Page 140 - 《精细化工》2021年第5期

第 38 卷第 5 期 精 细 化 工 Vol.38, No.5
202 1 年 5 月 FINE CHEMICALS May 2021

催化与分离提纯技术
液气射流技术改进单宁酸氧化制备高纯度鞣花酸

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徐 涓 ，张 弘 ，李 坤 ，李 凯 ，刘义稳 ，张雯雯
（1. 中国林业科学研究院资源昆虫研究所，国家林业和草原局特色森林资源工程技术研究中心，云南 昆
明 650233；2. 五峰赤诚生物科技股份有限公司，国家林业和草原局五倍子高效培育与精深加工工程技术
研究中心，湖北 宜昌 443413）
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
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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 6 h。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∶mL)、65 ℃下处理 1 h，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。
关键词：鞣花酸；单宁酸；氧化；射流；溶剂洗涤；分离提纯技术
中图分类号：TS202.3；TQ463 文献标识码：A 文章编号：1003-5214 (2021) 05-0994-09

Improved tannic acid oxidation by liquid-gas jet technology for
preparation of high purity ellagic acid

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XU Juan , ZHANG Hong , LI Kun , LI Kai , LIU Yiwen , ZHANG Wenwen
（1. 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; 2. 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）
Abstract: 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∶mL), 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

收稿日期：2020-08-22; 定用日期：2020-11-20; DOI: 10.13550/j.jxhg.20200785
基金项目：国家重点研发计划资助项目（2018YFD0600404）
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。