HJCET  >> Vol. 2 No. 2 (April 2012)

    响应面分析法优化乙酸正辛酯制备工艺研究
    Optimization of Process Variables in the Synthesis of Octyl Acetate by Response Surface Methodology

  • 全文下载: PDF(426KB) HTML    PP.24-29   DOI: 10.12677/hjcet.2012.22006  
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作者:  

何燕斐,韩晓祥,周凌霄,陈青:浙江工商大学食品与生物工程学院;
杨菊红:浙江工商大学食品与生物工程学院,浙江医学高等专科学校基础部

关键词:
乙酸正辛酯离子液体响应面分析法
Octyl Acetate; Ionic Liquid; Response Surface Methodology

摘要:

采用响应面分析法优化酸性离子液体催化制备乙酸正辛酯的工艺条件。在单因素实验的基础上,选取反应时间、酸醇物质的量比、带水剂用量和催化剂用量4个因素进行Box–Behnken中心组合设计。实验结果表明,带水剂量与催化剂用量的相互作用和反应物物质的量比和离子液体剂量的相互作用最大;离子液体1-甲基-3-(丙基-3-磺酸基)咪唑硫酸氢盐([HSO3-pmim]HSO4)催化合成乙酸正辛酯的最佳反应条件为:反应时间1 h,n(乙酸):n (正辛醇) = 1:1.8,离子液体剂量5%,带水剂用量10 mL,在该条件下,乙酸正辛酯的酯化率为95.4%,与模型预测值基本相符。[HSO3-pmim]HSO4离子液体在催化乙酸正辛酯制备过程中具有良好的催化活性和稳定性。

Response surface methodology (RSM) was applied to optimize the synthesis of octyl acetate from n-octanol catalyzed by acidic ionic liquid. Based on the single factor experiments, Box-Behnken central composite design was adopted to investigate the effects of various reaction conditions, including reaction time, alcohol/acid mole ratio, amount of water carrying agent, the amount of ionic liquid and their interactions on the esterification. The analysis from Design-Expert showed that the interactions between the amount of water carrying agent and the catalyst dosage, the molar ratio and the amount of ionic liquid were the strongest. The optimum conditions were as follows: reaction time 1 h, n(acetic acid):n(n-octanol) = 1:1.8, ionic liquid 5% of acid and the amount of water carrying agent 10 mL. Under the optimized conditions, the yield of octyl acetate reached 95.4%, in close agreement with values predicted by the mathe- matical model. [HSO3-pmim]HSO4 ionic liquid showed the good catalytic properties and stability on the esterification of n-octanol with acetic acid.

文章引用:
何燕斐, 韩晓祥, 周凌霄, 陈青, 杨菊红. 响应面分析法优化乙酸正辛酯制备工艺研究[J]. 化学工程与技术, 2012, 2(2): 24-29. http://dx.doi.org/10.12677/hjcet.2012.22006

参考文献

[1] L. O. Bernard, R. A. Ford. GRAS substances. Food Technology, 1998, 52(9): 81-91.
[2] 宋光林, 郭峰, 曾广铭等. 乳香中乙酸辛酯含量的测定[J]. 贵州科学, 2008, 26: 57-60.
[3] 北京化学试剂公司. 精细化学品手册[M]. 北京: 化学工业出版社, 2002: 857.
[4] N. D. Marti. Bioengineering techniques for streambank restoration: A review of central european practices. Watershed Restora- tion Project Report, 1995: 4-9.
[5] 汤晓君, 刘明武. 沸石分子筛催化合成乙酸辛酯[J]. 大庆石油学院学报, 2008, 32(3): 46-48.
[6] 韩杰丽, 李海峰, 王自为等. [(C6H5)2NH2][PW12O40]•4H2O催化合成乙酸辛酯的研究[J]. 山西大学学报(自然科学版), 2008, 31(2): 211-214.
[7] 章爱华, 邓斌, 刘文萍等. 对甲苯磺酸铜催化合成乙酸辛酯[J]. 应用化工, 2009, 38(11): 1586-1588.
[8] 张小曼. 离子液体催化合成食用香料乙酸辛酯的研究[J]. 中国食品添加剂, 2010, 2: 72-74.
[9] L. A. Blanch-ard, D. Hancu, E. J. Beckman, et al. Green proc- essing using ionic liquids and CO2. Nature, 1999, 399: 28.
[10] N. V. Plechkova, K. R. Seddon. Applications of ionic liquids in the chemical industry. Chemical Society Reviews, 2008, 37: 123- 150.
[11] J. X. Wang, Q. Wu, H. S. Li, et al. Research progress of acidic ionic liquids and their applications in catalysis reactions. Chemical Industry and Engineering Progress, 2008, 10(27): 1574-1592.
[12] T. Long, Y. F. Deng, S. C. Gan, et al. Appli-cation of choline chloride•xZnCl2 ionic liquids for prepara of biodiesel. Chinese Journal of Chemical Engineering, 2010, 18(2): 322-327.
[13] L. Yong, C. X. Jie, K. Yang, et al. Synthesis of tributyl citrate using acidic functional ionic liquid as catalyst. Journal of Mo- lecular Catalysis, 2008, 2(22): 105-110.
[14] X. X. Han, L. X. Zhou. Optimization of process variables in the synthesis of butyl butyrate using acid ionic liquid as catalyst. Chemical Engineering Journal, 2011, 172(1): 459-466.
[15] 葛静微, 罗均, 李小定等. 响应面分析法优化血红素提取工艺[J]. 食品科学, 2010, 31(8): 60-64.
[16] 朱升干, 郑典模, 张晓婕等. 响应面分析法优化乳化石蜡制备工艺[J]. 化学工程, 2010, 6(8): 87-90.
[17] 章凯, 黄国林, 黄小兰. 响应面法优化微波辅助萃取柠檬皮中果胶的研究[J]. 精细化工, 2010, 27(1): 52-56.
[18] 吴芹, 董斌琦, 韩明汉等. 新型Brφnsted酸性离子液体的合成与表征[J]. 光谱学与光谱分析, 2007, 10(27): 2027-2031.
[19] 章凯, 黄国林, 黄小兰. 响应面法优化微波辅助萃取柠檬皮中果胶的研究[J]. 精细化工, 2010, 27(1): 52-56.