In this work, we investigated the morphology and crystallinity changes of a β-ketoenamine COF, Tp-BD(Me)2 (Tp=1,3,5-triformylphloroglucinol, BD(Me)2=3,3′-dimethyl-[1,1′-biphenyl]-4,4′-diamine), with different reaction time and temperatures. Powder X-ray diffraction (PXRD) and Fourier-transform infrared (FTIR) spectra tests confirmed the synthesis of Tp-BD(Me)2, which has a specific β-ketoenamine linkage and a probable eclipsed stacking mode. At a reaction temperature of 50∘C, the morphology of Tp-BD(Me)2 underwent a progressive process of growing, extending and splitting. The band gaps of the Tp-BD(Me)2 obtained with the reaction time of 18–24 h were calculated near 2.0 eV. The BET surface areas of the Tp-BD(Me)2 were around 400–600 m2/g. It is not an optimal choice if the reaction temperature is below 50∘C, which could cause a low crystallinity and disordered morphology. However, slightly improving the reaction temperature to 60∘C is beneficial for generating high-crystallinity Tp-BD(Me)2.