摘要
通过硝基甲烷先成盐再溴化的方法合成了溴代硝基甲烷,合成最佳反应条件为:硝基甲烷、氢氧化钠与溴素的摩尔比为1∶1.1∶1.02,氢氧化钠的质量浓度为30%;成盐反应温度为-15℃^-10℃,成盐反应时间为15m in;溴化反应温度为-10℃^-5℃。优化条件下,收率可达93.7%,产品经红外色谱验证及气相色谱分析,百分含量为96.8%。
In the process for the preparation of bromonitromethane, nitromethane is reacted with salification and bromination method. The optimal reactive conditions were obtained as follows: ( 1 ) the molar ratio of nitromethane, sodium hydroxide and bromine was 1 : 1.1 : 1.02, ( 2 ) the mass concentration of sodium hydroxide is 30% , ( 3 ) the reaction temperature of the salification is between -15℃ and -10℃ and the time is 15rain, (4)the reaction temperature of the bromination is between - 10℃ and - 5℃ . The yield is 93.7% under this condition. The product was analyzed and confirmed by IR spectrum an GC ,the mass concentration is 96.8%.
出处
《盐业与化工》
CAS
北大核心
2007年第6期14-16,共3页
Jounral of Salt and Chemical Industry
关键词
溴代硝基甲烷
硝基甲烷
溴化
bromonitromethane
nitromethane
bromization