石油炼制与化工 ›› 2022, Vol. 53 ›› Issue (4): 82-88.

• 基础研究 • 上一篇    下一篇

X分子筛的热稳定性研究

王智远,高宁宁,王辉国,钟进   

  1. 中国石化石油化工科学研究院
  • 收稿日期:2021-08-16 修回日期:2021-12-28 出版日期:2022-04-12 发布日期:2022-03-29
  • 通讯作者: 高宁宁 E-mail:gaoningning.ripp@sinopec.com
  • 基金资助:
    中国石油化工股份有限公司科研开发课题

STUDY ON THE THERMAL STABILITY OF X ZEOLITE

  • Received:2021-08-16 Revised:2021-12-28 Online:2022-04-12 Published:2022-03-29

摘要: 为了研究X分子筛的热稳定性,采用水热晶化法合成了纯相X分子筛,在氮气气氛中分别于500,600,700,800,900 ℃对X分子筛进行高温焙烧处理。采用X射线衍射、N2吸附-脱附、扫描电镜、热重分析、差示扫描量热、固体核磁共振和傅里叶变换红外光谱对X分子筛及其热处理产物进行表征。结果表明,热处理温度不超过800 ℃时,X分子筛晶体结构和微孔孔道均没有被破坏,热处理产物仍然保持了八面体形貌,晶体结构中的Si-O-Al连接保持稳定,且没有形成非骨架铝物种。当热处理温度达到900 ℃时,X分子筛的晶体结构发生熔融破坏,转变为边缘圆滑的无定形物种,微孔孔体积降至0,但是热处理产物中并没有形成明显的独立无定形铝物种,而是仍然存在大量Si-O-Al和Si-O-Si连接。

关键词: 分子筛, FAU拓扑结构, 热稳定性

Abstract: In order to study the thermal stability of X zeolite, X zeolite was synthesized by using hydrothermal crystallization method, and then was calcined at 500, 600, 700, 800 and 900 ℃ in nitrogen atmosphere. X zeolite and its calcination products were thoroughly characterized by X-ray diffraction, N2 adsorption-desorption, scanning electron microscope, thermogravimetry, differential scanning calorimetry, magic angle spinning solid nuclear magnetic resonance and Fourier transform infrared spectroscopy. The results showed that when the calcination temperature was lower than 800 °C, the crystalline structure and micropores of X zeolite were not destroyed, the calcination products still maintained the same octahedral morphology as the original X zeolite, the Si-O-Al connection in the crystalline structure was stable, and no non-framework aluminum species were formed. When the calcination temperature reached 900 °C, the crystalline structure of X zeolite was completely destroyed after melting, leading to the formation of the amorphous species with smooth edge and the micropore volume of 0. There were still a lot of Si-O-Al and Si-O-Si connections, and no obvious independent amorphous aluminum species was observed in the calcination products.

Key words: zeolite, FAU topological structure, thermal stability