三段硝化法合成3,5-二硝基-4-氯三氟甲苯的工艺研究

论文编号:SW176  论文字数:11295,页数:23

摘要：本文以对氯三氟甲苯为起始原料经“三段硝化”合成除草剂氟乐灵中间体3，5－二硝基－4－氯三氟甲苯的工艺制法进行讨论研究。对一硝化安排了正交试验，找到了最佳工艺条件，收率可达到97.5％。对两段二硝化分别做了单独硝化和套酸试验，也进行了连续式硝化的试验，转化率达到了要求。证明了三段硝化法对合成3，5－二硝基－4－氯三氟甲苯的工艺有了一定的改进。
关键词：氟乐灵;3,5-二硝基-4-氯三氟甲苯；对氯三氟甲苯；三段硝化法；

Abstract: This paper to the chlorine trifluoromethyl toluene as the starting material by the "three of nitrification" synthetic herbicide trifluralin intermediate 3,5 - Nitro -4 - chlorine trifluoromethyl toluene system of law discussed. Arranged for a nitrification orthogonal experiment to find the optimum conditions. Second of two nitrification were done a separate set of nitrification and acid test, also had a continuous nitrification of the test, reached a conversion rate of demand. Three of the initial proof of the nitration of 3,5 - Nitro -4 - chlorine trifluoromethyl toluene Process Improvement better results.
Keywords：Trifluralin; 3,5 - Nitro -4 - chlorine trifluoromethyl toluene; chloro trifluoromethyl toluene; three denitrification;

目  录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
 1.1 引言 1
 1.2 除草剂氟乐灵简介 2
     1.2.1 理化性质 3
     1.2.2 药效 3
     1.2.3 氟乐灵制备方法 3
     1.2.4 中间体3,5-二硝基-4-氯三氟甲苯制备工艺现状 3
 1.3 三段硝化法合成3,5-二硝基-4-氯三氟甲苯的目的和意义 4
2. 实验部分 6
 2.1 试剂、样品 6
 2.2 仪器及玻璃器皿 6
 2.3 实验条件 7
     2.3.1 一硝化 7
     2.3.2 二硝化 7
             2.3.3 气相色谱分析条件 8
3. 结果与讨论 9
 3.1  硝化反应条件的优化试验 9
 3.1.1 一硝化反应条件的选择与优化 9
 3.1.2 二硝化反应的试验研究 10
    3.2 方法的评价 19
4．总结与展望 20
致谢 21
参考文献 22