氯甲苯均相催化氧化制备对氯苯甲酸相关异构体的气相色谱分析-分析化学专业毕业论文.docxVIP

氯甲苯催化氧化制备对氯苯甲酸相关异构体 氯甲苯催化氧化制备对氯苯甲酸相关异构体 的气相色谱分析 分析化学专业 研究生 刘恒 指导教师周在德副教授 对氯苯甲酸是一种重要的精细化工产品，广泛用于有机合成中间体、农 药、医药、防腐剂、染料和发光材料等。因此，研究对氯苯甲酸的制备及其 相关异构体的测定方法具有很重要的理论意义和实用价值。 本文研究了以混合氯甲苯为原料，异羟肟酸金属络合物为均相催化剂， 空气为氧源的对氯苯甲酸的制备反应，在1400C常压反应约9小时，对氯甲 苯的转化率达65％，收率达77．2％，产物经气相色谱分析，未检测出邻、间 氯苯甲酸，对氯苯甲酸的纯度达87．7％。同时，还考察了不同反应温度，不 同空气流速，不同催化助剂对反应的影响。 为了研究混合氯甲苯的均相催化氧化过程，快速有效地测定氧化产物及 其分布，本文分别建立了测定氯甲苯异构体和氯代苯甲酸异构体的气相色谱 分析方法。在PEG-20M毛细管柱上，通过直接迸样，邻、间、对氯甲苯混合 物得到了很好的分离。采用内标法定量，定量结果令人满意，回收率达94％ 以上，变异系数小于6％。在HP．5毛细管柱上，采用甲酯衍生化法，使邻、 间、对氯苯甲酸的甲酯化衍生物得到良好的分离。采用内标法定量，能准确 测定混和氯甲苯氧化过程中的氯代苯甲酸异构体的含量，回收率达92％以上， 变异系数小于3 6％。 关键词：对氯苯甲酸混合氯甲苯均相催化氧化气相色谱异构体分离 Gas Gas Chromatography Analyses of Relative Isomers in p—Chlorobenzoic Acid Prepared from Chloroto luene by Catalyst Oxidation MajOre：Analytical Chemistry Graduate：Liu Heng Advisor：Zhou Zaide As an important product of fine chemical．p—chlorobenzoie acid is widely used in the fields of organic intermidiates，pesticides，medicines，antiseptics，dyes and emitting materials．Therefore,it is important in scientificity and practicability to study the synthesis of P—chlorobenzoic acid and detection of its isomers 65 percent of transformation rate of p-chlorotoluene and 77．2 percent of yield of p-chlorobenzoie acid had been attained after about nine hours’reation under normal pressure at 1400C，on condition that ori#nal material was chlorotoluene mixtures，single phase catalyst was metal complexes of N—benzoyI-N-phenylhydroxylamine and oxidizer comed from air．The products， analyzed by gas chromatography,didn’t contain o．or m-chlorobenzoic acid but p-chlorobenzoic acid whose purity was 87 7 percent．Meanwhile，the influences of different temperature，air velocity of flow and catalyst additives on catalytic oxidatioil had been studied． In order to study the process of single phase catalyst oxidation of chloro． toluenes mixtures to detect the oxidized product and its distribution，two approaches to detecting chlorotoluene isomers and chlorobenzoic acid isomers throu曲gas chromatography