An optical polythiourethane based on m-xylylene diisocyanate (XDI) and 4-mercaptomethyl-3,6-dithia-1,8-octanedithiol (BES) has been studied. Triethylamine was adopted as a catalyst, and the solid-state isothermal cure reaction was carried out using FTIR spectroscopy, in the temperature range of 75°C-105°C. The -NCO absorption band of XDI was used to monitor the conversion of diisocyanate into polythiourethane. The reaction rate enhanced with an increase in the content of the catalyst, and the gel time determined by swelling test was shorter for the system with higher catalyst content. Kinetic parameters were calculated from the infrared spectrum data, and the results showed that the curing reaction of polythiourethane accords with first-order kinetic characteristics. The activation parameters obtained from the evaluation of kinetic data were △H∗=97.22 kJ mol−1, △S∗=−6.77 J K−1 mol−1, and Ea=100.23 kJ mol−1. The observed negative entropy of activation value supported the formation of a transition state in the cure reaction.