In this study, MCM-41 was synthesized by hydrothermal method, using non-toxic sodium metasilicate nonahydrate as the silicon source, cetyl trimethyl ammonium bromide (CTAB) as template, and sulfuric acid as the pH value adjustment agent. The effects of ratio of template agent to silicon source, pH value, crystallization temperature and crystallization time on the yield and crystallization of MCM-41 were investigated. MCM-41 was then characterized by XRD, FTIR, SEM, TEM and N2 adsorption-desorption testing techniques. Rhodamine B adsorption studies were carried out to study the effects of pH value and reaction time on the adsorption properties of MCM-41. The resulting MCM-41 had smooth surface with a pore size of 3-4nm and an average diameter particle of about 5μm. It had high specific surface area up to 784m2/g, thus adsorption rate of MCM-41 for rhodamine B obtained 93% when pH=3, t=15min. The reaction fitting curve of the Lagergren first order reaction model was lg (qe-qt) =-0.00586-0.803t, R2 = 0.97582.