摘要
硝基甲烷与25%氢氧化钠溶液同时滴加入甲醛溶液中反应,然后滴加溴反应得到溴硝醇;通过正交实验得出的优化条件为:烷羟基化反应中,n(硝基甲烷)∶n(甲醛)=1∶2.2,反应温度45℃,反应时间1.5 h,n(硝基甲烷)∶n(氢氧化钠)=1∶0.8;溴化反应中,n(硝基甲烷)∶n(溴)=1∶1,反应温度20℃,反应时间1.5 h,在此优化条件下收率达90.5%;产品用红外光谱和高效液相色谱进行分析确认,产品含量为99%。
In the process for the preparation of 2-bromo-2-nitro-1,3-propanediol （bronopol） ,nitromethane is firstly reacted with formaldehyde and alkali metal hydroxide and the reaction mixture obtained in this way is subsequently reacted with bromine. Based on orthogonal experiment, the optimum conditions of the reaction were determined. Hydroxyalkylation reaction ： the mole ratio of nitromethane to formaldehyde is 1 ：2.2 ,reaction temperature is 45℃ and time is 1.5 h. The mole ratio of nitromethane to sodium hydroxide is 1：0.8. Brominating reaction： the mole ratio of nitromethane to bromine is 1：1 ,reaction temperature is 20℃ and time is 1.5 h. The yield is 90.5% under this condition. The product was analyzed and confirmed by IR spectrum and HPLC, the mass fraction of that is 99%.
出处
《应用化工》
CAS
CSCD
2006年第11期841-843,共3页
Applied Chemical Industry
关键词
溴硝醇
抗菌剂
合成
正交
优化条件
2-bromo-2-nitro-1,3-propanediol （bronopol）
preservative
synthesis
orthogonal experiment
optimum conditions
