Abstract: Hexadecanol-palmitic acid-lauric acid/SiO₂ composite materials can be prepared by sol-gel method. The effect of absolute alcohol amount, deionized water amount and hexadecanol-palmitic acid-lauric acid amount on heat & moisture comprehensive property of hexadecanol-palmitic acid-lauric acid/SiO₂ composites, and the preparation technology parameters for hexadecanol-palmitic acid-lauric acid/SiO₂ composite materials was optimized. The results show that primary and secondary sequence of factors is the effect of absolute alcohol amount is obviously more significant than that of hexadecanol-palmitic acid-lauric acid amount, and the effect of hexadecanol-palmitic acid-lauric acid amount more significant than that of deionized water amount. Within the ranges of parameters in this study, absolute alcohol amount (mole ratio to tetraethyl orthosilicate) is 9.11, deionized water amount is 5.21 and hexadecanol-palmitic acid-lauric acid amount is 0.52. Hexadecanol-palmitic acid-lauric acid/SiO₂ composite materials have the best heat-moisture comprehensive performance in the range of human comfort, i.e. average equilibrium moisture content is 0.102 0 g/g in relative humidity 50%, phase change temperature is 26.81-28.52℃, phase change enthalpy is 95.69 J/g, and belong to micron organic phase change core materials/inorganic substrate composite materials.