机构地区: 青岛科技大学
出 处: 《精细石油化工进展》 2010年第5期9-12,共4页
摘 要: 采用先羟甲基化后溴化反应的方法合成布罗波尔,通过正交试验考察了原料配比、反应时间、反应温度对反应结果的影响,得到的较佳反应条件如下:n(硝基甲烷)∶n(氢氧化钠)∶n(甲醛)∶n(溴素)=1∶1∶2∶1,羟甲基化反应温度20℃,反应时间1.5h,溴化反应温度15℃。考察了布罗波尔在单一及复配溶剂中的溶解度和重结晶试验,确定的较佳复配溶剂比m(乙酸乙酯)∶m(氯仿)=1∶1。在较佳反应条件下,反应过程收率可达90%,重结晶单程收率可达83%,得到的产品纯度在99%以上。 Bronopol was synthesized by hydroxymethylation and bromination. The effects of n(nitromethane) : n(NaOH) :n(formaldehyde) :n( bromine), reaction temperature and reaction time on reaction result were ex- amined by orthogonal experiments. The optimum reaction conditions were ane) : n (NaOH) : n (formaldehyde) : n(bromine) = 1 : 1:2 : 1, hydroxymethy methylation time 1.5 hours, bromination temperature 15 ~C. The solubility obtained as follows : n ( nitrometh- lation temperature 20 ~C, hydroxy- and recrystallization of bronopol in different solvents were studied. The suitable solvent was the mixture of ethyl acetate and chloroform with the mass ratio of 1:1. Under the above conditions, the yield of product was up to 90%. Recrystallization yield and purity of product were 83% and 99% respectively.
领 域: [化学工程]