During the production of paper pulp, the waste water loaded with organic materials from pulping process is discharged. Therefore, water treatment should be performed before disposing of such effluent. The use of such effluent for production of activated carbon will be effective in omitting the wastewater treatment and in obtaining the product required in many industries. In this respect, this paper deals with evaluating the performance of activated carbons (ACs) produced from black liquors (BLs) as by-products from three pulping processes of rice straw (RS) and sugar-cane bagasse (SCB), namely: alkaline, sulfite and neutral sulfite, which are coded SP, SSP and NSP, respectively. Elemental analysis and thermal analysis (TGA and DTGA) are carried out on the BLs, while the surface area (
S
BET
), micro-/mesoporous distribution, adsorption capacity of methylene blue (MB) and iodine (I
2
-value), as well as Fourier transform infrared spectra (FT-IR) and scanning electron micrograph (SEM) are studied on synthesizing ACs. The optimal pulping approach for achieving BL-based AC, with the following characteristics: specific surface area (
S
BET
) ∼ 921 and 545 m
2
g
−1
, MB adsorption capacity 238 and 370 mg g
−1
, and I
2
-value 928 and 1255 mg g
−1
of BL-based ACs, are from neutral sulfite pulping of SCB (B-NSP) and RS (RS-NSP), respectively. These finding data are ascribed to the carbon content of BL, as well as greatest total volume (
V
T
0.786 and 0.701 cm
3
g
−1
) together with decreasing the volume of micropores/total (38 and 48%) of BL-NSP-ACs. It is interesting to note that the AC provided from RS-NSP has greater adsorption capacity for I
2
and MB than the AC produced from RS-pulp fibres.