β-水芹烯异构制备α-松油烯的研究
Preparation of α-Terpinene by Isomerization of β-Phellandrene
王婧 1陈玉湘 1赵振东 1李海兵 2冯盛2
作者信息
- 1. 中国林业科学研究院林产化学工业研究所;江苏省生物质能源与材料重点实验室;国家林业和草原局林产化学工程重点实验室;林木生物质低碳高效利用国家工程研究中心;江苏省林业资源高效加工利用协同创新中心,江苏南京 210042
- 2. 普洱市思茅区森盛林化有限责任公司,云南普洱 665099
- 折叠
摘要
对β-水芹烯酸催化异构制备α-松油烯的工艺进行了研究,结果表明:三甲基溴硅烷(TMSBr)因酸性适中对β-水芹烯表现出良好催化效果,但其对α-蒎烯、β-蒎烯、3-蒈烯、苧烯和异松油烯等单萜烯催化效果不佳;助剂30％(质量分数)H2O2因其所含的水可使TMSBr转化为H+从而催化异构反应进行,并通过对H+的扩散作用减少副反应发生,此外H2O2自身酸性对反应起到辅助催化效应,这3方面特性极大提升了反应效率.β-水芹烯异构制备α-松油烯的较佳工艺条件为:β-水芹烯0.1 mol、TMSBr 0.002 mol、30％H2O20.1 mol、反应温度100℃、反应时间6 h,此条件下原料转化率为88.4％,产物选择性为94.0％.
Abstract
Acid-catalyzed isomerization of β-phellandrene for the preparation of α-terpinene and relative reaction process were investigated.The results indicated that trimethylsilyl bromide(TMSBr)showed excellent catalytic activity on the isomerizationβ-phellandrene owing to its moderate acidity.However,its catalytic effects on other monoterpenes such as α-pinene,β-pinene,3-carene,limonene and terpinene were limited.The auxiliary agent of 30％(mass fraction)H2O2 greatly improved the reaction efficiency owing to its three characteristics including converting TMSBr to H+to catalyze the isomerization reaction due to the existence of water,dispersing H+to reduce the occurrence of side reactions,and assisting the reaction by its own acidity.The optimal conditions for the preparation of α-terpinene from the isomerization of β-phellandrene were β-phellandrene of 0.1 mol,TMSBr of 0.002 mol,30％H2O2 of 0.1 mol,temperature of 100 ℃,time of 6 h,and the raw material conversion and product selectivity were 88.4％and 94.0％,respectively.
关键词
β-水芹烯/α-松油烯/展松松节油/催化异构/三甲基溴硅烷Key words
β-phellandrene/α-terpinene/turpentine from Pinus patula/catalytic isomerization/trimethylsilyl bromide引用本文复制引用
基金项目
中央级公益性科研院所基本科研业务费专项中国林科院项目(CAFYBB2022MA003)
江苏省生物质能源与材料重点实验室项目(JSBEM-S-202205)
出版年
2024
国家科技期刊平台
NSTL
万方数据