摘要
以灭多威、S_(2)Cl_(2)为原料合成硫双威,采用吡啶兼作碱化剂和溶剂,灭多威溶解在吡啶中,反应在液相体系中进行,利于传质、传热并提高反应效果。利用正交实验得到最佳工艺条件为:反应温度30℃,时间6 h,原料灭多威、S_(2)Cl_(2)和吡啶的摩尔比为1:0.7:6.5,醇洗剂用量为500 g甲醇/mol灭多威。灭多威的转化率达92.5%,硫双威收率达89.6%,产品为白色粉末状、颜色一致、粒度分布均匀,含量大于97.8%,热分解率低于2.4%。硫双威合成过程无废水产生,吡啶及副产物吡啶盐酸盐采用碱化处理、共沸蒸馏回收,甲醇采用精馏回收。该工艺路线绿色、环保,可推广到工业生产中。
Thiodicarb was synthesised by using methomyl,disulfur dichloride.The pyridine was used as an alkalinising agent and solvent.The methomyl was dissolved in pyridine,so that the reactants were carried out in the liquid phase system,which was conducive to mass and heat transfer and improve the reaction effect.The optimum conditions for synthesis of thiodicarb were obtained by orthogonal experiment,the reaction temperature was 30℃,the molar ratio of methomyl,S2Cl2 and pyridine was 1:0.7:6.5,the alcohol lotion dosage was 500 g methanol/mol metocarb.The conversion rate of methomyl reaches 92.5%,and the yield rate of thiodicarb was more than 89.6%.The prepared product was white powder,the colour of each batch of products was consistent,the particle size was uniform,the content was greater than 97.8%,the thermal decomposition rate was less than 2.4%.There was no wastewater generated in the synthesis process of thiodicarb,phyline and by-product pyridine hydrochloride were recycled by alkalinisation,azeotropic distillation,and methanol was recycled by distillation.The process route was green and evironmentally friendly,and can be popularised into industrial production.
作者
罗永利
杨倩
党潇漫
孙若晴
杨荣华
Luo Yongli;Yang Qian;Dang Xiaoman;Sun Ruoqing;Yang Ronghua(College of Chemical and Pharmaceutical Engineering,Shandong First Medical University&Shandong Academy of Medical Sciences,Shandong,271000)
出处
《当代化工研究》
CAS
2024年第7期135-138,共4页
Modern Chemical Research
关键词
硫双威
灭多威
二氯化二硫
绿色合成
thiodicarb
methomyl
disulfur dichloride
green synthesis
