摘要
针对目前常压相转移催化法合成N,N-二乙基苯胺工艺中催化剂无法实现分离的问题,开展了非均相固体相转移催化剂催化合成N,N-二乙基苯胺工艺研究。以苯胺、溴乙烷为原料,氢氧化钠作为缚酸剂,在磷钼钒杂多酸季铵盐催化剂催化合成了N,N-二乙基苯胺,实现了固体非均相相转移催化剂的工艺路线,及催化剂的快速分离。利用单因素试验法对N,N-二乙基苯胺合成工艺进行了优化,得到最佳工艺条件为:反应温度为54℃,n(苯胺)∶n(溴乙烷)=1∶2.4,催化剂用量分别为1.6g,反应时间为5.5h,氢氧化钠用量为0.55 mol,氢氧化钠浓度为35%,收率达到82.8%。
In view of the problem that the catalyst cannot be separated in present atmospheric phase transfer catalytic synthesis of N,N-diethyl aniline process, heterogeneous solid phase transfer catalytic synthesis process of N,N-diethyl aniline was researched. Taking aniline and bromine ethane as raw materials, sodium hydroxide as acid binding agent, phosphorus vanadium molybdenum heteropoly acid quaternary ammonium salt as catalyst, N,N-diethyl aniline was synthesized to realize the fast separation of catalyst. The single factor test method was used to optimize the synthesis process of N,N-diethyl aniline. The optimum process conditions were determined as follows: the reaction temperature 54℃,n(aniline):n(bromoethane)=1:2.4, the catalyst dosage 1.6 g, the reaction time 5.5 h, sodium hydroxide dosage 0.55 mol, sodium hydroxide concentration 35%.Under above conditions, the yield reached 82.8%.
作者
范勇
赵军
FAN Yong;ZHAO Jun(College of Chemistry and Chemical Engineering,Yan'an University,Shaanxi Yan'an716000,China;College of Environmental Science and Engineering,Tongji University,Shanghai 200092,China)
出处
《当代化工》
CAS
2019年第11期2517-2520,共4页
Contemporary Chemical Industry
