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Thermal conductivity of the pyrolysis layer and the thermogravimetry data.Thermal conductivity of the pyrolysis layer in the charring material is of great importance for the optimal design of thermal protection system (TPS) in reentry vehicles. A method based on the thermogravimetry data of the charring material is presented to predict the thermal conductivity of the pyrolysis layer and the distribution of thermal conductivity of the pyrolysis layer is estimated. In addition, in order to validate the accuracy of this method, thermal response of the charring material is calculated with the predicted thermal conductivity and compared with the experimental data. The simulation results agree with the measured data and the numerical results indicate that taking this method to calculate the thermal conductivity of the pyrolysis layer is more compatible with the actual situation. This study is helpful to the optimization of the TPS. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019, 136, 48346.