›› 2020, Vol. 22 ›› Issue (4): 93-100.

• Catalyst Research • 上一篇    下一篇

高岭土/尿素插层复合材料合成ZSM-5分子筛及表征

郑淑琴1,陈欧2,刘思成3,张培青3   

  1. 1. 湖南理工学院化学化工学院,湖南省精细石油化工催化与分离重点实验室
    2. 湖南省精细石油化工催化与分离重点实验室
    3. .湖南理工学院化学化工学院
  • 收稿日期:2020-04-29 修回日期:2020-07-12 出版日期:2020-12-30 发布日期:2020-12-30
  • 通讯作者: 郑淑琴 E-mail:zhengshuqin37@163.com

Synthesis and Characterization of ZSM-5 Molecular Sieve Made from Kaolin/Urea Intercalation Composite

Zheng Shuqin1,Chen Ou2,Liu Sicheng2,Zhang Peiqing2   

  1. 1. Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology
    2.
  • Received:2020-04-29 Revised:2020-07-12 Online:2020-12-30 Published:2020-12-30
  • Contact: Zheng Shuqin E-mail:zhengshuqin37@163.com

摘要: 研究了直接插层法制备高岭土/尿素插层复合材料和以该材料采用原位技术合成含ZSM-5分子筛的催化复合材料。重点研究了插层率、脱嵌速率、插层复合材料加入量对合成分子筛复合材料的影响。采用粉末X射线衍射法(XRD),红外光谱(FT-IR),热重-差热(TG-DTA),N2 静态吸附法和电子扫描电镜(SEM)对样品进行表征。结果表明,在合成体系中加入高岭土/尿素插层复合物合成出的ZSM-5分子筛物相单一。随着插层复合物的插层率增加,ZSM-5分子筛的结晶度先增加随后降低。当插层率为62%时,ZSM-5分子筛的结晶度较低。当22%插层率的插层复合物的加入量为3%时,ZSM-5分子筛的结晶度达到65%。与不添加插层复合物合成的产物相比,ZSM-5分子筛的结晶度提高了54.8%。合成的ZSM-5分子筛复合材料具有较好的热稳定性和多级孔道结构,其粒径约为2.5μm,BET比表面积为236m2/g,孔径为10.6nm。

关键词: 插层复合材料, 尿素, 高岭土, ZSM-5沸石, 原位技术

Abstract: In this paper, the kaolin/urea intercalation composites prepared by direct intercalation method and the catalysis composites containing ZSM-5 molecular sieve synthesized based on the kaolin/urea intercalation composites by an in-situ crystallization technique were investigated. The effects of the intercalation ratios and de-intercalation rate and the amounts of added kaolin/urea intercalation composite on the synthesis of the catalysis composites containing the ZSM-5 molecular sieve were studied. The samples were characterized by X-ray diffraction, FT-IR, TG-DTA, N2 adsorption-desorption, and SEM, respectively. The results showed that the structure of the samples prepared by kaolin/urea intercalation composite was pure ZSM-5 molecular sieve. The crystallinity of ZSM-5 molecular sieve increased at first and then decreased with the increase of intercalation ratio of kaolin/urea intercalation composite. When the intercalation ratio was 62%, the crystallinity of ZSM-5 molecular sieve was lower. When the amount of added kaolin/urea intercalation composite with an intercalation ratio of 22% was 3%, the crystallinity of ZSM-5 zeolite was improved to reach 65%. Compared to the crystallization product formed without adding kaolin/urea intercalation composite, the crystallinity of ZSM-5 molecular sieve has increased by 54.8%. The catalytic composites containing ZSM-5 molecular sieve had better thermal stability with a wide pore structure, featuring a particle diameter of about 2.5 μm, a BET specific surface area of 236 m2/g, and a pore size of 10.6 nm.

Key words: intercalation composite, urea, kaolin, ZSM-5 zeolite, in-situ technique