以1,1,2-三氯乙烷為原料與氫氧化鈉溶液反應(yīng),生成偏二氯乙烯,偏二氯乙烯在混酸(硝酸與鹽酸)的作用下,生成1,1-二氯-2-硝基乙烯,考察了溫度,時同,三氯乙烷和氫氧化鈉的用量比,偏二氯乙烯與混酸的用量比等對于反應(yīng)產(chǎn)物的影響,得到了優(yōu)化的反應(yīng)條件為:1)反應(yīng)溫度60-70℃,反應(yīng)時間1.5-2.0 h,n(三氯乙烷):n(氫氧化鈉)=1:1.15,此時偏二氯乙烯的收率99%。

　　浩瀚色譜（山東）應(yīng)用技術(shù)開發(fā)有限公司研發(fā)氫火焰離子化檢測器(FID)測定烯啶蟲胺合成中間體中1,1-二氯-2-硝基乙烯含量的氣相色譜方法。此方法靈敏、準(zhǔn)確,可以應(yīng)用于實際樣品1,1-二氯-2硝基乙烯的測定。

　　名稱:毛細管柱

　　固定相:專用

　　規(guī)格:30m*0.32mm*0.5um

　　型號:HH-CLNO2

　　溫度:240°C

　　Using 1,1,2-trichloroethane as the raw material, it reacts with sodium hydroxide solution to generate vinylidene chloride. Under the action of mixed acids (nitric acid and hydrochloric acid), vinylidene chloride generates 1,1-dichloro-2-nitroethylene. The effects of temperature, time, the ratio of trichloroethane to sodium hydroxide, and the ratio of vinylidene chloride to mixed acids on the reaction products were investigated. The optimized reaction conditions were as follows: 1) reaction temperature 60-70 ℃, reaction time 1.5-2.0 hours, N (trichloroethane): n (sodium hydroxide)=1:1.15, at which point the yield of vinylidene chloride is 99%.

　　Haohan Chromatography (Shandong) Application Technology Development Co., Ltd. has developed a gas chromatography method for determining the content of 1,1-dichloro-2-nitroethylene in the intermediate of the synthesis of imidacloprid using a hydrogen flame ionization detector (FID). This method is sensitive and accurate, and can be applied to the determination of 1,1-dichloro-2-nitroethylene in actual samples.

　　Name: Capillary Column

　　Fixed phase: dedicated

　　Specification: 30m * 0.32mm * 0.5um

　　Model: HH-CLNO2

　　Temperature: 240 ° C