石油炼制与化工 ›› 2023, Vol. 54 ›› Issue (3): 48-53.

• 催化剂 • 上一篇    下一篇

基于FIB-SEM和TEM的催化裂化催化剂元素分布研究

安谧,徐华,张若霖,张兆前,郑方,王剑   

  1. 中国石油石油化工研究院
  • 收稿日期:2022-09-01 修回日期:2022-11-15 出版日期:2023-03-12 发布日期:2023-03-23
  • 通讯作者: 安谧 E-mail:anmi@petrochina.com.cn

STUDY ON ELEMENT DISTRIBUTION OF FCC CATALYST BASED ON FIB-SEM AND TRANSMISSION ELECTRON MICROSCOPE

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  • Received:2022-09-01 Revised:2022-11-15 Online:2023-03-12 Published:2023-03-23

摘要: 为了研究催化裂化(FCC)催化剂的失活机理,利用聚集离子束扫描电镜(FIB-SEM)制作透射电镜样品;采用扫描电镜、透射电镜、X射线荧光光谱、X射线能谱等手段,对FCC催化剂单个颗粒及其FIB切片的元素分布进行表征。结果发现:与新鲜剂相比,催化裂化过程中FCC平衡剂上沉积了Fe,Ni,V,Ca,P等元素;随着杂质元素沉积量的增加,催化剂的骨架密度逐渐增大;随着骨架密度增大,催化剂Fe,Ni,Ca含量提高,而其硅铝比、P含量、比表面积降低;Fe,Ni,P元素主要分布在催化剂颗粒外表面,V元素在催化剂内部和外部分布比较均匀。

关键词: 催化裂化催化剂, 铁污染, 单颗粒, 失活, 聚集离子束扫描电镜, 透射电镜

Abstract: In order to study the deactivation mechanism of fluid catalytic cracking (FCC) catalyst, transmission electron microscopy specimen was prepared by means of aggregation ion beam-scanning electron microscope (FIB-SEM). The elemental distribution of FCC catalyst on individual particle and their FIB sections was characterized by SEM, TEM, X-ray fluorescence spectrum, X-ray energy spectrum and other analysis instruments. The results showed that Fe, Ni, V, Ca and P were deposited on FCC equilibrium catalyst, and the skeleton density of FCC catalyst increased with the increase of impurity deposition. The contents of Fe, Ni and Ca in catalysts increased with the increase of skeleton density, while the Si/Al ratio, P content and specific surface area decreased, the distribution of V element in the inner and outer parts of the catalyst was relatively uniform.

Key words: FCC catalyst, Fe poisoning, individual particle, deactivation, FIB-SEM, transmission electron microscope