摘要
针对鞣花酸在实际生产过程中耗时长、纯度低等问题,以单宁酸为基质采用液气射流氧化法制备鞣花酸,考察了金属离子、单宁酸质量浓度、反应温度和反应时间对鞣花酸得率及纯度的影响。进一步探究了溶剂法、结晶法、碱溶酸沉法、反溶剂法对鞣花酸纯度的影响,并通过HPLC、FTIR、UV-Vis光谱和TG对鞣花酸高纯样进行表征。得到液气射流氧化的较优工艺条件为:质量浓度25 g/L单宁酸溶液中引入金属离子Na^(+)(即NaOH)调节反应液pH至8.5,反应温度20℃,反应时间6h。该条件制备的鞣花酸经碱溶酸沉后收率为46.72%、纯度84.55%;采用甲醇溶剂洗涤法在料液比1∶200(g∶m L)、65℃下处理1h,鞣花酸的纯度达98.13%,回收率约为75.03%,提高了鞣花酸的热稳定性。液气射流氧化法与溶剂洗涤法相结合,大幅缩短制备鞣花酸的反应时间并明显提高其纯度,有望在工业生产中提高鞣花酸的生产效率并拓宽其在医药和化妆品领域的应用。
In order to solve the problems of time consuming and low purity in practical production of ellagic acid, liquid-gas jet oxidation technology was used to prepare ellagic acid from tannic acid. The effects of metal ions, tannic acid mass concentration, reaction temperature, and reaction time on yield and purity of ellagic acid were investigated. The effects of solvent method, crystallization method, alkali-soluble acid precipitation method and antisolvent method on purity of ellagic acid were further explored. The high purity sample was characterized by HPLC, FTIR, UV-Vis spectra and TG. The results indicated that the optimum process conditions for the preparation of ellagic acid were obtained as follows: mass concentration of tannic acid solution 25 g/L, pH of tannic acid solution to 8.5 adjusted by NaOH solution, reaction time 6 h, temperature 20 ℃. Under the above-mentioned conditions, the yield and purity of ellagic acid after alkali-soluble acid precipitation were 46.72% and 84.55%. The methanol solvent washing method was used for purifying under the conditions of solid-liquid ratio 1∶200(g∶m L), temperature 65 ℃ and treatment time 1 h, the purity of ellagic acid reached 98.13%, and the recovery rate was about 75.03%. And the thermal stability of ellagic acid was improved after purification by methanol solvent washing. The combination of liquid-gas jet oxidation method and solvent washing method could remarkably shorten the reaction time and improve the purity of ellagic acid, which is expected to improve the production efficiency of ellagic acid in industrial production and broaden its application in the field of medicine and cosmetics.
作者
徐涓
张弘
李坤
李凯
刘义稳
张雯雯
XU Juan;ZHANG Hong;LI Kun;LI Kai;LIU Yiwen;ZHANG Wenwen(Research Institute of Resources Insects,Chinese Academy of Forestry,Research Center of Engineering and Technology of Characteristic Forest Resources,National Forestry and Grassland Administration,Kunming 650233,Yunnan,China;Research Center for Efficient Cultivation and Deep Processing of Chinese Gallnut,National Forestry and Grassland Administration,Wufeng Chicheng Biotechnology Co.,Ltd.,Yichang 443413,Hubei,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2021年第5期994-1001,1037,共9页
Fine Chemicals
基金
国家重点研发计划资助项目(2018YFD0600404)。
关键词
鞣花酸
单宁酸
氧化
射流
溶剂洗涤
分离提纯技术
ellagic acid
tannic acid
oxidation
jet
solvent washing
separation and purification technology
作者简介
徐涓(1989-),女,助理研究员;联系人:张弘(1963-),男,研究员,E-mail:kmzhhong@163.com。
