一种由2-辛烯制备正壬醇的工艺  

Preparation of N-Nonanol by 2-Octene

作　　者：曾天宇 杨海涛[1] 舒畅[2] 张志鹏[2] 奚强[2] 

机构地区：[1]武汉工程大学化工与制药学院,湖北武汉430074 [2]武汉工程大学化学与环境工程学院,湖北武汉430074

出　　处：《武汉工程大学学报》2016年第2期133-138,共6页Journal of Wuhan Institute of Technology

摘　　要：以2-辛烯及合成气为原料,甲苯为溶剂,乙酰丙酮二羰基铑与三齿膦配体形成的络合物为催化剂,经氢甲酰化反应合成了中间产物正壬醛;正壬醛经兰尼镍氢化还原制得正壬醇.确定了催化剂的用量、反应温度和反应压力等的最佳工艺条件.结果表明:对于氢甲酰化反应,当底物质量分数为30%,催化剂(以铑计)用量为底物质量的0.2%,乙酰丙酮二羰基铑、三齿膦配体摩尔投料比为1∶4,合成气充入压力为1 MPa,反应温度为120℃时,2-辛烯转化率可达80%,产物中正壬醛比例可占98.3%;加氢还原反应中,催化剂的用量为底物质量的3.0%,氢气压力为4 MPa,120℃反应3 h,正壬醛转化率可达99.8%.目标产物经核磁共振氢谱、碳谱进行了表征.N-nonanol was synthesized by two reactions of hydroformylation and hydrogenation,using 2-octene as the raw materials. The intermediate product N-nonanal was prepared with hydroformylation using 2-octene and syngas as starting materials,toluene as solvent and the complex of dicarbonyl（2,4-pentanedionato）rhodium with tridentate phsphorodiamidite ligand as catalyst. N-nonanal was reduced by Raney-Ni to get the final product N-nonanol. The effects of the amount of catalyst,reaction temperature and reaction pressure on the optimumreaction conditions were explored. In hydroformylation reaction,the conversion ratio of 2-octene is up to 80% and the ration of N-nonanal is 98. 3% at the concentration of substrate of 30%,mass ratio of catalyst（as rhodium）to substrate of 0. 2%,molar ratio of dicarbonyl（2,4-pentanedionato）rhodium to tridentate phsphorodiamidite ligand of 1∶4,syngas pressure of 1MPa and reaction temperature of 120 ℃;In hydrogenation reaction,the conversion ratio of N-nonanal is 99. 8% at the mass ratio of catalyst to N-nonanal of 3.0%,hydrogen pressure of 4 Mpa,reaction temperature of 120 ℃ and reaction time of 3 h. The final product was characterized by nuclear magnetic resonance hydrogen spectrum and nuclear magnetic resonance carbon spectrum.

关 键 词：2-辛烯 合成气 正壬醛 正壬醇 

分 类 号：O623.5[理学—有机化学]