In this paper, polyepichlorohydrin (PECH) quaternized with Nmethylimidazole (ImPECH) was successfully synthesized. ImPECH, polyvinyl alcohol, and tetraethyl orthosilicate were used to prepare anion exchange membranes that possessed a semi-interpenetrating polymer-network structure. These membranes were designed for acid recovery by diffusion dialysis (DD). The successful synthesis of ImPECH was verified via Fourier transform infrared spectroscopy (FTIR) and 1 H NMR spectroscopy. Meanwhile, the prepared anion exchange membranes were characterized by FTIR, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis (TGA). In addition, the ion exchange capacity (IEC), water uptake (W R ), tensile strength (TS), linear expansion rate (LER), and elongation at break (E b ) of each membrane were characterized. In DD application tests, acid dialysis coefficients (U H + ) of the membranes ranged from 8.56 × 10 −3 m/h to 27.33 × 10 −3 m/h and separation factor (S) values were all above 22.55. These results showed that anion exchange membranes had higher U H + and S values than commercial membrane DF-120 (U H + is 9.00 × 10 −3 m/h and S is 18.00) and other better general properties including the LER, TGA, TS, and so on. The prepared membranes showed a wide application prospective for acid recovery via DD.