Solid acid catalyst for the esterification of high free fatty acids of Zanthoxylum bungeanum seed oil

doi:10.16085/j.issn.1000-6613.2016-2116

Abstract

Abstract: A solid acid catalyst was synthesized by directly carbonization and sulfonation with glycerol.The solid acid catalyst was characterized with FTIR,SEM,XPS,XRD and Boehm titration methods,and was firstly employed as the catalyst for the esterification of Zanthoxylum bungeanum seed oil (ZSO).The effects of different reaction factors were investigated and the optimum conditions for the esterification reaction were obtained by the orthogonal experiment.The optimum conditions were:methanol-to-oil molar ratio,40:1;catalyst amount,10.0%;reaction temperature,75℃;reaction time,3.5h.The acid value of ZSO was reduced from 73.75mgKOH/g to 1.63mgKOH/g,which satisfied the next process of alkali-catalyzed transesterification for biodiesel production.The catalyst possesses desired stability and activity after being used for six cycles without any recovery treatments.

Key words: Zanthoxylum bungeanum seed oil, high free fatty acids, esterification, carbon-based catalyst

摘要： 以甘油为碳源，通过直接炭化-磺化制备了炭基固体酸催化剂。采用傅里叶转换红外光谱（FTIR）、扫描电子显微镜（SEM）、X射线光电子能谱分析（XPS）、X射线衍射（XRD）以及Boehm滴定法等方法对催化剂进行了表征，并将其首次应用于花椒籽油的酯化降酸反应。研究了反应条件对酯化反应的影响，并通过正交试验确定了最佳工艺条件：醇油比为40：1，催化剂用量为10.0%，反应温度为75℃，反应3.5h，花椒籽油的酸值可以由最初的73.75mKOH/g降到1.63mgKOH/g，符合后续制备生物柴油的碱催化酯交换反应要求（ < 2mg KOH/g）；并且该催化剂具有较好的重复利用性。

关键词: 花椒籽油, 高酸值, 酯化反应, 炭基固体酸

CLC Number:

O643.3

WANG Weitao, LU Ping, MA Yangmin, LI Na, YANG Xiufang. Solid acid catalyst for the esterification of high free fatty acids of Zanthoxylum bungeanum seed oil[J]. Chemical Industry and Engineering Progress, 2017, 36(07): 2504-2510.

王伟涛, 卢萍, 马养民, 李娜, 杨秀芳. 固体酸催化高酸值花椒籽油酯化降酸反应[J]. 化工进展, 2017, 36(07): 2504-2510.

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