The invention discloses a titanium-silicon-carbon/ferrocobalt high-temperature resistant electromagnetic wave absorbent. The titanium-silicon-carbon/ferrocobalt high-temperature resistant electromagnetic wave absorbent is prepared from Ti3SiC2 and Co3Fe7 through compounding. The invention further discloses a preparation method of the electromagnetic wave absorbent. The preparation method comprises the steps: pretreating Ti3SiC2 powder; preparing a precursor solution; preparing titanium-silicon-carbon/cobalt ferrite precursor sol from the pretreated Ti3SiC2 powder and the precursor solution; drying the titanium-silicon-carbon/cobalt ferrite precursor sol, so as to obtain titanium-silicon-carbon/cobalt ferrite precursor xerogel; subjecting the titanium-silicon-carbon/cobalt ferrite precursor xerogel to a self-propagation combustion reaction, carrying out cooling, and carrying out pulverizing, so as to obtain titanium-silicon-carbon/cobalt ferrite powder; subjecting the titanium-silicon-carbon/cobalt ferrite powder to heat treatment in a reducing atmosphere, thereby obtaining the titanium-silicon-carbon/ferrocobalt dual-loss-type high-temperature resistant absorbent. The titanium-silicon-carbon/ferrocobalt electromagnetic wave absorbent disclosed by the invention simultaneously has the characteristics of dielectric loss and magnetic loss to electromagnetic waves. The preparation method disclosed by the invention is simple and easy to implement.