Pd亚纳米簇@SiO2催化芳香硝基化合物加氢制芳胺
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大连理工大学 精细化工国家重点实验室

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TQ426

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中央高校基本科研业务费(DUT20JC31);辽宁省“兴辽英才”项目科技创新领军人才(XLYC1802030)


Subnano-Pd@SiO2 nanospheres for catalyzing hydrogenation of aromatic nitro compounds to arylamines
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State Key Laboratory of Fine Chemicals,Dalian University of Technology

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    摘要:

    以新配制的硝酸钯溶液为原料,在十六烷基三甲基溴化铵/正丁醇/环己烷形成的反相微乳液体系中采用一锅法制备Pd亚纳米簇@SiO2核壳材料,得到质量分数达4%(以SiO2的质量计)、平均粒径为0.7 nm的Pd亚纳米簇。采用TEM、XRD、XPS、N2吸附-脱附对材料的物化性质进行了表征,探讨了其对芳香硝基化合物加氢制芳胺反应的催化性能。结果表明,在温和的反应条件下(50 ℃、1.0 MPa H2),催化剂Pd亚纳米簇@SiO2上硝基苯加氢反应4 h,苯胺的收率高达99.5%。在该催化剂上,其他多种芳硝基化合物加氢反应同样获得了较高的芳胺收率(98.5%~100%)。催化剂Pd亚纳米簇@SiO2循环4次后,活性无明显下降。

    Abstract:

    Subnano-Pd@SiO2 core shell materials were prepared by a one-pot method in a microemulsion made up of cetyltrimethyl ammonium bromide/n-butanol/cyclohexane with newly prepared Pd(NO3)2 solution as raw material. Pd subnanoclusters with an average size of 0.7 nm are uniformly dispersed in the entire SiO2 nanospheres with a high loading amount of 4% on the basis of the mass of SiO2. The physico-chemical properties of the Subnano-Pd@SiO2 were characterized by TEM, XRD, XPS, and N2 adsorption-desorption. The catalytic performances of Subnano-Pd@SiO2 for the hydrogenation reaction of aromatic nitro compounds were investigated. The results showed a 99.5% yield of aniline was achieved through the hydrogenation of nitrobenzene under mild reaction conditions of 50 ℃ and 1.0 MPa H2 for 4 h. Meanwhile, Subnano-Pd@SiO2 was efficient for the hydrogenation of various aromatic nitro compounds to give high yields (98.5%~100%) of arylamines. The activity of Subnano-Pd@SiO2 did not decrease significantly even after being recycled for 4 times.

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王加升,张 莹,叶宏扬,王万辉,包 明. Pd亚纳米簇@SiO2催化芳香硝基化合物加氢制芳胺[J].精细化工,2022,39(12):

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  • 收稿日期:2022-03-30
  • 最后修改日期:2022-06-27
  • 录用日期:2022-07-01
  • 在线发布日期: 2022-10-25
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