Preparation,characterization of superacid SO4
2−/ZrO2-SiO2 and its activity on catalytic synthesis of methyl p-nitrobenzoate |
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引用本文: | 王刚,张立庆.Preparation,characterization of superacid SO4
2−/ZrO2-SiO2 and its activity on catalytic synthesis of methyl p-nitrobenzoate[J].武汉理工大学学报(材料科学英文版),2014,29(5):895-899. |
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作者姓名: | 王刚 张立庆 |
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基金项目: | Supported by Natural Science Foundation of Zhejiang Province(No.Y404082) |
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摘 要: | Solid superacid SO42-/Zr O2-SiO2 was prepared by dip-impregnation method, and its catalytic activity was tested with esterification of p-nitrobenzoic acid and methanol. The optimum conditions were also found, that is, the molar ratio between silica and zirconia was 10:1, the calcination temperature was 550 ℃ and the soaked consistency of H2SO4 was 1.0 mol?L-1. Under the conditions that the ratio of methanol to acid(m L/g) was 12:1, the amount of catalyst was 0.5 g, the reaction time was 5 h and the stirring speed was 800 r?min-1, the yield of methyl p-nitrobenzoate could reach up to 90.5%. Then the characterizations of cataslyst, including the acidity and types of acidic centers, specific surface area and surface structure was respectively examined by Hammett indicator, in-situ pyridine IR, BET method, FT-IR(KBr), transmission electron microscope(TEM), and X-ray diffraction(XRD). The results showed that the catalyst SO42-/Zr O2-SiO2 was superacid with high specific surface area due to Ho-12.70. It contained acidic sites of Lewis and BrΦnsted, and its surface structure changed after esterification. The zirconia crystal was mainly tetragonal and silica crystal was not found.
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关 键 词: | 固体超强酸 对硝基苯 表征 酸催化 对甲基 透射电子显微镜 FT-IR 氧化锆晶体 |
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