Quarernary ammonium acidic ionic liquids as esterification catalyst for synthesis of n-butyl acetate

林文俊

doi:10.3969/j.issn.0438-1157.2011.z2.012

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Quarernary ammonium acidic ionic liquids as esterification catalyst for synthesis of n-butyl acetate

更新时间：2025-12-10

- Quarernary ammonium acidic ionic liquids as esterification catalyst for synthesis of n-butyl acetate
- CIESC Journal Issue S2, Pages: 74-79(2011)
- 作者机构：
  
  华侨大学材料科学与工程学院
- 作者简介：
- 基金信息：
- DOI：10.3969/j.issn.0438-1157.2011.z2.012
  CLC：
- Online First：20 December 2011，
  
  Published：20 December 2011
- 稿件说明：
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林文俊. Quarernary ammonium acidic ionic liquids as esterification catalyst for synthesis of n-butyl acetate[J]. CIESC Journal, 2011, (S2): 74-79.
DOI：

林文俊. Quarernary ammonium acidic ionic liquids as esterification catalyst for synthesis of n-butyl acetate[J]. CIESC Journal, 2011, (S2): 74-79. DOI： 10.3969/j.issn.0438-1157.2011.z2.012.

摘要

一步法制备了4种季铵盐型离子液体，并用FT-IR和1H NMR表征结构。结果表明所合成的离子液体符合其理论结构；以它们为催化剂进行了乙酸正丁酯的合成研究，在相同条件下乙酸正丁酯的产率顺序为［Et2NH2］［HSO4］>［Et3NH］［HSO4］>［n-Pro3NH］［HSO4］>［n-But3NH］［HSO4］，并且［Et2NH2］［HSO4］和［Et3NH］［HSO4］与产物不互溶，而［n-Pro3NH］［HSO4］和［n-But3NH］［HSO4］与产物互溶，表明季铵盐离子液体的催化活性和极性都随阳离子链长度的增加而降低。以三乙胺硫酸为催化剂考察了反应时间、反应温度、醇酸摩尔比和离子液体用量对乙酸正丁酯产率的影响规律，结果表明：在n(正丁醇)∶n(乙酸)∶n(离子液体)=1∶2∶0. 25，反应时间8 h，反应温度 90℃的条件下乙酸正丁酯的产率达到81. 94%。采用减压蒸馏，除去离子液体相中的水、乙酸正丁酯和未反应的原料，将离子液体进行循环使用4次，结果表明乙酸正丁酯的产率没有明显下降，说明离子液体的稳定性和循环使用性较好。

Abstract

Four kinds of quaternary ammonium ionic liquid were prepared by one-step method. The IR and 1H NMR spectra showed that their structures were in accordance with their theoretical structure. n-Butyl acetate was synthesized with acetic acid and n-butyl alcohol catalyzed by the 4 kinds of ionic liquids prepared under the same conditions. Their catalytic activity sequence was ［Et2NH2］［HSO4］>［Et3NH］［HSO4］> ［n-Pro3NH］［HSO4］［n-But3NH］［HSO4］

［Et2NH2］［HSO4］and ［Et3NH］［HSO4］were immiscible with the product

［n-Pro3NH］［HSO4］and ［n-But3NH］［HSO4］were miscrible with the product

the result showed the catalytic activity and polarity of ionic liquids were related to their cation structure

especially the chain length of the cation

both the catalytic activity and polarity of the ionic liquids were getting lower with the chain length increasing. The effects of reaction time

reaction temperature

molar ratio of n-butyl alcohol to acetic acid and catalyst dosage on the yield of n-butyl acetate were investigated when ［Et3NH］［HSO4］was selected as the catalyst of esterification reaction. Under the conditions of molar ratio of n(n-butyl alcohol):n(acetic acid)∶n(［Et3NH］［HSO4］) =1∶2∶0.25

reaction temperature 90℃ and reaction time 8 h

the yield of n-butyl acetate reached to 81.94%。After removal of water

n-butyl acetate and unreacted raw materials by vacuum distillation

the ionic liquid was recovered and reused 4 times

the yield of n-butyl acetate did not decreased markdely

it showed that the ionic liquid was stable during the reaction and could be reused.

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