Abstract: Using dodecyl amine (DDA) as template agent, hexagonal mesoporous silica molecular sieve containing DDA(HMS-DDA) was successfully synthesized by sol-gel method at room temperature. Then the effects of calcination and solvent-extraction, especially the solvents and extraction time on the structure of HMS in the course of extracting or calcining DDA from HMS-DDA were investigated. Characterization of the mesoporous silica materials was carried out by means of FT - IR, XRD, HRTEM, XPS and TG - DTA. The experimental results showed that the calcination temperature, extraction time and solvents had great effects on the crystal lattice recombination, mesoporous degree and framework stability of HMS. The HMS material had higher mesoporous ordered degree and the most stable mesoporous structure when HMS - DDA was extracted with acetone for 9 hours. In addition, the S° I° molecule self-assembly mechanism of HMS - DDA was confirmed.