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Zeolite synthesis under acidic conditions has always presented a challenge. In this study, we successfully prepared series of ZSM‐5 zeolite nanosheets (Z‐5‐SCA‐X) over a broad pH range (4 to 13) without the need for additional supplements. This achievement was realized through aggregation crystallization of ZSM‐5 zeolite subcrystal (Z‐5‐SC) with highly short‐range ordering and ultrasmall size extracted from the synthetic system of ZSM‐5 zeolite. Furthermore, the crystallization behavior of Z‐5‐SC was investigated, revealing its non‐classical crystallization process under mildly alkaline and acidic conditions (pH<10), and the combination of classical and non‐classical processes under strongly alkaline conditions (pH≥10). What's particularly intriguing is that, the silanol nest content in the resultant Z‐5‐SCA‐X samples appears to be dependent on the pH values during the Z‐5‐SC crystallization process rather than its crystallinity. Finally, the results of the furfuryl alcohol etherification reaction demonstrate that reducing the concentration of silanol nests significantly enhances the catalytic performance of the Z‐5‐SCA‐X zeolite. The ability to synthesize zeolite in neutral and acidic environments without the additional mineralizing agents not only broadens the current view of traditional zeolite synthesis but also provides a new approach to control the silanol nest content of zeolite catalysts. [ABSTRACT FROM AUTHOR]

A mild alkaline modification treatment to both Lewis and Brønsted acid sites of Zr-Al-Beta zeolite, leading to its superior catalytic performance and resistance to coking in MPV reduction of furfural. • Zr-Al-Beta promoted by alkali-metal ions possess good stability and tolerance to carbon deposits. • Detailed characterizations demonstrated modification of alkali-metal ions on acid sites. • Alkaline ion modified Zr-Al-Beta high-selectively convert furfural under high concentration. • Alkaline treatment to zeolites was proved possibility of potential application. Zirconium-substituted zeolites prepared by post-synthetic procedure have demonstrated excellent performance in the upgrading process of biomass platform compounds owing to the unique Lewis acid character. However, many pressing questions still surround these materials, especially relating to specific conversion, catalyst stability and substrate scalability. In the present study, a simple alkaline treatment to the Zr-Al-Beta zeolite in alcoholic solution of alkali metal hydroxide was conducted. The modification of alkali-metal ions on both Lewis acid sites and Brønsted acid sites in Zr-Al-Beta was evidenced by XPS and FT-IR spectroscopy (CO and pyridine). The untreated materials displayed poor product selectivity and high coke deposit in the Meerwein-Ponndorf-Verley reduction of furfural and isopropanol; however, the treatment of alkali-metal ions promoted their catalytic performance with improved recalcitrance to deactivation and coking significantly. Both the type of alkali-metal ions and the concentration of alkaline solution influenced the catalytic performance, which were found to correlate to the acidity and textual properties. The optimum reaction result (97.3% yield of furfuryl alcohol at 99.6% conversion of furfural) can be obtained on 0.025 M-Na+-Zr-Al-Beta with high tolerance to the furfural concentration. [ABSTRACT FROM AUTHOR]