The invention relates to a preparation method of hollow superparamagnetic nanospheres. The preparation method comprises the following steps: (1) pretreating cellulose raw materials through alkali liquor, soaking in oxidizing salt solution, and then hydrolyzing to obtain carboxyl cellulose nanospheres; (2) dispersing the cellulose nanospheres into water, adding little organic solvent and uniformly stirring, then sequentially adding ferric salt and ferrous salt, dropping alkali to react, and collecting the product by a magnet, so as to obtain the superparamagnetic nanospheres; and (3) roasting the superparamagnetic nanospheres at high temperature under inert atmosphere, so as to obtain the hollow magnetic nanospheres. The preparation method is simple, convenient and green in preparation technology, free from expensive equipment, wide in source of raw materials for production, low in cost and easy for mass production; and the hollow magnetic nanospheres prepared by the preparation method are higher in superparamagnetic response, controllable in dimension and uniform in chemical components, and can be applied to the fields such as the sewage treatment filed, the catalysis field, the magnetofluid field, the microwave absorption filed, the drug carrier filed, the biological enzyme fixation field and the biosensor field.