The curing reactions of novolac cyanate ester resin were studied by using FT-IR in situ technology.The relationship between the conversion rates of several groups in resin and curing time were obtained and the conversion of important groups during each curing period were analyzed in order to establish better curing parameters,and fixed on its curing parameters: 120 ℃2h +150 ℃2h + 180 ℃3h + 200 ℃2h + 250 ℃2h + 300 ℃2h.It is proved that its mechanical properties are correspond to the traditional phenolic resin,but have more excellent heat resistant property.