无机盐工业

无机盐工业 ›› 2021, Vol. 53 ›› Issue (3): 93-96.doi: 10.11962/1006-4990.2020-0224

• 催化材料 • 上一篇    下一篇

超声辅助稀土改性二氧化锡催化合成乙酰水杨酸

徐菁璐1(),陈浩1(),陈桂2(),张海科3,熊飞2   

  1. 1.岳阳职业技术学院,湖南岳阳 414000
    2.怀化学院
    3.岳阳兴长石化股份有限公司
  • 收稿日期:2020-09-14 出版日期:2021-03-10 发布日期:2021-03-11
  • 通讯作者: 陈浩,陈桂
  • 作者简介:徐菁璐(2000— ),女,主要研究方向为应用化工;E-mail:1574430445@qq.com
  • 基金资助:
    湖南省教育厅科研项目(17C1261)

Catalytic synthesis of acetosalicylic acid over ultrasound-assisted rare earth modified SnO2

Xu Jinglu1(),Chen Hao1(),Chen Gui2(),Zhang Haike3,Xiong Fei2   

  1. 1. Yueyang Vocational and Technical College,Yueyang 414000,China
    2. Huaihua University
    3. Yueyang Xingchang Petrochemical Co.,Ltd.
  • Received:2020-09-14 Online:2021-03-10 Published:2021-03-11
  • Contact: Chen Hao,Chen Gui

摘要:

以水杨酸、乙酸酐为原料,稀土钇(Y3+)、铈(Ce3+)、镧(La3+)改性氧化锡(SnO2)为催化剂,在超声辅助下合成乙酰水杨酸,Y3+/SnO2催化剂表现出最佳的催化效果。通过单因素实验考察了水杨酸与乙酸酐物质的量比、催化剂用量、反应时间、超声功率、反应温度、析晶时间对合成乙酰水杨酸反应的影响。通过红外光谱(FT-IR)、扫描电镜(SEM)和X射线衍射(XRD)等手段对催化剂和合成的产物进行了表征。最佳实验条件:水杨酸与乙酸酐物质的量比为1∶2、催化剂(Y3+/SnO2)用量为水杨酸质量的8%、反应时间为30 min、反应温度为70 ℃、超声功率为70 W、析晶时间为2 h。在此条件下,乙酰水杨酸的产率为83.6%。催化剂重复使用5次后仍有较高的催化活性。该催化剂具有催化效果好、无污染、无腐蚀性、重复利用率高等优点。

关键词: 二氧化锡, 乙酰水杨酸, 固体酸催化剂, 酯化反应

Abstract:

Acetylsalicylic acid was synthesized with salicylic acid and acetic anhydride as raw materials,rare earth(Y3+,Ce3+,La3+) modified SnO2 as catalyst assisted by ultrasound irradiation and the Y3+/SnO2 catalyst showed the best catalytic perfor-mance.The effects of amount-of-substance ratio of salicylic acid to acetic anhydride,amount of catalyst,reaction time,ultrasonic power,reaction temperature and crystallization time on the synthesis of acetylsalicylic acid were investigated.The catalysts and synthetic products were characterized by FT-IR,SEM and XRD.The optimum experimental condition with the yield of acetylsalicylic acid of 83.6 % was obtained as follows:the amount of substance ratio of salicylic acid to acetic anhy-dride is 1∶2,the amount of catalyst(Y3+/SnO2 ) is 8% that of salicylic acid,reaction temperature is 70 ℃,ultrasonic power is 70 W,reaction time is 30 min and crystallization time is 2 h.The catalyst can be reused for 5 times which still remains high catalytic activity.The catalyst has the advantages of good catalytic effect,no pollution,no corrosion and high reuse rate.

Key words: SnO2, acetylsalicylic acid, solid acid catalyst, esterification reaction

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