一步法合成松油醇的原料筛选和条件优化

Optimization of Raw Materials and Conditions for One-step Terpineol Synthesis

为挑选适合一步水合制备松油醇的松节油原料及优化松节油水合反应条件,通过钻孔法收集马尾松、湿地松和湿加杂交松共3种松脂后,采用水蒸气蒸馏得到3种松节油,以Amberlyst-15为催化剂催化3种松节油一步水合制备松油醇,通过气相色谱-质谱、气相色谱分析3种松节油组分、蒎烯的转化率和松油醇的得率;通过改变反应时间、反应温度、催化剂用量及投料比,探究较优的水合反应条件。结果显示:马尾松松节油是较优的制备松油醇的原料,在相同的催化条件下马尾松松节油水合反应中松油醇的产率最高;最优的反应条件为马尾松松节油和水的用量均为8.00 g,溶剂异丙醇用量为40.00 mL,催化剂Amberlyst-15的用量为0.80 g,催化反应温度为80℃,反应时间为6 h;在最优催化条件下,蒎烯的转化率为87.863%,松油醇的产率为36.571%,松油醇的选择性为48.027%。

In order to select turpentine raw materials suitable for one-step hydration to prepare terpineol and optimize turpentine hydration reaction conditions,which is expected to provide support for the high-value utilization of turpentine,three kinds of turpentine were collected from Pinus massoniana,P.elliottii and P.elliottii×P.caribaea by drilling method.Three kinds of turpentine were obtained by steam distillation.Terpineol was prepared by one-step hydration of three kinds of turpentine catalyzed by Amberlyst-15.The components of three kinds of turpentine,the conversion of pinene and the yield of terpineol were analyzed by gas chromatography-mass spectrometry and gas chromatography.Change the reaction time,reaction temperature,catalyst dosage and feed ratio to explore the better hydration reaction conditions.The results showed that P.massoniana turpentine was the best raw material for preparing terpineol,and the yield of terpineol was the highest in the hydration reaction under the same catalytic conditions.The optimal reaction conditions were as follows:the amount of turpentine and water was 8.00g,the amount of isopropanol was 40.00 mL,the amount of Amberlyst-15 was 0.80 g,the reaction temperature was 80℃,and the reaction time was 6 h.Under the optimal catalytic conditions,the conversion of pinene was 87.863%,the yield of terpineol was 36.571%,and the selectivity of terpineol was 48.027%.