【作者】 于家涛；

【导师】 宋华；

【作者基本信息】 大庆石油学院 ， 化学工程， 2008， 硕士

【摘要】 本文研究了以对叔丁基甲苯(PTBT)为原料,分别以氧气和30%双氧水为氧化剂,常压下氧化PTBT合成对叔丁基苯甲酸(PTBA)的工艺路线。在以氧气为氧化剂的实验中,我们分别研究了以醋酸钴和硫酸锰为催化剂时两种工艺条件下氧化PTBT合成PTBA的反应。当以醋酸钴为催化剂时,在常压无溶剂条件下,考察了促进剂种类、催化剂用量、促进剂用量、反应时间、温度、氧气流速等一系列因素对反应的影响。常压下适宜的反应条件为:催化剂与原料的质量比0.027、促进剂用量0.3mL、反应时间8h、反应温度130℃、氧气流速100mL/min。在此反应条件下,PTBA产率达到68.09%。当以硫酸锰为催化剂时,研究了不同种类氧化促进剂、催化剂量、促进剂量、温度、氧气流速、反应时间等一系列因素对反应的影响。常压下适宜的反应条件为:催化剂与原料的质量比0.027、溴化钠0.5g、反应温度130℃、氧气流速100mL/min、反应时间8h。此时,PTBA的收率达到66.94%。在以双氧水为氧化剂的实验中,发现双氧水—溴化钠是一个很好的催化氧化体系,同时研究了双氧水用量、乙酸酐用量、反应时间、溴化钠用量、温度以及盐酸用量等因素对反应的影响。常压下适宜的反应条件为:PTBT4mL、乙酸酐6mL、溴化钠与PTBT质量比0.029、盐酸0.06mL、双氧水与PTBT摩尔比2.653、反应时间6h、反应时间8h,此时PTBA的收率达到47.76%。本文所研究的液相催化氧化PTBT合成PTBA的工艺路线具有绿色环保、条件缓和、成本低廉等优点,为氧化合成其它有机物探索出了一条可循之路,具有一定的参考价值。更多还原

【Abstract】 In this text,the craft route of p-tert-butylbenzoic acid（PTBA） synthesis is studied under atmospheric pressure,which taked p-tert-butyltoluene（PTBT） as material,oxygen and 30% hydrogen peroxide as green oxidant respectively.In the experiment with no solvent,the reaction under two kind of crafts were studied conditions separately,which taked Co（COOH）₂ and MnSO₄ as catalyst respectively to synthesize PTBA from PTBT.The influence of a series factors such as species and dosage of the promoter,the dosage of the catalyst,the time and temperature of the reaction as well as the velocity of oxygen on the reaction were investigated in the experiment taking oxygen as oxidant and Co（COOH）2 as catalyst under atmospheric pressure without solvent,and the proper reaction conditions were determined under atmospheric pressure as follows:the mass ratio of the catalyst and the material,dosage of the promoter,time and temperature of the reaction and the velocity of oxygen were 0.027,0.3mL, 8hours,130℃and 100mL/min respectively.Under such reaction conditions,the yield of p-tert-butylbenzoic acid reached 68.09%. The influence of a series factors such as species and dosage of the promoter,the dosage of the catalyst,the time and temperature of the reaction as well as the velocity of oxygen on the reaction were investigated in the experiment using oxygen as oxidant and MnSO4 as catalyst under atmospheric pressure without solvent,and the proper reaction conditions were determined under atmospheric pressure as follows:the mass ratio of thecatalyst and the material,dosage of the promoter,time and temperature of the reaction and the velocity of oxygen were 0.027, 0.5g, 8hours,130℃and 100mL/min respectively.Under such reaction conditions,the yield of p-tert-butylbenzoic acid reached66.94%.In the experiment taking H₂O₂ as oxidant, we discovered that the H₂O₂-NaBr was a very good catalyzed system,and the influence of a series factors on the reaction such as the dosage of hydrogen peroxide,the dosage of acetic anhydride,the dosage of bromide natrium,the time and temperature of the reaction and the dosage ofhydrochloric acid were investigated.Under optimal reaction conditions: the dosage ofPTBT was 4 mL,the dosage of acetic anhydride was 6 mL,the mass ratio of the NaBr and the material was 0.029,the dosage of hydrochloric acid was 0.06mL,the mo l ratio of the H₂O₂ and the material was 2.653,the temperature and time of reactionwas 80℃and 8h respectively, the yield of p-tert-butylbenzoic acid reached 47.76%.The craft route of synthesis of PTBA by Liquid-phase oxidation of PTBT that was studied in this text has many advantages such as environment-friendly,conditions moderately and lowest costing etc. This work opened up a new way that can be followed by green synthesis of other organic compounds and has a certain referencevalue.更多还原