd/C with H2S at 150-750°C, and were characterized by means of XRD, XPS, TEM, HRTEM, EDS, BET and H2-TPR techniques. The results indicated that the sulfidation atmosphere, the sulfidation temperature and the metal-support interaction all played important roles in determining the crystal structure and composition of the PdxSy/C catalysts, which in turn gave different catalytic performances in the synthesis of N-(1,3-dimethylbutyl)-N′- phenyl-p-phenylenediamine (6PPD) by the reductive N-alkylation of aromatic amines. PdS/C showed the highest selectivity (>97%) and stability among all the PdxSy/C catalysts.
- Xu, Wei,Ni, Jun,Zhang, Qunfeng,Feng, Feng,Xiang, Yizhi,Li, Xiaonian
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- Method for preparation of anti-aging agent 6PPD by using micro-reactor
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The invention discloses a method for preparation of an anti-aging agent 6PPD by using a micro-reactor; a homogeneous solution of p-aminodiphenyl amine and methyl isobutyl ketone and hydrogen gas are subjected to a reaction in a gas-liquid reactor, then are introduced into a solid-liquid reactor and are subjected to a reaction, and the obtained reaction liquid repeats the above operations. Compared with the prior art, the gas-liquid reactor and the solid-liquid reactor are connected in series, the gas-solid-liquid three-phase reaction is performed in a micro-channel, and eventually, the conversion rate of raw materials is improved and the reaction time is shortened. The micro-reactor has the advantages of large specific surface area and strong heat transfer and mass transfer abilities, and enables the reactions to be carried out efficiently; and the reaction temperature, time and material ratio and other conditions can be precisely controlled through the micro-channel reactor, by-products are reduced, and the security is improved.
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Paragraph 0029; 0030; 0031; 0032; 0033; 0034; 0035-0046
(2017/08/25)
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- Preparation, structural characterization of a novel egg-shell palladium sulfide catalyst and its application in selective reductive alkylation reaction
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A novel egg-shell Pd-S catalyst with palladium metal as the core and a membrane of palladium sulfide as the surface has been prepared by sulphidizing Pd/C with H2S. This catalyst is effective for the reductive alkylation of p-amino diphenylamine (PADPA) and methylisobutyl ketone (MIBK) to afford N-(1,3-dimethylbutyl)-N′-phenyl-p-phenylenedianine (DBPPD) with conversion up to 99.42% and selectivity to 97.46%. Comparing with the other common palladium sulfide catalysts, the membrane of palladium sulfide on the surface and the core of palladium metal cause the Pd on the surface of the new catalyst in a lower sulfur coordination, which improves its activity. Our result indicates that this new egg-shell Pd-S/C is an efficient hydrogenation catalyst.
- Zhang, Qun Feng,Wu, Jia Chun,Su, Chang,Feng, Feng,Ding, Qiao Ling,Yuan, Zhao Lian,Wang, Hong,Ma, Lei,Lu, Chun Shan,Li, Xiao Nian
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p. 1111 - 1114,4
(2020/08/20)
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