A good method of synthesizing Ti3C2Tx (MXene) is critical for ensuring its success in practical applications, e.g., electromagnetic interference shielding, electrochemical energy storage, catalysis, sensors, and biomedicine. The main concerns focus on the moderation of the approach, yield, and product quality. Herein, a modified approach, organic solvent-assisted intercalation and collection, was developed to prepare Ti3C2Tx flakes. The new approach simultaneously solves all the concerns, featuring a low requirement for facility (centrifugation speed < 4000 rpm in whole process), gram-level preparation with remarkable yield (46.3%), a good electrical conductivity (8672 S cm−1), an outstanding capacitive performance (352 F g−1), and easy control over the dimension of Ti3C2Tx flakes (0.47–4.60 μm2). This approach not only gives a superb example for the synthesis of other MXene materials in laboratory, but sheds new light for the future mass production of Ti3C2Tx MXene.