中国炼油与石油化工 ›› 2012, Vol. 14 ›› Issue (3): 68-74.

• Catalyst Research • 上一篇    下一篇

气相转移法合成MnSAPO-34及其催化性能研究

韶晖1,陈霞1,王彬彬1,钟璟1,杨超2   

  1. 1. 常州大学
    2. 中国科学院过程工程研究所
  • 收稿日期:2012-03-12 修回日期:2012-05-23 出版日期:2012-09-30 发布日期:2012-10-22
  • 通讯作者: 韶晖 E-mail:shaohui200800@gmail.com
  • 基金资助:
    Production and Research Prospective Joint Research Project;江苏省高校自然科学研究重大项目(11KJA610002)

Vapor-Phase Transport Synthesis of MnSAPO-34 and Its Catalytic Properties

  • Received:2012-03-12 Revised:2012-05-23 Online:2012-09-30 Published:2012-10-22

摘要: 以三乙胺为结构导向剂,采用气相转移法合成MnSAPO-34磷铝分子筛,通过XRD, BET, SEM, UV-Vis, FT-IR等分析手段对其进行表征。考察了晶化条件,干胶组成对分子筛合成的影响。结果表明,合成条件对分子筛的晶相有一定的影响,当干胶中n(MnO) / n(Al2O3 )为 0. 1~0. 2,在140 °C下晶化18 h,可以得到具有CHA结构的高纯度MnSAPO-34分子筛。超出此范围,具有AFI结构的MnSAPO-5将以杂晶的形式出现。UV-Vis和FT-IR的表征结果显示,Mn2+进入了分子筛骨架。将分子筛催化1,2-丙二醇和环己烷的缩酮反应,产物环己酮1,2-丙二醇缩酮的收率较高,说明MnSAPO-34对该缩酮反应有较好的催化性能。

关键词: MnSAPO-34, 气相转移法(VPT), 缩酮反应

Abstract: MnSAPO-34 molecular sieves were synthesized by vapor-phase transport (VPT) method using triethylamine (Et3N) as a structure directing agent (SDA), and were characterized by XRD, BET, SEM, UV-Vis and FT-IR and TG. The influence of the crystallization conditions and the dry-gel composition were investigated. The results showed the synthesis conditions had an effect on the crystalline phase. Pure MnSAPO-34 had been obtained when crystallized at 140 °C for 18 hours. The ratios of MnO/Al2O3 in the starting gel from 0.1 to 0.2 resulted in pure MnSAPO-34 with CHA topology. Beyond the scope, MnSAPO-5 with AFI topology structure was obtained as an impurity. UV-Vis spectroscopy and FT-IR indicated that manganese incorporated into the framework of the molecular sieve. The catalytic performance of MnSAPO-34 molecular sieve was tested by ketalation reaction of 1, 2-propanediol and cyclohexanone. High yield of cyclohexanone1, 2-propanediol ketal was obtained.

Key words: MnSAPO-34, Vapor-phase transport (VPT), Ketalization