左旋海松酸的分离及其理化数据测试  

Isolation and Physical-chemical Data Testing of Levopimaric Acid

作　　者：齐志文 王成章[1] 蒋建新[2] QI Zhiwen;WANG Chengzhang;JIANG Jianxin(Institute of Chemical Industry of Forest Products,CAF/National Engineering Lab.for Biomass Chemical Utilization/Key Lab.of Chemical Engineering of Forest Products,National Forestry and Grassland Administration/Key Lab.of Biomass Energy and Material,Jiangsu Province,Nanjing 210042,China;College of Materials Science and Technology,Beijing Forestry University,Beijing 100083,China)

机构地区：[1]中国林业科学研究院林产化学工业研究所/生物质化学利用国家工程实验室/国家林业和草原局林产化学工程重点实验室/江苏省生物质能源与材料重点实验室,江苏南京210042 [2]北京林业大学材料科学与技术学院,北京100083

出　　处：《生物质化学工程》2019年第6期45-50,共6页Biomass Chemical Engineering

基　　金：国家自然科学基金资助项目(31570564);江苏省生物质能源与材料重点实验室基本科研业务费项目(JSBEM-S-201509)

摘　　要：采用胺化法从松脂中分离左旋海松酸,然后利用超声波辅助左旋海松酸粗品重结晶进行纯化,通过单因素和正交试验优化左旋海松酸分离的工艺条件,得到的最佳工艺条件为:无水乙醇用量20mL(1 g左旋海松酸),结晶温度0℃,超声波频率为53 kHz,重结晶次数为2次,此条件下得到的左旋海松酸纯度达97%。超声波辅助左旋海松酸重结晶,大幅度缩短了晶体成核时间,5~6 h可得到晶型细小均匀分散的长方型片状透明晶体。通过红外光谱(FT-IR)、核磁共振(1H NMR,13C NMR)、气相色谱-质谱联用(GC-MS)表征了纯化后左旋海松酸的分子结构,依据氧弹量热法、TG-DSC法和基团贡献法分析得到左旋海松酸的标准摩尔生成焓(Δf H m^θ)-700.23 kJ/mol和熔化焓94.99 kJ/mol。Levopimaric acid was isolated from turpentine by amination method and ultrasonic assisted recrystallization,and its physical and chemical data were experimental measured.By single factor and orthogonal test,the optimum isolation conditions of levopimaric acid were as follows:ethanol concentration 100%,crystallization temperature 0℃,volume ratio of ethanol used for crystallization 20∶1(mL∶g),ultrasonic frequency was 53 kHz,2 recrystallization times;purity of levopimaric acid was 97%.Ultrasonic assisted crystallization was used to shorten the nucleation time of the levopimaric acid crystal,and a fine-uniform rectangular transparent crystal was obtained after 5-6 h.The molecular structure of levopimaric acid was characterized by FT-IR,NMR(1 H NMR,13 C NMR)and GC-MS.According to the oxygen elastic calorimeter,TG-DSC and group contribution,the standard molar enthalpy(Δf H m)and melting enthalpy of levopimaric acid were-700.23 and 94.99 kJ/mol,respectively.

关 键 词：左旋海松酸 分离 超声波 焓变 

分 类 号：TQ35[化学工程]