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Zeolite Fe-MFI was synthesized and applied as catalysts in the liquid-phase dehydration of 1-phenylethanol (PHE). The ferrum may influence the nucleation/crystallization processes, the crystal size is varied with the ferrum content. However, all the ferrum were incorporated into the framework when the Fe:Si = 0.005–0.025. In the PHE dehydration, the extra-framework ferrum is inactive. Nevertheless, the Fe-MFI is highly active, a PHE conversion of about 90% and a styrene selectivity >99% were achieved. The Fe-MFI with 1.5–1.8 mmol/g acid sites and Brönsted to Lewis in the 0.13–0.18 range is preferred. Moreover, the Fe-MFI could be reused for at least five times. [ABSTRACT FROM AUTHOR]