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• 工艺技术 •    下一篇

正交实验优化紫胶色酸酯的制备工艺

刘兰香,普真琪,郑华,徐涓,李坤,张弘   

  1. 中国林业科学研究院资源昆虫研究所
  • 收稿日期:2016-04-29 修回日期:2016-09-02 出版日期:2016-12-25 发布日期:2016-11-18
  • 通讯作者: 张弘 E-mail:kmzhhong@163.com
  • 基金资助:
    国家高技术研究发展计划(863计划)项目

Optimizing preparation technology of lac dye ester on orthogonal experiment

  • Received:2016-04-29 Revised:2016-09-02 Online:2016-12-25 Published:2016-11-18
  • Contact: Zhang Hong E-mail:kmzhhong@163.com

摘要: 紫胶色酸是附加值较高的紫胶综合利用产品之一,通过化学方法改善其溶解性,可使紫胶色酸得到高效利用。本文对紫胶色酸分子中的羧基先进行甲酯化,然后再用醋酸酐进行乙酰化,最后制备得到了紫胶色酸酯。通过单因素及正交实验确定了紫胶色酸酯的制备工艺条件为:紫胶色酸1.0g,甲醇20ml,对甲苯磺酸用量为紫胶色酸质量的5.0%,甲酯化时间为36h,醋酸酐用量为1.0 ml,此条件酯化率为81.3%,标准偏差为0.67。通过FT-IR,UV-Vis表征,表明紫胶色酸酯分子中有酯基及烷基;通过DSC及TG测定,表明紫胶色酸酯的熔融温度为68℃,温度高于198℃时出现热分解。紫胶色酸酯的色价为121,可溶于大多数有机溶剂,脂溶性增强,其在菜籽油的溶解度0.340g/L,保存28d后,油样呈红色,且澄清无沉淀,保存率达96.2%,说明其稳定性良好,对油脂类物质染色效果好,具有潜在的应用价值和前景。

关键词: 紫胶色酸,紫胶色酸酯,正交实验,脂溶性

Abstract: Laccaic acid is one of the higher value-added utilization of shellac products, it will be used efficiently if the solubility was improved. Laccaic acid reacted with methanol and then with acetic anhydride, and finally laccaic acid ester had been preparation by two-step reactions. Basing on the results of the single factor experiments, optimizing preparation technology of lac dye ester on orthogonal experiment had been applied. Under the conditions: laccaic acid 1.0g, methanol 20ml, p-toluenesulfonic acid dosage of laccaic acid was 5.0%, the reaction time 36h, acetic anhydride 1.0ml, the esterification rate was 81.3%, the SD was 0.6. The structure of the laccaic acid ester was characterized by FT-IR and UV-Vis, its melt temperature was 68℃, there was a thermal decomposition when temperature higher than 198℃by DSC and TG. Color value of laccaic acid ester was 121, it soluble in most organic solvents, and its solubility 0.340g/L in rapeseed oil, the oil sample was red, no precipitation and clarification, preserve rate was 96.2% within 28d. Laccaic acid ester has good stability for oil substances dyeing effect, has potential application and prospect.

Key words: Laccaic acid, laccaic acid ester, orthogonal experiment

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