应用化学 ›› 2011, Vol. 28 ›› Issue (06): 667-672.DOI: 10.3724/SP.J.1095.2011.00454

• 研究论文 • 上一篇    下一篇

硅胶微球负载钛硅分子筛TS-1催化剂的制备及对苯氧化合成苯酚的催化性能

刘雅哲1,肖剑白2,盖鸿玮1,肖如亭1*   

  1. ( 1.天津理工大学化学化工学院 天津 300384;2.北京博源恒升高科技有限公司 北京)
  • 收稿日期:2010-08-05 修回日期:2010-09-27 出版日期:2011-06-10 发布日期:2011-06-10
  • 通讯作者: 肖如亭,教授; Tel/Fax:022-23732051; E-mail:xrt16@sina.com; 研究方向:绿色化学与工艺

Preparation and Catalytic Properties for Synthesis of Phenol by Oxidizing Benzene of TS-1 Loaded on Silica Gel Microsphere

LIU Yazhe1, XIAO Jianbai2, GAI Hongwei1, XIAO Ruting1*   

  1. (1.School of Chemistry anc Chemical Cngineering,Tianjin University of Technology,Tianjin 300384;
    2.Beijing Boyuan-Hengsheng High-Technology Co.,Ltd,Beijing)
  • Received:2010-08-05 Revised:2010-09-27 Published:2011-06-10 Online:2011-06-10

摘要:

将硅胶微球浸渍于钛硅分子筛(TS-1)合成液中,经晶化、焙烧制得负载TS-1分子筛硅胶微球催化剂。 用XRD、IR和SEM测试技术对其进行表征,将其用于过氧化氢氧化苯合成苯酚的反应中。 结果显示,TS-1分子筛能够很好地负载于硅胶表面,晶化温度160 ℃,晶化时间72 h,焙烧温度550 ℃,焙烧时间6 h时,获得的催化剂显示良好的催化性能。 在苯和H2O2初始原料量分别为0.5和0.1 mol、催化剂加入量为8 g、反应温度为60 ℃条件下,经过3 h的反应,苯的转化率达到10.32%,苯酚选择性达到97.12%。 9次重复使用后的苯转化率为9.42%,苯酚选择性为93.14%。

关键词: 微球硅胶, 负载催化剂, 钛硅分子筛(TS-1), 苯, 苯酚

Abstract:

Catalysts of titanosilicate zeolite(TS-1) supported on silica gel microsphere were prepared after direct crystallization and calcination of the microspheric silica gel soaked in the TS-1 synthetic solution, in order to produce catalysts with good catalytic and recycling properties. The catalysts were characterized by XRD, IR and SEM, and were used in the synthesis of phenol by a direct oxidation of benzene with the hydrogen peroxide as the oxidant. The result showed that TS-1 molecular sieve was loaded on the surface of silica gel very well. On the conditions with the crystallization temperature at 160 ℃, crystallization time of 72 h, calcination temperature of 550 ℃, and calcination time of 6 h, the catalysts prepared showed good catalytic properties. On the conditions of the initial material content of benzene 0.5 mol and hydrogen peroxide 0.1 mol, catalyst 8 g, the reaction temperature at 60 ℃, and the reaction time 3 h, the convertion of benzene was 10.32%, and the selectivity to phenol was 97.12%. After recycling for nine times, the convertion of benzene was 9.42%, and the selectivity to phenol was 93.14%.

Key words: silica gel microsphere, supported catalyst, titanosilicate zeolite TS-1, benzene, phenol

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