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In photocatalytic system, singlet oxygen can be generated based on the excitonic energy transfer process. Here, the 2D layered hallyosite (Hal) as a support hydroxyl group's substrate to anchor molybdenum trioxide (MoO_3-x) with oxygen vacancies (Hal/MoO_3-x) was prepared. Electron spin resonance and quenching experiments showed that the combination of Hal and MoO_3-x enhances the generation of singlet oxygen (¹O₂) and inhibits the production of other reactive oxygen species. Furthermore, photocatalytic molecular oxygen activation experiments were carried out to evaluation of ¹O₂ generation. Phosphorescence spectroscopy revealed improved triplet exciton production in the composite. The Hal/MoO_3-x shows great degradation response in TC removal. The value for the rate constant (k) of the composite was 0.0209 min⁻¹ under light irradiation, which is about 5.64 and 3.02 times larger than that of Hal …