Methyl orange dye (MO) is one of the azo dyes, which is not only difficult to degrade but also hazardous to human health, therefore, it is necessary to develop an efficient photocatalyst to degrade MO. In this paper, a facile and low-cost elemental doping method was used for the surface modification of Ti3C2 MXene, i.e., nitrogen-doped titanium carbide was used as the nitrogen source, and the strategy of combining solvent heat treatment with non-in situ nitrogen doping was used to prepare N-Ti3C2 MXene two-dimensional nanomaterials with high catalytic activity. It was found that the catalytic efficiency of N-Ti3C2 MXene materials was enhanced and improved compared to the non-doped Ti3C2 MXene. In particular, N-Ti3C2 1:8 MXene showed the best photo-catalytic ability, as demonstrated by the fact that the N-Ti3C2 1:8 MXene material successfully degraded 98.73% of MO (20 mg/L) under UV lamp irradiation for 20 min, and its catalytic efficiency was about ten times that of Ti3C2 MXene, and the N-Ti3C2 photo-catalyst still showed good stability after four cycles. This work shows a simplified method for solvent heat-treating non-in situ nitrogen-doped Ti3C2 MXene, and also elaborates on the photo-catalytic mechanism of N-Ti3C2 MXene, showing that the high photo-catalytic effect of N-Ti3C2 MXene is due to the synergistic effect of its efficient charge transfer and surface-rich moieties. Therefore, N-Ti3C2 MXene has a good prospect as a photo-catalyst in the photocatalytic degradation of organic pollutants.