A promising strategy to design crosslinked photoluminescent hydrogel (PL hydrogel) is to synthesize the covalently bonded polymer chains by thermal polymerization. A proper ratio of methacrylic acid and m-phenylenediamine was used to prepare the PL hydrogel, and doping with graphene oxide and carboxymethyl chitosan improves the structure of the gel. The green and efficient hydrothermal synthesis realized a high polymerization and a short reaction time. Meanwhile, a series of properties were investigated for several combinations of hydrogels. Ultraviolet spectra, fluorescence spectra, and particle size distributions were used to characterize the PL composites. Scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, thermogravimetric analysis, rheological studies, and stress-strain tests were conducted to characterize the morphology, structure, and performance of the compound hydrogel. The adsorption properties of the PL hydrogel were characterized in adsorption tests. The results indicated that the PL hydrogel exhibited a favorable luminescence property, a certain degree of mechanical strength, and good adsorption performance. The prepared PL hydrogel has potential applications in adsorption and visual detection. V C 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018, 135, 46354.