The invention discloses a process for activating a Haemophilus influenzae type b (Hib) polysaccharide conjugate vaccine, which comprises the following steps of: A, preparing Hib polysaccharide; B, dissolving 1-Cyano-4-dimethylaminopyridinium tetrafluoroborate (CDAP) by using acetonitrile into a solution; C, preparing the Hib polysaccharide into a solution; D, adding the CDAP solution to the Hib polysaccharide solution, and stirring for 2-5 minutes at the room temperature; E, dissolving adipic dihydrazide (ADH) by using NaHCO3 into a solution, adding the ADH solution to a mixed solution, and stirring for 0.5-2 hours at the room temperature; and F, collecting eluent of the void volume from a loading solution after the reaction is ended at a SephadexG-25 gel chromatography column balanced in advance by water for injection, and performing freeze drying to obtain a Hib polysaccharide-ADH derivative. The process for activating the Hib polysaccharide conjugate vaccine has the beneficial effects that the quality index of the prepared Hib polysaccharide-ADH can reach the industrial standard, and moreover, the safe and nontoxic CDAP is adopted to serve as an activating agent instead of cyanogen bromide which is greatly harmful to human and environment, and therefore, the safety is enhanced, and the harm to the human and the environment are avoided.