Rapid and high efficient synthesis of carbon dots is crucial problem for scalable synthesis and practical biomedical or environmental application. However, synthesis of carbon dots still has the challenges, such as long reaction time of hydrothermal carbonization and low synthetic yield of rapid microwave carbonization. To develop rapid and high-yield synthesis of carbon dots, we proposed acrylamide/chitosan boost the synthetic yield of carbon dots via microwave-hydrothermal carbonization. The reaction time and synthesis yield were 30 min and 45.9%, respectively. As increasing of the carbon-carbon double bonds content, the synthetic yield of carbon dots (45.9%) was improved 5.85 and 4.53 times higher than carbon dots derived from chitosan or acrylamide, respectively. Carbon dots with amino and carboxylic groups exhibited the chelating ability benefiting for detection of ferrous ions, and the detection limit for ferrous ions was as low as 160 nM with the concentration range of 0-50 mu M. Rapid and high yield synthesis carbon dots derived from acrylamide/chitosan provides carbonaceous probe with chelating ability for detection of ferrous ions sensitively and specifically.