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The photocatalytic degradation of organic dyes in waste water using carbon quantum dots (CQDs) remains a hot topic due to the importance of environmental protection. However, identifying suitable carbon resources and successful surface modification are still challenging. Herein, the hydrothermal method and surface modification of ammonia and thionyl chloride were applied to synthesize CQDs with different surface groups using PEO₁₀₆PPO₇₀PEO₁₀₆ (Pluronic F127) as a carbon source. The average particle size of the as-prepared CQDs was in the range of 2.3–3.5 nm. The unmodified CQDs had the highest relative photoluminescence intensity, while all as-prepared CQDs exhibited abnormal photoluminescence located outside the scope of the visible spectrum. Interestingly, CQDs modified with ammonia achieved a degradation rate of 99.13% (15 d) for 50 mg/L indigo carmine solution, while CQDs modified with thionyl chloride reached a degradation rate of 97.59% (15 d) for light green SF yellowish solution. Therefore, in this work, two typical organic dyes can be effectively photocatalytically degraded by as-prepared CQDs, with suitable surface modification.