控制氧化合成对氯苯甲醛的研究-应用化学专业毕业论文.docxVIP

南京理工大学硕士论文 南京理工大学硕士论文 控制氧化合成对氯苯甲醛的研究 摘 要 对氯苯甲醛是重要的有机合成中间体。近年来，随着绿色化学的发展，以氧气 作为清洁、廉价氧源，实现对氯甲苯的选择性氧化制备对氯苯甲醛的反应受到研究 者们的普遍关注。论文主要研究了AmocoMC催化体系下对氯甲苯的选择性氧化， 对AmocoMC催化剂进行了筛选，得出较佳的催化体系为：co(oAc)2．MnS04．KBr 作催化剂，冰乙酸为反应介质，并对该催化体系下各工艺参数的影响迸行了研究， 得出最优工艺条件：Co／Mn／Br混合催化剂加入量7％(质量分数)，质量比2：2：1， 反应温度80℃，．反应时间30min，氧气压力O．3MPa，在此条件下，对氯苯甲醛收 率达21．95％，此时的选择性为41．85％。为了提高反应的选择性，论文初步研究了 以乙醛作为添加荆条件下各工艺参数的影响，并进行正交优化，得出最佳条件为： 乙醛加入量l；10(与底物的摩尔比)，反应温度100℃，反应时间30min，氧气压 力0．2MPa，Co／Mn／Br混合催化剂加入量7％(质量分数)，质量比2：2：l。在此 条件下，反应产率为24．10％，选择性可达75．03％。 关键词：AmocoMC催化体系，选择性氧化，对氯甲苯，对氯苯甲醛 南京理工大学硕士论文 南京理工大学硕士论文 控制氧化合成对氰苯甲醛的研究 Abstract P—chlorobenzaldehyde is an important intermediate in the organic synthesis．In recent years，with the development of green chemistry,great aRenfion has been paid on the selective oxidation of P--chlorotolueno to prepare P-ehlorobenzaldehyde，using 02 as clean and cheap oxidant．In the present work,we aimed tO study the selective oxidation catalyzed by the Amoco MC catalyst system．Different AmoenMC catalysts were selected and the optimum catalyst system Was obtained：Co(OAth·-MnS04-·KBr as cmalyst and acetic acid as reaction medium．The effects of different variables On the catalyst system were studied and the optimum reaction conditions were as follows：the amount of the composite catalyst Co／Mn／Br 7％(mass percentage based on)，the mass ration of different ingredients 2：2：l，reaction temperature 80℃，reaction time 30min，the oxygen pressure 0．3ma．Under these conditions，21．95％ P-chlorobenzaldehyde Was obtained with 41．85％selectivity．To improve the selectivity, the Co／Mn／Br catalyst system with ethanal as all additive was studied and the reaction conditions were also optimized，which Wgle as follows：the amount ofcthanal tO％(mole ration base on the substrate)，reaction temperature 100℃，reaction time 30min，the oxygen pressure O．2MPa,the amount of the composite‘catalyst Co／Mn／Br 7％(mass percentage based on)．the mass ration of different ingredients 2：2；1．Under these condition