In this work, the AC loaded Ti3+ self-doped TiO2 composite material was synthesized by the microwave method. Through XRD, XPS, SEM, RT-IR, UV-vis and other characterization methods to analyze the crystallinity, valence, morphology and other properties of the composite material. There is a synergistic effect between AC and TiO2, C—O—Ti and O—Ti—C bonds are formed between them. And promote the formation of anatase, make TiO2 form a mixed crystal form, and improve the efficiency of electron-hole separation. The doping of Ti3+ produces the Jahn-Teller effect, which reduces the band gap energy of the composite material to 2.2~2.4eV. The adsorption-catalysis experiment showed that the TiO2/Ti3+/AC composite prepared under microwave conditions has a removal rate of more than 96% for Rh-B, and the removal rate of pure TiO2/Ti3+ is only 50.44%. In addition, the effects of different preparation methods on the removal rate of Rh-B were compared. And it was found that the maximum removal rate of composite materials prepared under conventional conditions was 90.58%, which was significantly lower than the efficiency under microwave conditions. At the same time, the change in the adsorption capacity of AC was explored, and it was found that the saturated adsorption capacity of the 283K composite material was 161.67mg/g. When the temperature was 323K, the maximum adsorption capacity was 250.93mg/g, and the pure AC was only 115.47mg/g. Therefore, the composite material prepared by the microwave method can be regarded as an efficient and economical material for wastewater treatment.