Synthesis and Crystallization Mechanism for SAPO-34 Zeolite Derived from Magadiite

Bo Liu, Yu Gao, Hanlu Xu, Yuhang Feng,Zihan Zhou,Yuan Gao,Rongli Jiang

CHEMPLUSCHEM(2024)

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Abstract
In this work, we explored the hydrothermal synthesize and crystallization process of SAPO-34 zeolites from two-dimensional layered silicate magadiite by using tetraethylammonium hydroxide (TEAOH) as a templating agent. Comprehensive characterization was conducted by XRD, SEM, FTIR, Raman, and BET. Time-resolved PXRD analysis revealed that SAPO-34 zeolite exhibited a steep growth curve when the crystallization time was 30 h, and the crystallinity reached 98.65 % at 48 h. Specifically, the disruption of the magadiite layer exposed charged silanol groups on the surface, fostering an affinity for AlO4 and PO4 species, thereby initiating the nucleation process. Under the guidance of TEAOH, these nucleation sites transformed into SAPO-34 nuclei, gradually advancing towards crystallization. FTIR and Raman analyses affirmed the presence of 6Rs, followed by D6R and 4Rs SBUs, along with the characteristic CHA structure. Combined with 29Si NMR established that disaggregated silicate minerals served as zeolite synthesis "seeds", enhancing nucleation sites and overall crystallization efficiency. The disturbance of the magadiite layer exposed surface silanol groups, which in turn attracted AlO4 and PO4 species, leading to their incorporation into the 6Rs and D6R units and initiating the nucleation process. These sites then evolved into SAPO-34 nuclei, facilitating subsequent crystal growth.+ image
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Key words
crystallization process,hydrothermal synthesis,magadiite,SAPO-34,templating agent
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