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1、广灭灵的生产合成工艺牛亚军（河南科技学院，化学化工学院制药 051班，河南，新乡，453003）摘 要广灭灵是 20 世纪 80 年代美国 fmc（富美实）公司研制开发生产的品种，中文通用名称是异恶草酮、异恶 草松，英文通用名称 为 2-（2-氯苄基）-4，4-二甲基异唑-3-酮 ，原 药有效成分含量大于 90%，为淡黄色粘稠液体，易溶于氯仿、甲醇、二甲苯、乙腈、甲苯等有机溶剂，常温贮存稳定期为 1 年以上。广灭灵是我国 90 年代中期从国外引进的新型高效农药,使用效果良好,目前国内仍以进口为主。本品通 过抑制异戊二烯化合物合成,阻碍胡萝卜素和叶绿素生物合成 ,因此效力很高。可用于大豆田防除阔
2、叶杂草和禾本科杂草及用于木薯、玉米、油菜和烟草田以除去杂草。 该药一般用于芽前或植前混土处理,用量仅为1.1 gPL, 所以其应用将越来越广泛。 尽管目前对该农药残留提出限量的国家或地区有限,但随着该农药应用的普及和国际贸易的发展,对其残留限制的国家将日趋增多,所以广灭灵残留的检测也就显得格外重要,残留分析结果的准确性直接取决于所使用农药标准品质量的高低 ,所以农药的制 备纯化已成为分析工作者的一个重要研究方向。由于我国目前尚没有该农药标准品,也无该农药的生产厂家,进口的该农药制剂含量仅为 48 %, 如以此为原料提 纯标准品,仍有很多不便。我国生产广灭灵的农药公司有 100 多家，全国广灭灵
3、年生产量达 2 亿吨。但是各个厂家的生产工艺各不相同。 （可否将红色部分内容做一下更改？论文内容没有涉及农药残留问题摘要中不应有这方面体现， ）本文研究了广灭灵粗品的合成工艺，由原料酰氯、二氯乙烷、 盐酸羟胺、盐酸、液碱、四丁基羟胺、 纯碱等通 过酰化、 环化、缩合并进一步脱溶最终得到广灭灵粗品。并进一步研究了一些控制变量实验，从中得出更为合理的控制条件和一些注意事项。从而完善了广 灭灵的生产工艺和操作条件。关键词：异恶草松；高效农药；残留；合成；酰化；环化；缩合；脱溶；蒸馏THE PRODUCTION PROCESS OF CLOMAZONE SYNTHETICAbstractClomazo
4、ne is the production of varieties which developed by the company of the U.S. fmc (Phu My ) in the 80 age of the 20th century. the Chinese common name is Clomazone, clomazone, English common name for 2 - (2 - chloro-benzyl) -4 , 4 - dimethyl triazole vary -3 one, the original drug content of the acti
5、ve ingredient is more than 90%, in order to light yellow viscous liquid, soluble in chloroform, methanol, xylene, acetonitrile, toluene and other organic solvents , room temperature storage stability over a period of a year.Clomazone is an efficient introduction of new pesticides from abroad in the
6、mid-90s in our country, the use of which is effective, currently still the main imports. This product by inhibiting is the synthesis of isoprene compounds that prevent the biosynthesis of carotenoids and chlorophyll, so the effectiveness is very hingh. Soybean field can be used to control broad-leav
7、ed weeds and grass weeds and for cassava, corn, rapeseed and tobacco fields to remove weeds. The drug is generally used before the mixed-sik before germination or soil treatment, the amount of only 1.1 gPL, so its use will become more and more widely. However, the toxicity of certain pesticides Alth
8、ough the pesticide residue limits to limited countries or regions, but with the popularity of the application of pesticides and development of international trade, their residues will become increasingly limited number of countries, so Clomazone residue detection will be particularly important resid
9、ual analysis of the accuracy of the direct use of pesticides depends on the quality standard, so the preparation and purification of pesticide analysis of workers has become an important research direction. Because of the pesticides currently no standard, nor does the pesticide manufacturers, pestic
10、ide formulations of the import content of only forty-eight percent, such as the purification of raw materials as a standard, there are still a lot of inconvenience.In china there is more than 100 companies that product pesticides of clomazone across the country Clomazone annual production capacity o
11、f 200 million tons. However, all manufacturers of production technology varies.In this paper, the design of a simple synthesis process, from raw materials chloride, dichloroethane, hydroxylamine hydrochloride, hydrochloric acid, liquid, tetrabutylammonium hydrochloride, sodium carbonate, such as thr
12、ough the acylation, cyclization, reduced further from the merger finally dissolved Clomazone crude. And the design of the experiment a number of experimental control variable, which was out of control conditions is more reasonable, and some attention. To work together in order to improve the product
13、ion of synthetic Clomazone process.Key words: Clomazone; efficient pesticide; residues; synthesis; acylation; cyclization; condensation; from melting; distillation目 录摘 要.ABSTRACT.1 绪论.11.1 作用及特点.11.2 适用作物及登记作物.11.3 防治对象.11.4 基本特性及应用现状.12 合成条件的选择.22.11-氯-2，2-二甲基- 丙酰羟胺合成路线.2（1）溶剂二氯乙烷的选择.3（2）酰氯的选择.32.2*的合成路线.3（1）环化中二氯乙烷的影响.3（2）二氯乙烷废渣蒸馏.42.3*的合成路线.4（1）四丁基溴化铵实验.4（2）废油相处理.52.4 破坏性实验.63 3. 广灭灵粗品的的合成.63.1 酰化.73.2 环化.
