紫胶皂化废液中回收紫胶桐酸工艺研究  

The Process of Recovering Aleuritic Acid in Lac Saponification Waste Liquid

作　　者：王世贤 唐保山 张弘[1] 马金菊 刘兰香 徐涓 WANG Shixian;TANG Baoshan;ZHANG Hong;MA Jinju;LIU Lanxiang;XU Juan(Institute of Highland Forest Science,Chinese Academy of Forestry,Research Center of Engineering and Technology on Characteristic Forest Resources,Key Laboratory of Breeding and Utilization of Resource Insects,National Forestry and Grassland Administration,Kunming 650233,China;College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,China)

机构地区：[1]中国林业科学研究院高原林业研究所,国家林业和草原局特色森林资源工程技术研究中心,国家林业和草原局资源昆虫培育与利用重点实验室,云南昆明650233 [2]南京林业大学化学工程学院,江苏南京210037

出　　处：《林产化学与工业》2023年第5期56-62,共7页Chemistry and Industry of Forest Products

基　　金：中国林科院中央级公益性科研院所基本科研业务费专项资金(CAFYBB2020SY029)。

摘　　要：为提高紫胶桐酸得率,以工厂制备紫胶桐酸所残留的紫胶皂化废液为原料,通过构型转化法经盐析、酸析、脱色、重结晶等步骤回收紫胶桐酸,通过单因素试验优化紫胶桐酸构型转化工艺,采用核磁、质谱、红外、热重对制备的紫胶桐酸结构进行分析,采用差示扫描量热、高效液相色谱C18柱拆分法等表征方法对制备的紫胶桐酸进行构型分析。研究结果表明:通过构型转化法回收紫胶桐酸可提高紫胶桐酸得率,确定了最佳制备条件为原料和浓盐酸的料液比3∶5(g∶mL)、反应温度100℃、反应时间7 h,活性白土用量为紫胶桐酸粗品质量的10%,活性白土脱色及使用20%乙醇溶液重结晶各2次后,所制备的紫胶桐酸得率为3.78%±0.5%,纯度为80.65%±0.41%。产物结构及构型分析结果表明:所制备的产物为赤式紫胶桐酸。该方法制备的紫胶桐酸来自废弃物,且精制后杂质较少,从而可有效提高紫胶桐酸得率。In order to improve the yield of aleuritic acid,the lac saponification waste liquid left in the preparation of aleuritic acid by the factory was used as raw material to recover aleuritic acid by configuration conversion method through salting out,acid analysis,decolorization,recrystallization and other steps.The configuration conversion process of aleuritic acid was optimized by single factor experiment,and the structure of aleuritic acid was analyzed by nuclear magnetic resonance,mass spectrometry,infrared and thermogravimetric analysis.The configuration analysis of aleuritic acid was carried out by differential scanning calorimetry and C18 column resolution by high performance liquid chromatography.The results showed that the recovery of aleuritic acid by configuration conversion method could improve the yield of aleuritic acid.The optimal preparation conditions were determined as the ratio of solid to liquid of raw material and concentrated hydrochloric acid of 3∶5(g∶mL),reaction temperature of 100℃and reaction time of 7 h,and the amount of active clay was 10%of the quality of the crude aleuritic acid.After decolorization and recrystallization with 20%ethanol solution for two times,the yield and purity of aleuritic acid were 3.78%±0.5%and 80.65%±0.41%respectively.The results of structure and configuration analysis of the product showed that the product prepared by this method was erythron aleuritic acid.The eleostearic acid prepared by this method came from waste and had fewer impurities after refining,so it could effectively improve the yield of aleuritic acid.

关 键 词：紫胶桐酸 构型转化 苏式构型 赤式构型 

分 类 号：TQ35[化学工程]