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作 者:卢荣[1] 黄金艳[1] 朱路群[1] 胡春梅[1] 吕兴强[1] LU Rong;HUANG Jinyan;ZHU Luqun;HU Chunmei;LYU Xingqiang(School of Chemical Engineering,Northwest University,Xi’an 710069,China)
出 处:《化工技术与开发》2018年第6期5-10,共6页Technology & Development of Chemical Industry
基 金:陕西省教育厅专项科研计划项目(12JK0577)
摘 要:以3,5-二叔丁基水杨醛和邻苯二胺为单体,合成单边席夫碱配体L2,再在配体L2的基础上,以金属离子Ni2+为活性中心,与3种带有不同推拉电子基团的醛进行反应,制备了3个双边不对称席夫碱镍配合物,并利用FT-IR、元素分析对所制备的配体及配合物结构进行了表征。以70%的TBHP为氧源,考察不对称席夫碱镍配合物对苯乙烯环氧化反应的催化性能,并对反应工艺条件进行优化,考察反应时间、氧化剂用量、反应温度、溶剂类型、催化剂用量等条件对苯乙烯的转化率和环氧苯乙烷选择性的影响。实验结果表明,当反应时间为4h、氧化剂用量为9mmol、反应温度为65℃、溶剂为CHCl3、催化剂用量为0.01mmol时,苯乙烯的转化率和选择性达到最大,分别为79.05%、37.17%。Firstly, three unilateral single-site schiff-base Ni^2+ catalysts were synthesized with Ni^2+, three different aldehydes containing different electronic-pulling and electronic-withdrawing groups and ligand L2 which was synthesized with 3,5-di-tert-butylsalicylaldehtde and 1,2-diaminobenzene. The molecular structures of the catalysts and ligand L2 were characterized by infrared spectra(FTIR) and elemental analysis. Then, the catalytic ability on epoxidation of styrene by the oxidant of 70% TBHP was tested. Thirdly, the reaction by change the reaction time, the molar ratio of styrene to TBHP, the temperature, the solvent and the amount of catalyst, was optimized. A maximum of 79.05% conversion and 37.17% selectivity was obtained when the time was 4 h, molar ratio was 1:3, 65℃, CHCl3 as solvent and 0.01 mmol catalyst.
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