柠檬腈的合成工艺研究  

The Optimization of Synthesis Process of Geranyl Nitrile

作　　者：王九龙 司红燕 陈尚钘[1] 饶小平 王宗德[1] 廖圣良[1] WANG Jiulong;SI Hongyan;CHEN Shangxing;RAO Xiaoping;WANG Zongde;LIAO Shengliang(College of Forestry,Jiangxi Agricultural University/East China Woody Fragrance and Flavor Engineering Research Center of National Forestry and Grassland Administration,Nanchang 330045,China;College of Chemical Engineering,Huaqiao University,Xiamen 361021,China)

机构地区：[1]江西农业大学林学院/国家林业草原木本香料(华东)工程技术研究中心,江西南昌330045 [2]华侨大学化工学院,福建厦门361021

出　　处：《林产化学与工业》2022年第6期77-83,共7页Chemistry and Industry of Forest Products

基　　金：江西省主要学科学术和技术带头人培养计划-青年人才项目(20204BCJL23045);江西省科学技术厅重大科技研发专项(20203ABC28W016);江西省研究生创新专项资金项目(YC2021-S364)。

摘　　要：对柠檬醛催化氨氧化法制备柠檬腈的工艺进行优化,探讨了氨水(NH_(3)·H_(2)O)用量、过氧化氢(H_(2)O_(2))用量、反应时间、反应温度、催化剂的类型和用量以及溶剂的类型等因素对柠檬醛转化率和柠檬腈产率的影响。通过单因素试验和正交试验优化得到柠檬腈的最佳合成工艺条件:柠檬醛35 mmol,n(柠檬醛)∶n(NH_(3)·H_(2)O)∶n(H2O2)∶n(CuCl)=1∶2.7∶5.5∶0.045,H_(2)O_(2)为氧化剂,CuCl为催化剂,36 mL异丙醇为溶剂,反应时间为5 h,反应温度为10~15℃。在该条件下,柠檬醛的平均转化率可达97.50%,柠檬腈的平均产率可达94.59%。对工艺条件分别放大2、3和5倍进行试验,柠檬醛的转化率分别为95.75%、95.05%和95.00%,柠檬腈的产率分别为92.88%、92.20%和92.15%。The synthesis process of geranyl nitrile from citral by catalytic ammoxidation was optimized.The factors affecting the conversion rate of citral and the yield of geranyl nitrile,including ammonia(NH_(3)·H_(2)O)dosage,hydrogen peroxide(H_(2)O_(2))dosage,reaction time,reaction temperature,the type and dosage of catalyst,and solvent type were investigated.Through univariate and onthogonal experiments,the optimal synthesis conditions for geranyl nitrile was citral 35 mmol,n(citral)∶n(NH_(3)·H_(2)O)∶n(H_(2)O_(2))∶n(CuCl)=1∶2.7∶5.5∶0.045,H_(2)O_(2) as oxidant,CuCl as catalyst,36 mL isopropanol as solvent,and the reaction time of 5 h,the reaction temperature of 10-15℃.At these synthesis conditions,the conversion ratio of citral was 97.50% and the yield of geranyl nitrile was 94.59%.When the conditions were amplified by 2,3 and 5 times,the conversion rates of citral were 95.75%,95.05% and 95.00%,and the yields of geranyl nitrile were 92.88%,92.20% and 92.15%,respectively.

关 键 词：柠檬醛 柠檬腈 氨化氧化 工艺优化 

分 类 号：TQ35[化学工程]