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Photocatalysis has been attracting much research interest because of its wide applications inrenewable energy and environmental remediation. As compared with other photoactive materials, titania attracts increasing attention of researchers owing to its relatively low cost, availability, stability, and functionality. However, the band gap for titania is 3.0–3.2 eV, and it absorbs only in the UV range. Therefore, the performance of titania based photocatalysts under sunlight is low. To increase the yield of the photocatalytic reaction products, separation of the oxidative and reductive sites at the catalyst surface is of crucial importance. Of special interest in this respect is the use of layered compounds, in particular, perovskite like titanates. In the present work, particles of nanocrystalline perovskite-like sodium neodymium titanate, photoactive not only in the UV but also in the visible range, were prepared through hydrothermal route, and their physicochemical and photocatalytic properties were studied in comparison with the sample synthesized by a solid phase method. It has been found that the photocatalytic decomposition of methylene blue in an aqueous solution over the perovskite-like sodium neodymium titanate synthesized by the hydrothermal method under visible light illumination occurs with a high rate (3.5 times higher than that TiO2 P25 Evonik Degussa sample, and 2 times higher than the sample synthesized by a solid phase method).