The invention discloses a preparation method of a conjugated carboxylate negative electrode material of a lithium ion battery. The method comprises the steps of enabling [2, 2': 6', 2''- terpyridine]-4, 4', 4''-tricarboxylic acid and alkali to be subjected to a neutralization reaction to synthesize [2, 2': 6', 2''- terpyridine]-4, 4', 4''-lithium tricarboxylate; reacting with nitrates corresponding to fourth periodic element metals cobalt, nickel, copper and zinc at a temperature of 60 DEG C for 5 hours to synthesize [2, 2': 6', 2''- terpyridine]-4, 4', 4''-tricarboxylate; and grinding the synthetic material, acetylene black, and polyvinylidene fluoride in N-methyl pyrrolidone, coating the mixture on a copper foil, drying the coated copper foil, cutting the dried copper foil into pieces, manufacturing button cells in a glove box, and carrying out electrochemical performance characterization. The conjugated carboxylate synthesized according to the method provided by the invention contains multiple discharge sites such as a valence-variable metal center and carboxylate radicals; the conjugated carboxylate synthesized according to the method can make good use of a synergistic lithiumstorage effect among the carboxylate, a conjugated aromatic system and variable-valence metal, and the electrochemical performance of the material is improved. It is found that the material has relatively high specific discharge capacity and excellent cycle performance through a constant current charge-discharge test.