The invention discloses a SnO2 / MoS2 two-dimensional macroporous composite material film as well as a preparation method and an application thereof, and belongs to the field of sensor material preparation. According to the invention,the preparation method comprises the following steps: soaking a PS template so that gaps among PS microspheres can be filled with a SnCl4. 5H2O solution, then annealing, gasifying the PS microspheres, and forming the SnO2 macroporous film; taking a PS template as a template, then carrying out hydrothermal reaction, introducing MoS2 nanosheets on the basis of keeping a regularly arranged SnO2 macroporous structure, and regulating to enable the PS template to pass through a SnO2 macroporous film to pass through a SnO2 / MoS2 macroporous film. According to the SnO2 / MoS2 two-dimensional macroporous composite film disclosed by the invention, the porous structure is beneficial to gas discharge, and the compounding of nanosheets enables the specific surface area of the film to be increased and the surface active sites to be increased, so that the gas-sensitive property is greatly improved, the gas-sensitive property is more excellent, and the SnO2 / MoS2 two-dimensional macroporous composite film has good gas-sensitive response to nitrogen dioxide gas.