Synthesis of monolithic SSZ-13 zeolite by dry-gel conversion method

FENG Qing; PEI Renyan; LIU Hongguang; YU Haibin; ZHANG Lijuan; ZHANG Yaori

doi:10.11949/j.issn.0438-1157.20161381

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Synthesis of monolithic SSZ-13 zeolite by dry-gel conversion method

更新时间：2025-12-10

- Synthesis of monolithic SSZ-13 zeolite by dry-gel conversion method
- CIESC Journal Issue 3, Pages: 1231-1238(2017)
- 作者机构：
  
  1. 河北工业大学化工学院,天津,300130
  2. 中海油天津化工设计研究院有限公司,天津,300130
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20161381
  CLC： Q426.94
- Online First：05 March 2017，
  
  Published：05 March 2017
- 稿件说明：
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FENG Qing, PEI Renyan, LIU Hongguang, et al. Synthesis of monolithic SSZ-13 zeolite by dry-gel conversion method[J]. CIESC Journal, 2017, (3): 1231-1238.
DOI：

FENG Qing, PEI Renyan, LIU Hongguang, et al. Synthesis of monolithic SSZ-13 zeolite by dry-gel conversion method[J]. CIESC Journal, 2017, (3): 1231-1238. DOI： 10.11949/j.issn.0438-1157.20161381.

摘要

采用干胶转化法合成了整体式SSZ-13分子筛，先成型后晶化，系统地考察了物料配比及晶化条件对合成结果的影响，通过X射线衍射（XRD）、X射线荧光（XRF）、热重-差热分析仪（TG-DTA）、扫描电子显微镜（SEM）、氨气的程序升温吸附-脱附（NH3-TPD）、傅里叶红外光谱仪（FI-IR）、液体核磁共振谱（NMR）对产物进行表征分析，并讨论了混合模板剂N，N，N-三甲基-1-金刚烷氢氧化铵和氯化胆碱在晶化过程中起的作用。结果表明，合成的整体式SSZ-13分子筛具有典型的介孔堆积孔、较大的比表面积，在空气中热稳定性良好。氯化胆碱加速了分子筛晶化，缩短了晶化时间，提高产物的结晶度，明显降低了N，N，N-三甲基-1-金刚烷氢氧化铵的使用量，起到了辅助结构导向的作用，且混合模板剂均填充产物孔道。

Abstract

In this work

monolithic SSZ-13 zeolite was synthesized using dry-gel conversion method. The influences of the gel composition and crystallization conditions on the crystallization of SSZ-13 zeolite were investigated. The as-synthesized product was characterized by X-ray diffraction (XRD)

X-ray fluorescence (XRF)

thermo gravimetric-differential thermal analysis (TG-DTA

scanning electron microscope(SEM)

NH3 temperature-programmed desorption(NH3-TPD

Nuclear Magnetic Resonance (NMR). The roles of N

N-trimethyl-1-adamantanammonium (TMADa+) and choline chloridein crystallization reaction were discussed. According to the result

the monolithic SSZ-13 zeolite has typical accumulated mesopores

larger surface area and better thermal stability in air. The results in FT-IR and NMR spectra show that choline chloride could act as a secondary structure-directing agent and fill in the pores of zeolite

which significantly reduced the amount of TMADa+. It was confirmed that Choline Chloride favors accelerating zeolite nucleation

shortening the crystallization time

and improving crystallinity of the as-synthesized product.

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