A new nano-sized inorganic/organic (IO) hybrid material was synthesized by self-assembly of OSB-12 into layered aluminum silicate via a coprecipitation method. The process of the fabrication of hybrid material consisted of the following steps. Firstly, aluminum nitrate and OSB-12 were homogeneous mixed in the water. Thereafter, sodium silicate was slowly added in. Elemental analysis indicated that the combination ratio of aluminum silicate and OSB-12 was 2.2∶1. The hybrid was characterized by Zeta potential, Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscope (TEM) and surface area and porosity analyzer. The results showed that OSB-12 was inserted into the aluminum silicate layer in hydbrid material with lamellar and porous structure. Based on the amphiphilic characteristic of OSB-12, the resulted hybrid could be used as a sorbent to cationic and anionic dyes simultaneously. Meanwhile, the micron fiber contained hybrid and polyacrylonitrile (PAN) was also prepared by electrospinning, which can provide a convenient recycle of sorbent from water. Various factors affecting the adsorption were investigated. Under the optimum conditions, the maximum adsorption capacity was 471 mg/g of cationic (weak acid pink red B) and 847 mg/g of anionic dyes (victoria blue BO) respectively. The adsorptions process obeyed the Langmuir isothermal model and Frendlich isothermal model, because of the electric charge attraction playing a key role between ionic dye and OSB-12 embedding in the hybrid sorbent. The changes of Zeta potential of dye solution confirmed the point. In addition, the reused of the waste fiber was also been considered, the fiber was roasted in high temperature (600 ℃) to obtain a porous kaolin material which had tremendous adsorption capacity to heavy metal, the adsorption capacity was more than 8.3 mg/g of Cr 3+ . It can be predicted that the hybrid had a tremendous application potential in dye wastewater treatment from dye removal efficiency and material separation properties.