引用本文:
荆涛, 覃志乐, 宋伟明, 赵云鹏, 邓启刚. 三丁基锡/SBA-15功能配合物的合成、表征及对Friedel-Crafts反应的选择性催化[J]. 应用化学,
2013, 30(8): 945-950.
doi:
10.3724/SP.J.1095.2013.20580
Citation: JING Tao, QIN Zhile, SONG Weiming, ZHAO Yunpeng, DENG Qigang. Synthesis,Characterization and Catalytic Performance Toward the Friedel-Crafts Acylation of Tributyltin Functionalized SBA-15[J]. Chinese Journal of Applied Chemistry, 2013, 30(8): 945-950. doi: 10.3724/SP.J.1095.2013.20580
Citation: JING Tao, QIN Zhile, SONG Weiming, ZHAO Yunpeng, DENG Qigang. Synthesis,Characterization and Catalytic Performance Toward the Friedel-Crafts Acylation of Tributyltin Functionalized SBA-15[J]. Chinese Journal of Applied Chemistry, 2013, 30(8): 945-950. doi: 10.3724/SP.J.1095.2013.20580
三丁基锡/SBA-15功能配合物的合成、表征及对Friedel-Crafts反应的选择性催化
摘要:
将三丁基氯化锡与SBA-15介孔分子筛在N2气气氛中进行回流反应,得到有机锡无机配合物(C4H9)3Sn-O-SBA-15[Bu3SnS]。利用X射线衍射(XRD)、透射电子显微镜(TEM)、氮气吸附脱附、固体核磁(NMR)和吡啶吸附脱附红外光谱分析(Py-IR)等方法对产物的组成、结构和性质进行了表征。结果表明,产物Bu3SnS具有高度有序的六方介孔结构,与SBA-15相比,Bu3SnS比表面积、孔容和孔径变小,酸性增强。Bu3SnS对苯甲醚Friedel-Crafts酰基化反应具有优异的催化性能,当反应温度为130℃,n(苯甲醚):n(苯甲酰氯)=1.0:2.0,w(cat)=6%(相对于苯甲醚用量),反应时间为5 h,苯甲醚的转化率达到76.0%,对甲氧基二苯酮(p-MBP)选择性达到97.8%。
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关键词:
- 三丁基锡
- / SBA-15
- / 功能配合物
- / Friedel-Crafts反应
- / 选择性催化
English
Synthesis,Characterization and Catalytic Performance Toward the Friedel-Crafts Acylation of Tributyltin Functionalized SBA-15
Abstract:
The organotin inorganic complexes(C4H9)3Sn-O-SBA-15[Bu3SnS]were successfully synthesized by grafting tributyltin on SBA-15 mesoporous molecular sieves in a nitrogen atmosphere. The composition,structure and properties of the samples were characterized by X-ray diffraction(XRD),transmittance electron microscopy(TEM),Hammett indicator method,N2 adsorption-desorption,solid nuclear magnetic resonance(NMR),in-situ pyridine infrared spectroscopy(Py-IR) and so on. The results show that the hexagonal P6 mm mesostructure of parent siliceous SBA-15 is maintained in Bu3SnS. The surface areas,proe size and volume of Bu3SnS are all deceased with the increase of acidity,compared to those of SBA-15. Friedel-Crafts acylation of anisole and benzoyl chloride can be efficiently catalyzed in the presence of Bu3SnS. The reaction conversion of anisole and the selectivity of p-benzoylanisole are 76.0% and 97.8%,respectively,when the molar ratio of anisole to benzoyl chloride is 0.5:1.0,the amount of catalyst is 6%,the reaction temperature is 130℃ and the reaction time is 5 h.
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Key words:
- tributyltin
- / SBA-15
- / functional complex
- / Friedel-Crafts reaction
- / selective catalytsis
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