A set of organic bentonite preparation means different from traditional technology was proposed, and the COD (chemical oxygen demand) and XRD (X-ray diffraction) double indicators were used for the first time to measure the synthetic effect of organic bentonite. COD tests showed that the selection of the appropriate type and the amount of modifier made up two prerequisites for preparing organic bentonite used in organic wastewater treatment. As two kinds of modifiers, both solid di-octadecyl dimethyl ammonium chloride from Shanxi and solid esterquat from Henan were suitable for preparing organic bentonite used in organic wastewater treatment. XRD analysis demonstrated that the d001 value of montmorillonite mineral was increased from 1.251 nm to 3.373 nm after the modification of bentonite by di-octadecyl dimethyl ammonium chloride, whereas the d001 value of montmorillonite mineral was increased from 1.251 nm to 5.103 nm through the modification by esterquat. The d001 value of montmorillonite in the new preparation process of organic bentonite increased significantly, and long-chain molecules of organic modifier had been inserted between layers of montmorillonite minerals, which indicated that the synthetic effect was good. The new synthesis process of organic bentonite can eliminate the need for filtering, washing, drying, grinding and other steps, thus significantly reducing energy consumption and production cost, and can also effectively promote the larg-scale application of organic bentonite in the field of wastewater treatment.