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A thermal protection material (TPM) was prepared using Al2O3-phosphate, expanded aluminosilicate, and phenolics through compression molding and the gradient heating reaction technique, and the effect of the high-temperature treatment on the properties of the composites were investigated. Scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy were used to analyze the structures and compositions of the composites. After the high-temperature treatment, the composites exhibited increased porosity, decreased density, and generated SiC particles with high strength and temperature resistance. The prepared composites have high compressive strength and compression deformation ability of the bending point. Thermogravimetric analysis, coefficient of thermal conductivity measurements, and expansion analysis were carried out to evaluate the thermal properties of the composites, and the effects of the preparation conditions on the thermal properties of the composites were investigated. The results showed that the prepared composites exhibited complete morphology, excellent high-temperature resistance, high compressive strength and toughness, and low thermal conductivity before and after the high-temperature treatment at 1000 °C, and hence showed great potential for future thermal protection applications.