2-Ethyl hexanol and maleic anhydride were used to synthesis the mon-2-ethylhexyl maleate, then the mon-2-ethylhexyl maleate were reacted with calcium acetate (zinc acetate) to prepare the calcium(zinc) mon-2-ethylhexyl maleate. The mon-2-ethylhexyl maleate and the final productions verified by FTIR. The thermal stabilities of PVC in the presence of the calcium/zinc mon-2-ethylhexyl maleate were evaluated systematically by means of thermal aging oven test,Congo red test and conductivity test and thermogravimetric analysis(TGA), the mechanism of calcium/zinc mon-2-ethylhexyl maleate thermal stabilizer was investigated by testing the absorption of acid.And then the synergistic effects of layered double hydroxide(LDH) with Ca/Zn system were explored. When the mass fraction of metal ions of the calcium / zinc mon-2-ethylhexyl maleate compound heat stabilizer were 3% and 2%，respectively, the system exhibited the best thermal stability, which provided the initial whiteness time of 50 min and the static thermal stabilization time of 26 min. At the same time when added 0.08g hydrotalcite (LDH), the system’s thermal stability had improved significantly, whoes the static thermal stabilization time reached at 53.5min.