Using the SuperSolubilization Nanometer SelfAssembly method, bulk  N i - A l 2O3 catalyst is prepared with nickelnitratehexahydrate as the precursor and urea as precipitation agent, the mixture of the surfactantgather isobutylene maleic acid triethanolamine esters and petroleum hydrocarbon150SN as template agent. The  N i - A l 2O3  catalysts were characterized by TEM and TPR, and reaction mechanism of precipitation was studied. The results indicate that nanosized  N i - A l 2O3  bulk catalyst has a crystalline form with not only spherical shape，but also nanorod and nanometer silk, etc. Particles prepared by this method have good dispersion and uniform size, and narrow diameter distribution is observed between 10～50 nm. The N i - A l 2O3  reduced by hydrogen also has a crystalline form, and nanostructure of reduced  N i - A l 2O3  is more orderly than before. Particles size after reduction is still in the nanoparticles scope. TPR results show that there are two reduction peak appeared in the structure of nanometer bulk  N i - A l 2O3  catalyst,and the lowtemperature peak is NiO，high temperature reduction peak attributes to spinel structure which produced by the interaction of nickel and aluminum oxide.

Bulk NiAl2O3 catalysts was synthesized in the way of supersolubilization nanometer selfassembly. The bulk NiAl2O3 catalyst was characterized by Xray diffraction (XRD) and the mercury porosimeter. The influence of affecting factors on physical properties of catalysts was investigated, such as the amount of urea and surfactant, and the amount of nikel oxide. The results show that bulk NiAl2O3 catalysts has a better bore structure, which is made from based amount plus 2 of surfactants, based amount plus 5 of urea and plus 3 of NiO. Specific area of the bulk NiAl2O3 catalyst is between 186 m2/g to 324 m2/g, bore diameter is 3~12 nm, and the diameter of bore is even and distribute concentration, witch is belong to medium and big bore scope, the bore permits is 0.45~0.89 mL/g. This bulk catalyst is a more ideal bulk catalyst which can satisfy the request of hydrogenation. This synthesize method has more merits,such as decreasing the dosage of surfactant and aqueous, operation craft simple, reaction can be controlled easily.Nanometer bulk catalyst has a good application value in industrialize production because of its better property than the residue oil hydrogenation catalyst.