The invention relates to a pH (Potential of Hydrogen) responsive fluorescent carbon nanoparticle hybrid microgel and a preparation method thereof. The preparation method comprises the following steps: (1) weighing fluorescent carbon nanoparticles, using methylene dichloride to dissolve and prepare a fluorescent carbon nanoparticle solution, adding acyl chloride monomers, reacting for 10 h under room temperature, removing a reaction solvent, adding water, and drying through rotation; (2) weighing to obtain double-bonded fluorescent carbon nanoparticles, adding the double-bonded fluorescent carbon nanoparticles into distilled water, transferring the liquid into a reaction container, adding a cross-linking agent, sodium dodecyl sulfate and pH responsive polymer monomers after exhausting air, introducing nitrogen gas to exhaust the air, heating, and adding an initiating agent into a three-opening bottle after reaction liquid begins to backflow; (3) continuously introducing nitrogen gas and stirring, and carrying out a backflow reaction for 5-20 h at 50-90 DEG C; (4) filtering after cooling to room temperature, taking filter liquor, and placing the filter liquor in a dialysis bag for dialyzing for 48 h. The obtained product is free of biological toxicity, the grain diameter of the product is about 760 nm, fluorescent light has good pH responsiveness under the excitation of the same wavelength, and the product has a good application in the fields of drug release, pH sensing and catalysis.