Abstract: Ni-MOF-74 materials were prepared by hydrothermal synthesis. The pore structure, crystal morphology and thermal stability of the materials were characterized by full automatic surface area adsorbent apparatus, PXRD, scanning electron microscopy and synchronous thermal analyzer. The adsorption isotherms of CO, N₂, CH₄ and CO₂ on Ni-MOF-74 were determined by static adsorption method. The molding material of Ni-MOF-74 was prepared, and the changes of crystal structure and micro structure and the adsorption property for CO were studied. The results show that the specific surface area of the prepared Ni-MOF-74 material is as high as 1 212.61 m²/g, the pore size is mainly between 0.8-1.0 nm, the adsorption capacity of CO is much higher than that of N₂ and CH₄ under the same conditions, and it has good thermal stability. The adsorption force of CO by Ni-MOF-74 is significantly higher than that of N₂, CH₄ and CO₂. The number of complete crystals of Ni-MOF-74 in extrusion samples decreases significantly, and some of the microporous structures are destroyed, and the adsorption properties of CO decrease significantly after extrusion.