Covalent Organic Frameworks (COFs) exhibit a range of exceptional attributes, including notable porosity, outstanding stability, and a precisely tuned π-conjugated network, rendering them highly promising candidates for fluorescence sensors applications. In this study, the synthesis of two emissive hydrazone-linked COFs designed for hydrazine detection is presented. The partially conjugated structure of the hydrazone linkage effectively weakens the fluorescence quenching processes induced by aggregation. Additionally, the incorporation of flexible structural components further reduces conjugation, thereby enhancing luminescent efficiency. Remarkably, these COFs possess a significant abundance of heteroatoms, enabling distinctive interactions with hydrazine molecules, which in turn results in exceptional selectivity and sensitivity for hydrazine detection. The detection limit of these COFs reaches the nanomolar range, surpassing all previously reported COFs, thereby underscoring their superior performance in chemical sensing applications.