The reaction kinetics of synthesis of tetraacetylhexaazaisowurtzitane (TAIW) by hydrogenolysis debenzylation of tetraacetyldibenzylhexaazaisowurtzitane (TADB) was investigated,using Pd/C as catalyst in an atmosphere of hydrogen. Results show that the reaction is the first-order to TADB during the stage from the beginning to the moment when about 90% H₂ is absorbed under the experimental conditions. When the solvent is acetic acid mixture,the apparent activation energy and pre-exponential factor of this reaction are 45.63 kJ·mol^-1 and 10^6.04 min^-1,respectively. While for acetic acid,they are 79.90 kJ·mol^-1 and 10^9.93 min^-1,respectively.