硫氰化工艺条件对甲基硫菌灵含量的影响论文.docVIP

硫氰化工艺条件对甲基硫菌灵含量的影响 摘 要 甲基硫菌灵是目前全球使用量最大的高效低毒、广谱、内吸性杀菌剂，具有低毒、低残留的优点。甲基硫菌灵的合成过程中，采用硫氰酸钠与氯甲酸甲酯合成中间体异硫氰基甲酸甲酯，然后与邻苯二胺反应生成甲基硫菌灵的方法，此法第一步硫氰化反应对合成产品中甲基硫菌灵原粉的含量影响十分明显。因此对于硫氰化反应条件的讨论将有助于提高产品含量，提高产品质量，为生产指导提供一定的依据。 本研究通过实验确定了硫氰化反应的最佳保温温度、最佳保温时间、最佳条件下进反应物的物料配比，实验结果表明在最佳条件下制得的甲基硫菌灵含量达到了98%以上。 关键词：甲基硫菌灵; 硫氰化反应;反应条件 Processing conditions of sulfur cyaniding response on thiocyanate thiophanate-methyl content Zhangfeng (Biochemistry engineering department, Anhui University of Technology and Science ,Wuhu, Anhui 241000) Abstract Thiophanate-methyl to be the world’s most efficient use of low toxicity, broad-spectrum, with absorption of fungicides with low toxicity, the advantages of low-residue. In the process of thiophanate-methyl synthesis, we use the method that cyano-methyl isothiourea intermediates which is made by sodium thiocyanate with methyl chloroformate synthesis with o-phenylenediamine reaction , In this method the first step of the synthesis of sulfur cyanation is very obvious to the content of the thiophanate-methyl original. Therefore the discussion for thiocyanate reaction conditions will help us to improve the utilization of raw materials, improve product quality, to provide a guide for the production basis. Through a lot of experiments this study identified the best insulation temperature, the best holding time, the best material ratio under the best conditions in sulfur cyaniding response. The results show that the content of products for thiophanate-methyl under the best conditions is more than 98%. Key words：thiophanate-methyl ; sulfur cyaniding response ; reaction conditions 目 录 引言 6 第1章 实验部分 7 1.1 试剂及仪器 7 1.1.1试剂 7 1.1.2仪器 7 1.2实验原理 7 1.3实验思路 7 1.4实验方法 8 1.4.1产品的合成 8 1.4.2产品含量的检测 8 第2章 结果与讨论 9 2.1工艺条件的对比实验 9 2.1.1原料配比的对比实验 9 2.1.2保温温度的对比实验 10 2.1.3保温时间对比实验 10 2.2工艺条件的验证实验 11 2.2.1原料配比验证实验 12 2.2.2保温温度验证实验 12 2.2.3保温时间验证实验 13 结论与展望 15 谢 辞 16 参考文献 17 插图清单 图2- 1 氯甲酸甲酯（98.50%）用量对比实验数据分析 9 图2- 2 保温温度对比实验数据分析 10