对三氟甲基苯腈的合成

论文编号:ZY031    论文字数:7844,页数:19

摘 要：介绍了含氟化合物的特性，结合当今农业中含氟农药的应用现状，阐述研究含氟农药中间体的意义。对农药中间体对三氟甲基苯腈的合成进行了探索性研究。以对三氟甲基氯苯与氰化钠在活性膦镍[Ni(PPh3)3]催化剂下发生均相催化反应，得到的产物进行精馏分离提纯，即得对三氟甲基苯腈。催化剂中镍盐、三苯基膦与还原剂锌粉的最佳配比为1:3:9，催化反应的原料比Ni(PPh3)3: 对三氟甲基氯苯:氰化钠为1:31:34，以对三氟甲基氯苯计收率达到52.6%。采用红外光谱、质谱、气相、氢核磁共振谱等手段对产物结构进行分析鉴定。该结果对开发实际生产技术具有一定的指导作用。
关键词：含氟农药中间体；对三氟甲基氯苯；对三氟甲基苯腈；均相催化；膦镍催化剂 
 
Abstract: This article describes the characteristics of fluorine-containing compounds, and explain the significance of fluoride pesticide intermediates, combining with the current application status of fluorine-containing pesticides. Special attention to the pesticide intermediates 4-trifluoromethyl benzonitrile synthesis is drawn. 4-Chlorobenzotrifluoride and sodium cyanide in the activity of nickel-phosphine catalyst [Ni(PPh3)3] have the homogeneous catalysis reactions, The product obtained by distillation separation and purification, that get 4-trifluoromethyl benzonitrile. Nickel salt, triphenylphosphine and zinc have the best molar ratio of 1:3:9, raw material [Ni(PPh3)3], 4-chlorobenzotrifluoride and NaCN feed ratio of 1:31:34 .the yield reached 52.6%. The IR, MS, GC, 1HNMR will be prepared for structural analysis and identification of pure product. .This study optimizes the reaction conditions and improves the conversion rate and selectivity, increased industrial applicability.

Keywords：Fluoride pesticide intermediates; 4-chlorobenzotrifluoride; 4-trifluoromethyl benzonitrile; Homogeneous catalysis, Phosphine nickel catalyst
目  录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
 1.1 含氟化合物的特征及用途 1
 1.2 含氟农药中间体 1 
 1.3 对三氟甲基氯苯简介 2
 1.4 对三氟甲基苯腈 3
2. 实验部分 5
 2.1 化学试剂和仪器 5
6
 2.2 实验步骤 6
 2.3 气相色谱（GC）检测条件 7
3. 结果与讨论 7
 3.1 催化剂的制备条件优化 7
 3.3 对三氟甲基苯腈产品的含量分析及结构鉴定结果 10
4．总结与展望 13
致谢 15
参考文献 16

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