四正丁基溴化铵的合成  

Study on Synthesis of Tetrabutyl Ammonium Bromide

作　　者：秦瑞霞 于世涛[1] QIN Rui-xia;YU Shi-tao(Qingdao University of Science and Technology, Shandong Qingdao 266042, Chin)

机构地区：[1]青岛科技大学,山东青岛266000

出　　处：《当代化工》2018年第4期696-698,702,共4页Contemporary Chemical Industry

基　　金：泰山学者建设工程专项经费资助项目;项目号:NOts201511033

摘　　要：以三正丁胺和1-溴丁烷为原料,在加压条件下一步合成目标产物四正丁基溴化铵。试验研究了溶剂种类和用量、原料物料比、反应温度、反应时间等因素对反应结果的影响。结果表明:在4 MPaN_2压力下,反应溶剂乙酸乙酯20 m L、洗涤溶剂质量比1.0:1.3的石油醚和1-溴丁烷的混合物、n(三正丁胺):n(1-溴丁烷)=1.0:1.1(三正丁胺18.54 g)、反应温度100 ℃、反应时间14 h。在该条件下,四正丁基溴化铵收率为83.93%,纯度为98.96%。采用~1H NMR、^(13)C NMR和FT-IR确定合成产物。Using tributylamine and 1-bromobutane as raw materials, tetrabutyl ammonium bromide was synthesized under pressure by one-step method. The effect of solvent type and dosage, reactant proportion, reaction temperature, reaction time on the reaction was investigated to determine the optimal synthesis conditions. The results showed that the conversion of n-butyl ammonium bromide reached 83.93% and the purity reached 98.96% under optimal synthesis conditions including initial pressure 4 MPa（N_2）, solvent ethyl acetate 20 m L,the mass ratio of 1-bromobutane to light petroleum 1.3：1.0, n（tributylamine） ： n（1-bromobutane） = 1.0 ： 1.1（tributylamine 18.54 g）, the reaction temperature 100 ℃, reaction time 14 h. At last, the product was characterized by ~1H NMR, ^（13） C NMR and FT-IR techniques.

关 键 词：四正丁基溴化铵 三正丁胺 1-溴丁烷 合成 

分 类 号：TQ016[化学工程]