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Walnut shell biochar (WSC) and wood powder biochar (WPC) prepared using the limited oxygen pyrolysis process were used as raw materials, and ZnCl2, KOH, H2SO4, and H3PO4 were used to modify them. The evaluation of the liquid-phase adsorption performance using methylene blue (MB) as a pigment model showed that modified biochar prepared from both biomasses had a mesoporous structure, and the pore size of WSC was larger than that of WPC. However, the alkaline modified was more conducive to the formation of pores in the biomass-modified biochar materials; KOH treatment resulted in the highest modified biochar-specific surface area. The isothermal adsorption of MB by the two biomass pyrolysis charcoals conformed to the Freundlich equation, and the adsorption process conformed to the quasi-second-order kinetic equation, which is mainly physical adsorption. The large number of oxygen-containing functional groups on the particle surface provided more adsorption sites for MB adsorption, which was beneficial to the adsorption reactions. The adsorption effects of woody biomass were obviously higher than that of shell biomass, and the adsorption capacities of the two raw materials’ pyrolysis charcoal were in the order of WPC > WSC. The adsorption effects of different treatment reagents on MB were in the order ZnCl2 > KOH > H3PO4 > H2SO4. The maximum adsorption capacities of the two biomass treatments were 850.9 mg/g for WPC with ZnCl2 treatment and 701.3 mg/g for WSC with KOH treatment.