摘要
在相转移助剂苄基三乙基氯化铵(BTEAC)存在下,以氢型丝光沸石(HM)为催化剂,原料α-蒎烯经开环、重排及水合反应一步法合成了α-松油醇。研究了各种因素对α-蒎烯转化率及α-松油醇收率的影响,采用5因素4水平L16(45)进行了正交实验,得出最佳的工艺条件:反应温度80℃,w(BTEAC)=15%,m(HM)∶m(α-蒎烯)=0.6,反应时间40h,m(乙酸乙酯)∶m(α-蒎烯)=0.9。在此条件下,α-蒎烯转化率为75.2%,α-松油醇收率为42.0%。用气相色谱-质谱联用仪对反应产物进行分析,共鉴定出14种化合物,主要成分为α-松油醇、α-蒎烯、柠檬烯、桉叶油素、异松油烯、龙脑等。实验得到的α-松油醇具有光学活性,旋光值[α]=+61°,同时香气纯正,可用于制作香料。
α - Terpineol was one - steply synthesized from α - pinene on hydrogen mordenite （HM） as catalyst. The reactions were carried out in presence of benzyl triethyl ammonium chloride（ BTEAC）, and through ring- opening ,rearrangement and hydration successively. The factors affecting product yield and conversion of α - pinene were investigated by means of orthogonal design. The optimal reaction conditions obtained were as follows： reaction temperature 80 ℃, w （ BTEAC ） 15%, m （ HM ） ： m （ α - pinene） = 0.6, reaction time 40 h, m （ ethyl acetate） ： m （ α - pinene ） = 0.9. Under above conditions, conversion of a - pinene and yield of α - terpineol could reach 75.2% and 42. 0%, respectively. The reaction products were characterized by means of GC - MS. 14 components were identified. The main components were α - terpineol, α - pinene, limonene, eucalyptol, 1- methyl - 4 - （ 1 - methylethyl） - 1, 4 - cyclohexadiene and bomeol. A photoactive α - terpineol was obtained, of which optic rotation was ＋ 61°. The product could be used in preparation of perfume because of its pure fragrance.
出处
《石油化工》
EI
CAS
CSCD
北大核心
2006年第1期60-64,共5页
Petrochemical Technology
