A hybrid cyanate ester resin containing polysilazane was prepared via the prepolymerization of bisphenol-A dicyanate ester monomer (BADCy) in the presence of polysilazane (PSZ) under low temperature conditions in a short period of time. Fourier transform-infrared (FT-IR) spectroscopy and nuclear magnetic resonance (NMR) spectroscopy reveal that the polymerization reaction of BADCy can be carried out in the presence of PSZ to obtain a hybrid resin below 100°C and polymethylsilazane (PHS) exhibits an improved prepolymerization effect when compared to polydimethylsilazane (PMS). FT-IR spectroscopy and gel permeation chromatography (GPC) showed that the prepolymerization degree of the PHS/BADCy resin increased upon increasing PHS mass fraction from 0 to 12 wt%, polymerization temperature from 60 to 100°C and polymerization time from 0 to 4 h. The PHS/BADCy hybrid resins samples were prepared and their process properties were investigated by rheometry and Differential scanning calorimetry (DSC). The results indicated that their viscosity was <10 Pa.s in the temperature range of 60–130°C, and the initial curing temperature and curing exothermic enthalpy were 121.9°C and 358.9 J/g, respectively. Furthermore, the cured PHS/BADCy resin possesses excellent thermal and mechanical properties, the 5% weight loss temperature (Td5) and glass transition temperature (Tg) were 424–441°C and 273–282°C, respectively. The cured PHS/BADCy resin with 4 wt% PHS showed the highest flexural strength of 146 MPa and flexural modulus of 4.1 GPa.