Abstract: PVC disulfide (2SPVC) was synthesized by solution crosslink and its molecular structure was confirmed by infrared spectrum. 2SPVC’s specific area is 36.1 m2•g-1 tested by stand BET method, and granularity experiment gives out the particle size of d0.5 = 11.3 m. With SEM (Scanning Electron Microscope) experiment the surface morphology and particle shape of 2SPVC were observed. Cyclic voltammetry (scan rate: 0.5 mV•s-1) shows that 2SPVC experience an obvious S―S redox reaction in charge-discharge process. When 2SPVC was used as cathode material for secondary lithium battery in a 1 mol•L-1 solution of lithium bis(trifluoromethylsulfonyl) imide (Li(CF3SO2)2N) in a 5:45:50 volume ratio mixture of o-xylene (oxy), diglyme (DG) and dimethoxymethane (DME) at 30℃, the first discharge capacity of 2SPVC is about 400.3 mAh•g-1 which is very close to its theoretical value (410.5 mAh•g-1) at a constant discharge current of 15 mA•g-1. It can retain at about 346.1 mAh•g-1 of discharge capacity after 30 charge-discharge cycles. So 2SPVC is a very promising cathode candidate for rechargeable lithium batteries.