[1] Zhao Huan, Xiao Guomin, Lü Jianhua,. Separation of picolines by dissociation extraction [J]. Journal of Southeast University (English Edition), 2005, 21 (1): 68-72. [doi:10.3969/j.issn.1003-7985.2005.01.015]
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Separation of picolines by dissociation extraction(
)
甲基吡啶的解离萃取分离实验研究
)Journal of Southeast University (English Edition)[ISSN:1003-7985/CN:32-1325/N]
- Volumn:
- 21
- Issue:
- 2005 1
- Page:
- 68-72
- Research Field:
- Chemistry and Chemical Engineering
- Publishing date:
- 2005-03-30
Info
- Title:
- Separation of picolines by dissociation extraction
- 甲基吡啶的解离萃取分离实验研究
- Author(s):
- Zhao Huan; Xiao Guomin; Lü Jianhua
- Department of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096, China
- Keywords:
- 3-picoline; 4-picoline; separation; dissociation extraction; orthogonal test
- PACS:
- TQ028.8
- DOI:
- 10.3969/j.issn.1003-7985.2005.01.015
- Abstract:
- The separation of the by-product(The volume fraction of 3-picoline is 68.472 2% and 4-picoline 26.517 6%.)in the synthesis of pyridine by dissociation extraction was studied.Six separation conditions of the dissociation extraction—the kind and the dosage of extractant and organic solvent, the concentration of the extractant and separation temperature—were investigated.Different levels of each factor were chosen to form an orthogonal test of six factors and five levels.The results show that the volume ratio of 3-picoline and 4-picoline in organic phase is the highest when 24 mL picolines are separated at 0 ℃ by 2.0 mol/L p-toluenesulfonic and n-heptane whose dosages are 40 mL and 48 mL, respectively.The effect of the separation is considerably improved with repetition test.This process of dissociation extraction has commendable potential for industrial exploitation.
- 应用解离萃取分离合成吡啶产生的3-甲基吡啶(3-MPD)与4-甲基吡啶(4-MPD)的混合物(φ(3-MPD)=68.472 2%;φ(4-MPD)=26.517 6%), 对影响解离萃取分离的6个因素萃取剂、萃取剂的浓度及投料量、有机溶剂及投料量, 以及分离温度进行了研究.选取了各因素的不同水平进行了六因素五水平的正交试验, 以有机相两甲基吡啶的体积比为主要考查对象, 筛选出了解离萃取分离甲基吡啶混合物的最佳工艺条件:当甲基吡啶的混合物为24 mL时, 以浓度为2 mol/L的对甲基苯磺酸为萃取剂, 用量为40 mL, 正庚烷为溶剂, 用量为48 mL, 温度为0 ℃时分离效果最好.通过重复性实验, 分离效果得到明显提高, 说明此法具有工业化潜力.
References:
[1] Zhao Huan, Xiao Guomin.Separation of mixtures of 3-methylpyridine with 4-methylpyridine [J].Science and Technology in Chemical Industry, 2003, 12(4):52-56.(in Chinese)
[2] Sun Xuefei, Han Fujun, Qin Wei, et al.Dissociation extraction and its applications[J].Modern Chemical Industry, 2000, 20(5):14-17.(in Chinese)
[3] Anwar M M, Hanson C, Patel A N, et al.Dissociation extraction, Part Ⅱ:Multi-stage extraction [J].Trans Instn Chem Engrs, 1973, 51:151-158.
[4] Anwar M M, Arif A S, Pritchard D W.Multistage separation of quinoline and iso-quinoline by dissociation extraction [J].Solvent Extractive and Ion Exchange, 1998, 16(47):931-935.
[5] Wu Guisheng.Experiment design and data processing[M].Beijing:Metallurgy Industry Press, 1997.(in Chinese)
[6] Anwar M M, Hanson C, Patel A N.Detection of pyridine derivatives [J].J Chromat, 1968, 34(5):529.
[7] Gaikar Vilas G, Mahapatra Alpana, Sharma Man Mohan.Separation of close boiling point mixtures(p-Cresol/m-Cresol, Guaiacol/Alkylphenols, 3-picoline/4-picoline, substituted anilines)through dissociation extractive crystallization[J].Ind Eng Chem Res, 1989, 28(2):199-204.
[8] Sun Chunxia, Peng Panying, Wang Yuping, et al.Separation of 3-picoline and 4-picoline [J].Journal of Nanjing Normal University (Engineering and Technology), 2004, 4(2):11-13.(in Chinese)
Memo
- Memo:
- Biographies: Zhao Huan(1981—), female, graduate;Xiao Guomin(corresponding author), male, doctor, professor, xiaogm@seu.edu.cn.