石油炼制与化工 ›› 2022, Vol. 53 ›› Issue (2): 69-76.

• 催化剂 • 上一篇    下一篇

低硅X分子筛的合成研究

高宁宁,刘相李,拓鹏飞,高俊魁,钟进,王辉国,郁灼   

  1.  中国石化石油化工科学研究院
  • 收稿日期:2021-06-18 修回日期:2021-10-11 出版日期:2022-02-12 发布日期:2022-01-20
  • 通讯作者: 高宁宁 E-mail:gaoningning.ripp@sinopec.com
  • 基金资助:
    中国石化科技部

SYNTHESIS OF X ZEOLITE WITH LOW SILICA TO ALUMINA RATIO

  • Received:2021-06-18 Revised:2021-10-11 Online:2022-02-12 Published:2022-01-20

摘要: 为了合成结晶度较高的纯低硅X分子筛,系统研究了合成体系的硅铝比[n(SiO2)/n(Al2O3)]、碱硅比[n(Na2O+K2O)/n(SiO2)]、水碱比[n(H2O)/n(Na2O+K2O)]、钾碱比[n(K2O)/n(Na2O+K2O)]及老化温度、晶化温度对产物性质的影响规律,采用X射线衍射、甲苯动态吸附、X射线荧光光谱、固体核磁共振、扫描电镜对产物进行表征。结果表明:随着合成体系硅铝比、碱硅比、水碱比、钾碱比、老化温度、晶化温度的升高,所得低硅X分子筛的结晶度和合成产物的甲苯吸附容量均呈先升高后降低趋势;合成体系优选的硅铝比为2.05、碱硅比为3.25、水碱比为17、钾碱比为0.23、老化温度为50~80 ℃、晶化温度为95 ℃,所得低硅X分子筛的形貌为0.5~1.5 μm晶粒聚集的球体,硅铝比为2.0,不含非骨架铝。

关键词: FAU, 分子筛, 吸附, 芳烃

Abstract: In order to synthesize pure low silicon X zeolite with high crystallinity, the effects of n(SiO2)/n(Al2O3, n(Na2O+K2O)/n(SiO2),n(H2O)/n(Na2O+K2O)  and n(K2O)/n(Na2O+K2O)  as well as aging and crystallization temperature on the properties of the products were systematically investigated. The products were characterized by X-ray diffraction, dynamic adsorption of toluene, X-ray fluorescence spectrum, solid state nuclear magnetic resonance, and scanning electron microscopy. The results showed that with the increase of n(SiO2)/n(Al2O3n(Na2O+K2O)/n(SiO2,n(H2O)/n(Na2O+K2O) n(K2O)/n(Na2O+K2O) , aging temperature and crystallization temperature, the crystallinity and toluene adsorptive capacity of the synthesized low silicon X zeolite was increased firstly and then decreased. Under the optimum conditions covering a n(SiO2)/n(Al2O3) of 2.05, a n(Na2O+K2O)/n(SiO2) of 3.25, a n(H2O)/n(Na2O+K2O) of 17, a n(K2O)/n(Na2O+K2O) of 0.23, an aging temperature of 50-80 °C, and a crystallization temperature of 95 °C, the low silicon X zeolite with high crystallinity degree can be obtained. The low silicon X zeolite with a n(SiO2)/n(Al2O3of 2.0 without non-framework Al, shows sphere morphorology with a diameter of 0.5-1.5 μm.

Key words: FAU, zeolite, adsorption, aromatics