2D materials show outstanding properties that can bring many applications in different technological fields. However, their uses are still limited by production methods. In this context, antimonene is recently suggested as a new 2D material to fabricate different (opto)electronic devices, among other potential applications. This work focuses on optimizing the synthetic parameters to produce high‐quality antimonene hexagons and their implementation in a large‐scale manufacturing procedure. By means of a continuous‐flow synthesis, few‐layer antimonene hexagons with ultra‐large lateral dimensions (up to several microns) and a few nanometers thick are isolated. The suitable chemical post‐treatment of these nanolayers with chloroform gives rise to antimonene surfaces showing low oxidation that can be easily contacted with microelectrodes. Therefore, the reported procedure offers a way to solve two critical problems for using antimonene in many applications: large‐scale preparation of high‐quality antimonene and the ability to set electrical contacts useful for device fabrication. A continuous‐flow synthesis approach offers large‐scale preparation of high‐quality few‐layer antimonene (FLA) hexagons. This procedure is based on colloidal synthesis followed by a post‐treatment with chloroform to isolate FLA hexagons which present ultra‐large lateral dimensions and a few nanometers thickness. Mechanical and electrical analyses reveal their high‐quality and low surface oxidation, opening the door for applications in electronics and beyond.