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In this work, we report a stable g-C
3
N
4
, Bi
2
S
3
, and g-C
3
N
4
/Bi
2
S
3
composite catalysts were prepared via a facile one-pot microwave-assisted method and characterized. The orthorhombic phase and nearly spherical shape of the particles with an average diameter of 5-25 nm of g-C
3
N
4
/Bi
2
S
3
composite were obtained from XRD and TEM. The composite also exhibits a high surface area (32.15 m
2
/g), which may provide convenient transportation and diffusion for substrate molecule. The optical studies were displayed the g-C
3
N
4
/Bi
2
S
3
composite has a sharp absorption band in the visible region, higher charge separation, and reduced recombination rate. These results show that the Bi
2
S
3
NPs have good crystallinity and are uniformly deposited on the surface of the g-C
3
N
4
sheet. The catalytic performance of the g-C
3
N
4
/Bi
2
S
3
composite for the reduction of 4-NP to 4-AP was exhibited approximately 100%, which is 1.48 and 2.34 times higher than the Bi
2
S
3
and g-C
3
N
4
catalysts, respectively. The pseudo-first-order rate constant was estimated as 1.648 × 10
−2
min
−1
for the reduction of 4-NP using g-C
3
N
4
/Bi
2
S
3
composite in 1 h reaction time. The effect of catalyst dosage (0-30 mg) was also investigated for the reduction of 4-NP using g-C
3
N
4
/Bi
2
S
3
composite catalyst. Moreover, the reusability of the g-C
3
N
4
/Bi
2
S
3
composite was exhibited a better reduction of the 4-NP even after 5 cycles and it was found that 8% reduction in the initial reduction rate. The obtained results from this study show that g-C
3
N
4
/Bi
2
S
3
composite has the potential efficiency and stability to make it an ideal catalyst for the reduction of toxic effluents and wastewater treatment.