生漆制备漆酚缩醛及其加氢历程的研究  

The Preparation of Urushiol Acetal from Lacquer Sap and Its Hydrogenation Process Mechanism

作　　者：何源峰[1,2,3,4] 鲁黎[5] 王成章[1,2,3,4,6] 杨志斌[5] 周昊[1,2,3,4,6] 陈虹霞[1,2,3,4] 叶建中[1,2,3,4,6] 

机构地区：[1]中国林业科学研究院林产化学工业研究所 [2]生物质化学利用国家工程实验室 [3]国家林业局林产化学工程重点开放性实验室 [4]江苏省生物质能源与材料重点实验室,江苏南京210042 [5]湖北省林业科学研究院,湖北武汉430075 [6]中国林业科学研究院林业新技术研究所,北京100091

出　　处：《林产化学与工业》2014年第4期113-117,共5页Chemistry and Industry of Forest Products

基　　金：国际合作项目(S2012GR0138);国家林业局948技术引进项目(2012-04-05)

摘　　要：以毛坝生漆为原料,经过丙酮浸提得到漆酚,漆酚通过缩醛反应、硅胶柱分离、常压加氢等方式制备和分离了不同饱和程度的漆酚缩醛;分别应用红外光谱和核磁对漆酚缩醛产物进行表征,采用HPLC实时分析了三不饱和漆酚缩醛的加氢历程.结果表明：经过正相硅胶分离得到93.8％的高纯度三不饱和漆酚缩醛,通过HPLC色谱分析,三不饱和漆酚缩醛衍生物加氢的历程为：三不饱和在前90 min主要先转换为二不饱和和单不饱和,经过8h加氢反应二不饱和和单不饱和漆酚还原为纯度95.65％的饱和漆酚缩醛.红外光谱数据表明漆酚缩醛酚羟基的特征吸收3650～3100 cm-1消失,同时观察到醚的红外特征吸收1049 cm-1;1H NMR中δ 5.92为亚甲基醚的吸收.Urushiol acetal was prepared from the acetone extracted lacquer sap by acetalation which decreased the polarity of urushiol. Thus it is easy to be separated from dimmer and oglimer of urushiol. The tri-unsaturated urushiol were obtained through silica gel column. The rushiol aeetal products were analysed by IR and NMR. IR absorptanee at 3100 - 3650 cm^-1 indicates phenol to disappear while ether 1049 cm-l was found after acetalation. The absorption of 5.92 in 1H NMR represents methylene ether group in rushiol acetal. The tri-unsaturated urushiol aeetal was hydrogenised. Its hydrogenation process was detected by HPLC. It was found that tri-unsaturated urushiol acetal gradually became di-unsaturate and mono-unsaturate, and turned into saturate state after 8 h.

关 键 词：漆酚 缩醛反应 氢化历程 

分 类 号：TQ35[化学工程] Q946.91[生物学—植物学]