The invention relates to a preparation method of a 
carbon dioxide responded 
graphene nano hybrid material, which comprises the following steps of reacting 5,10,15,20-tetrakis(4-aminophenyl)-21H,23H-porphine with 1,1-dimethoxy-N,N-dimethylethylamine so as to obtain 5,10,15,20-tetrakis(4-phenyl-N,N-dimethyl-N''-acetamidine 
bicarbonate)-21H,23H-porphine; and then, adding 
grapheme, so that molecules of the 5,10,15,20-tetrakis(4-phenyl-N,N-dimethyl-N''-acetamidine 
bicarbonate)-21H,23H-porphine are coupled on the surface of the 
grapheme, and then a 
grapheme-5,10,15,20-tetrakis(4-phenyl-N,N-dimethyl-N''-acetamidine 
bicarbonate)-21H,23H-porphine 
nano hybrid material is formed. The grapheme 
hybrid material prepared according to the invention has 
carbon dioxide responsiveness, and the dispersion of the 
hybrid material in an 
aqueous solution can be reversibly regulated through feeding 
carbon dioxide or 
argon into the 
aqueous solution, and therefore, the 
hybrid material has wide applications in the fields of 
drug controlled release carriers, intelligent switches, intelligent sensors, biological nano-devices and the like. The preparation method disclosed by the invention is simple and practicable, and raw materials can be subjected to industrialized production, and therefore, the preparation method has good popularization and application values.