Beta zeolite was prepared via hydrothermal method using cheap diatomite and sodium meta-aluminate as raw material. The acidity and pore structure of the zeolite were adjusted by soft template method, organic alkali (urea) treatment and inorganic alkali (NaOH) treatment to synthesize multi-stage hole Beta molecular sieve, and bimetallic-loaded Beta zeolite catalyst (NiMo/Beta) was prepared by loading non-noble metals Ni and Mo via ultrasound-assisted impregnation method. The crystal structure, micromorphology, pore structure, acidity and metal reducibility of the catalyst were comprehensively characterized by XRD, SEM, N2 adsorption-desorption, NH3-TPD and H2-TPR. The effects of modified treatment methods and process conditions (reaction temperature, reaction H2 pressure, solvent n-dodecane amount, reaction time) on the catalyst"s catalytic performance in the hydrodeoxygenation of guaiacol were investigated. The results showed that under the conditions of 300 ℃, H2 pressure 4 MPa, reaction time 3 h and solvent n-dodecane 20 mL, the NiMo/Beta-3.0CB modified with 3.0 g CTAB in 6.0 g diatomite exhibited the best catalytic activity, and the conversion of guaiacol was 99.8%，the selectivity of cyclohexane was 92.7%; and after three times of recycling of the NiMo/Beta-3.0CB, the conversion of guaiacol was 85.7%.