Titanium tetrachloride is produced through the chlorination of a variety of titanium bearing ores. The chlorination step can produce a variety of metal chloride impurities, such as iron chlorides and vanadium chlorides. The technological process of removal vanadium with copper wires is widely used in China. In the process of removal vanadium, a solid and liquid mixture will be discharged as waste. V–Cu residue is a kind of solid waste filtered from the solid and liquid mixture generated in the purification process. V–Cu residue samples from Zunyi, Guizhou, China, were investigated using X-ray fluorescence spectroscopy, inductively coupled plasma optical emission spectrometry, X-ray diffraction, and scanning electron microscope. The results showed that this waste residue contained Ti (29%), Cu (9.87%), Cl (8.83%), V (5.77%), and an amount of niobium and tantalum. Mainly mineral phases were composed of vanadium niobium oxides, titanium niobium oxides, titanium oxides, and eriochalcite. Ti and V mainly existed in the form of oxides, as dense clumps, and were accompanied by a small amount of Nb. Cu in the V–Cu residue mainly existed in the form of chlorides, adsorbing on the surface of the Ti–V–Nb oxides.