The mesoporous TiN powder was prepared by non-hydrolyzed sol-gel method combined with ammonia gas reduction nitrification method using ethanol as oxygen donor, titanium tetrachloride (TiCl4) as titanium source and P123 as pore-forming agent. The effect of reduction nitride temperature on the phase, pore structure and electrochemical performance of mesoporous TiN powder was test by XRD, SEM, BET, XPS, CV, GDC and EIS. The results showed that as the reduction nitrification temperature increased, TiO2 was reduced TiO in the powder and then turned into TiN, and Ti-O bond was gradually replaced by Ti-N bond. In addition, the phase purity and particle size increased, and the pore diameter of the intermediate hole first increased and then decreased. When the reduction nitrification temperature is 800℃, the specific surface area of the powder is 41 m2/g, the pore structure is developed, and the average pore diameter is 24nm, which is conducive to ion transfer and electrochemical performance improvement. At this point, the internal impedance is 0.9 Ω. As the current density is 20 mA/g, the specific capacitance is 130 F/g. It is worth mentioning that after 1000 cycle also can keep the initial specific capacitance of nearly 90% under the 50 mA/g.