超声辐射下酸性离子液体催化合成1,1-二乙酸酯

doi:10.13218/j.cnki.csdc.2014.12.155

日用化学工业 ›› 2014, Vol. 44 ›› Issue (12): 695-699.doi: 10.13218/j.cnki.csdc.2014.12.155

超声辐射下酸性离子液体催化合成1,1-二乙酸酯

汤小芳^1,2, 刘显明^1,2, 周昊^1,2, 仇涛涛¹, 储海蓉¹, 邢志恒¹

1.南京理工大学泰州科技学院化工学院,江苏泰州 225300;
2.泰州南京理工大学研究院,江苏泰州 225300

收稿日期:2014-07-04 出版日期:2014-12-22 发布日期:2019-04-08
作者简介:汤小芳(1982-),女,江苏南通人,讲师,硕士,电话:(0523)86150058,E-mail:754477121@qq.com。
基金资助:
江苏省高等学校大学生实践创新训练计划资助项目(201413842004Y);南京理工大学泰州科技学院化工学院"梦兰神彩"大学生创新基金资助项目(CX2014005)

Synthesis of 1,1-diacetates with acidic ionic liquid as catalyst under ultrasonic irradiation

TANG Xiao-fang^1,2, LIU Xian-ming^1,2, ZHOU Hao^1,2, CHOU Tao-tao¹, CHU Hai-rong¹, XING Zhi-heng¹

1.Chemical Engineering Institute,Taizhou College of Science and Technology, Nanjing University of Science and Technology,Taizhou,Jiangsu 225300,China;
2.Taizhou Research Institute of Nanjing University of Science and Technology,Taizhou,Jiangsu 225300,China

Received:2014-07-04 Online:2014-12-22 Published:2019-04-08

摘要/Abstract

摘要： 室温无溶剂超声辐射下,以功能化酸性离子液体[C₃SO₃Hnhm][HSO₄]为催化剂、芳香醛和乙酸酐为原料合成1,1-二乙酸酯。通过单因素试验优化了反应条件,研究了该离子液体的重复使用性能及催化剂的底物适用性。结果表明,当苯甲醛与乙酸酐的摩尔比为1:2.3,20 ℃超声辐射反应15 min,催化剂用量为苯甲醛物质的量的1%时,收率可达96%以上;[C₃SO₃Hnhm][HSO₄]重复使用5次,其催化活性下降不明显;将[C₃SO₃Hnhm][HSO₄]用于其他芳香醛的催化,收率为84%~98%。

关键词: 1,1-二乙酸酯, 酸性离子液体, 超声辐射, 催化合成, 绿色工艺

Abstract: Under conditions of room temperature,solvent-free and ultrasonic irradiation,with an aromatic aldehyde and acetic anhydride as starting materials and functionalized acidic ionic liquid [C₃SO₃Hnhm][HSO₄] as catalyst,1,1-diacetates was synthesized.The optimal reaction conditions were found by single factor experiments.Reusing performance of the catalyst as well as applicability of the substrate were investigated.Results showed that when the molar ratio of benzaldehyde and acetic anhydride is 1:2.3;the reaction temperature is 20 ℃;ultrasonic irradiation applies for 15 min;and the dosage of catalyst is 1% of benzaldehyde;the yield can reach more than 96%.The catalyst [C₃SO₃Hnhm][HSO₄] can be reused for 5 times with no significant declining of the catalytic activity.In case the catalyst [C₃SO₃Hnhm][HSO₄] is used to catalyze the reaction of other aromatic aldehydes,the yield achieves 84%-98%.

Key words: 1,1-diacetate, acidic ionic liquid, ultrasonic irradiation, catalytic synthesis, green technology

中图分类号:

TQ655

汤小芳, 刘显明, 周昊, 仇涛涛, 储海蓉, 邢志恒. 超声辐射下酸性离子液体催化合成1,1-二乙酸酯[J]. 日用化学工业, 2014, 44(12): 695-699.

TANG Xiao-fang, LIU Xian-ming, ZHOU Hao, CHOU Tao-tao, CHU Hai-rong, XING Zhi-heng. Synthesis of 1,1-diacetates with acidic ionic liquid as catalyst under ultrasonic irradiation[J]. China Surfactant Detergent & Cosmetics, 2014, 44(12): 695-699.

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超声辐射下酸性离子液体催化合成1,1-二乙酸酯

Synthesis of 1,1-diacetates with acidic ionic liquid as catalyst under ultrasonic irradiation

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