以莰烯和烯丙醇为原料,研究了烯丙基异冰片基醚的绿色合成工艺,探讨了催化剂种类及用量、反应温度、反应时间,以及烯丙醇与莰烯物质的量之比对莰烯醚化反应选择性及烯丙基异冰片基醚产物得率的影响。采用正交试验方法确定了烯丙基异冰片基醚的最适工艺条件:A-15型阳离子树脂为催化剂,催化剂用量为烯丙醇和莰烯原料总质量的5%,烯丙醇与莰烯物质的量之比为1.5∶1,反应温度75℃,反应时间7 h。在此条件下工业莰烯转化率为85.5%,反应选择性为97.5%,烯丙基异冰片基醚得率为83.4%。最后采用GC-MS、IR等分析技术对合成所得产物的结构进行了分析测定。
Green synthetic method of allyl isobornyl ether was investigated by using camphene and allyl alcohol as the raw materials in this paper.Influence of catalysts and their usages,reaction temperature,reaction time,and the molar ratio of allyl alcohol to camphene on the selectivity of etherification and the yield of allyl isobornyl ether were examined,and the optimum synthesis conditions were determined based on the orthogonal test results as follows: A-15 resin was used as the catalyst for etherification,and the amount of A-15 cationic exchange resin was 5 %(based on the total weight of camphene and allyl alcohol);molar ratio of allyl alcohol to camphene was 1.5∶1;reaction temperature and reaction time were 75 ℃ and 7 h,respectively.The conversion ratio of camphene and the reaction selectivity reached 85.5 % and 97.5 % respectively,and the yield of allyl isobornyl ether also reached 83.4 %.The structure of allyl isobornyl ether was identified by GC-MS and IR spectra.