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| 无催化酯化合成不饱和蜡酯及其分离纯化工艺 |
| Synthesis of unsaturated wax esters by non-catalytic esterification and its separation and purification |
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| DOI： |
| 中文关键词: 蜡酯 无催化 酯化 分离纯化 |
| 英文关键词:wax ester non-catalytic esterification separation and purification |
| 基金项目:国家自然科学基金项目（31772003） |
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| 中文摘要: |
| 不饱和蜡酯在食品、化妆品以及医药产品中有着广泛的用途。研究了无催化条件下，油酸与十六醇直接酯化合成不饱和蜡酯（油酸十六醇酯）的工艺条件。通过单因素试验得到最佳酯化合成工艺条件为反应温度180 ℃、反应时间8 h、酸醇摩尔比1.5∶ 1，此时十六醇转化率达到99.1%，蜡酯产率为98.1%。采用溶剂萃取法对蜡酯粗产品进行分离纯化，采用单因素试验对溶剂萃取工艺条件进行优化，得到最佳工艺条件为：以甲醇为萃取溶剂，萃取温度20 ℃，液料比4∶ 1，萃取时间0.5 h，萃取次数5次。在最佳分离纯化条件下，油酸十六醇酯得率为92.0%，纯度可达到98.7%，酸值（KOH）为2.7 mg/g，达到美国药典（酸值（KOH）为3 mg/g以下）的要求。 |
| 英文摘要: |
| Unsaturated wax esters are widely used in food, cosmetics and pharmaceutical products. The synthesis of unsaturated wax ester (cetyl oleate) by direct esterification of oleic acid and hexadecanol without catalysis was studied. The optimal synthesis conditions were obtained by single factor experiment as follows: reaction temperature 180 ℃, reaction time 8 h, molar ratio of oleic acid to hexadecanol 1.5∶ 1. Under these conditions, the conversion rate of hexadecanol reached 99.1% and the yield of the wax ester was 98.1%. The solvent extraction method was used to purify the crude wax ester products, and the extraction process was optimized by single factor experiment as follows: methanol used as the solvent, extraction temperature 20 ℃, ratio of methanol to crude products 4∶ 1, extraction time 0.5 h and extraction times 5. Under these conditions, the yield of cetyl oleate was 92.0%, the purity reached 98.7%, and the acid value was 2.7 mgKOH/g, which met the requirements of United States Pharmacopoeia with acid value below 3 mgKOH/g. |
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