氧掺入MoS2调节芳香硝基化合物选择性转氢还原

doi:10.1016/S1872-2067(16)62504-4

催化学报 ›› 2016, Vol. 37 ›› Issue (9): 1569-1578.DOI: 10.1016/S1872-2067(16)62504-4

• 论文 • 上一篇

氧掺入MoS₂调节芳香硝基化合物选择性转氢还原

张超锋, 王旭, 李名润, 张志鑫, 王业红, 司锐, 王峰

a. 中国科学院大连化学物理研究所催化基础国家重点实验室, 洁净能源国家实验室(筹), 辽宁大连 116023;
b. 中国科学院大学, 北京 100049;
c. 中国科学院上海应用物理研究所, 上海同步辐射光源, 上海 201204

收稿日期:2016-06-03 修回日期:2016-07-11 出版日期:2016-09-21 发布日期:2016-09-21
通讯作者: Feng Wang
基金资助:
国家自然科学基金（21422308，21403216，21273231）；大连市优秀青年基金（2014J11JH126）.

Chemoselective transfer hydrogenation to nitroarenes mediated by oxygen-implanted MoS₂

Chaofeng Zhang, Xu Wang, Mingrun Li, Zhixin Zhang, Yehong Wang, Rui Si, Feng Wang

a. State Key Laboratory of Catalysis, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China;
b. University of Chinese Academy of Sciences, Beijing 100049, China;
c. Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201204, China

Received:2016-06-03 Revised:2016-07-11 Online:2016-09-21 Published:2016-09-21
Contact: Feng Wang
Supported by:
This work was supported by the National Natural Science Foundation of China(21422308, 21403216, 21273231) and Dalian Excellent Youth Foundation(2014J11JH126).

摘要/Abstract

摘要：

芳香胺类化合物及其衍生物是一类重要的有机合成中间体，广泛应用于染料、农药、医药及其他精细化学品.目前催化芳香硝基化合物还原制备芳香胺的多相催化体系多使用含有d₆-d₁₀贵金属以及高活性Ni的催化剂.为了提高反应的选择性，金属纳米颗粒的尺寸控制、合金效应、金属载体强相互作用、溶剂以及添加剂的筛选等不同手段被采用.考虑到该类催化剂复杂的制备方法以及易氧化的性质，近年来稳定高效的非贵金属体系的开发得到了广泛关注.MoS₂是一类重要的高温加氢催化剂，不饱和的Mo位点（CUS Mo）被认为在催化过程中起到了关键性作用.但是理论与实践已经证明，作为代表性的二维材料，MoS₂的活性位点多集中于层状结构的边楞结构处.占有最大暴露面积的基面结构因为稳定的Mo-S化学键组成在化学反应中多表现为催化惰性.通过剥离的手段可以有效提升活性位点的数目，但新增的活性位点仍然多集中于层状结构的边楞结构处而不是基面.在MoS₂与MoO₂结构中Mo-S和Mo-O的键长不同，同时S和O的配位形式也不同.可以预见的是，如果MoS₂结构中的一部分S元素被O元素取代，在这样的材料中将会出现大量缺陷以及活性CUS Mo结构.结合先前关于硫化钼材料的制备方法，我们通过部分硫化还原[Mo₇O₂₄]^6-前驱物的方法制备了氧掺杂的MoS₂材料（标记为O-MoS₂）.通过XRD，XPS，Raman和EDX等表征发现，不同的Mo-O结构存在于O-MoS₂材料中.HRTEM表征结果显示，O-MoS₂表面存在着丰富的结构缺陷.EXAFS结果显示，O-MoS₂材料中可能含有四配位以及五配位的CUS Mo结构.以甲酸铵还原硝基苯为探针反应检测了CUS Mo结构.发现O-MoS₂可以在水相条件下高效催化芳香硝基化合物还原生成相应的芳香胺，且催化剂稳定，可以多次循环使用.结合对照不同催化剂的NH₃-TPD数据以及MoS₂结构模型，我们发现O-MoS₂材料中含有丰富的CUS Mo结构，这些CUS Mo结构更多地存在于材料的基面而非边楞结构.我们认为，对于该类掺杂MoS₂材料的制备及结构表征将有利于拓宽MoS₂催化剂从高温气相反应到温和液相反应中的应用.

关键词: 二硫化钼, 不饱和Mo位点, 芳香硝基化合物, 转氢氢化, 甲酸盐, 多相催化

Abstract:

We present an efficient approach for the chemoselective synthesis of arylamines from nitroarenes and formate over an oxygen-implanted MoS₂ catalyst(O-MoS₂). O-MoS₂ was prepared by incomplete sulfiidation and reduction of an ammonium molybdate precursor. A number of Mo-O bonds were implanted in the as-synthesized ultrathin O-MoS₂ nanosheets. As a consequence of the different coordination geometries of O(MoO2) and S(MoS₂), and lengths of the Mo-O and Mo-S bonds, the implanted Mo-O bonds induced obvious defects and more coordinatively unsaturated(CUS) Mo sites in O-MoS₂, as confirmed by X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, high resolution transmission electron microscopy, and extended X-ray absorption fine structure characterization of various MoS₂-based materials. O-MoS₂ with abundant CUS Mo sites was found to efficiently catalyze the chemoselective reduction of nitroarenes to arylamines.

Key words: MoS₂, Coordinative unsaturated Mo, Nitroarene, Transfer hydrogenation, Formate, Heterogeneous catalysis

张超锋, 王旭, 李名润, 张志鑫, 王业红, 司锐, 王峰. 氧掺入MoS₂调节芳香硝基化合物选择性转氢还原[J]. 催化学报, 2016, 37(9): 1569-1578.

Chaofeng Zhang, Xu Wang, Mingrun Li, Zhixin Zhang, Yehong Wang, Rui Si, Feng Wang. Chemoselective transfer hydrogenation to nitroarenes mediated by oxygen-implanted MoS₂[J]. Chinese Journal of Catalysis, 2016, 37(9): 1569-1578.

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氧掺入MoS₂调节芳香硝基化合物选择性转氢还原

Chemoselective transfer hydrogenation to nitroarenes mediated by oxygen-implanted MoS₂

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