Under microwave irradiation the di-esters of lubricating oil are synthesized by the reaction of adipic acid or azelaic acid with 2-ethylhexyl alcohol or dodecanol. The results show that for catalyst amount of 3.0% ～3.5% and microwave power of 300 w～320 w the yields of di-(2-ethylhexyl)adipate and di-(2-ethylhexyl) azelate are respectively 99.4% and 98% for 12 min and 8 min, and the yields of didodecyl adipate and didodecyl azelate are respectively 97%and 95% for 6.5 min and 7.5 min. The experimental parameters of microwave synthesis for four di-esters are investigated. The chromaticity and crystallization point of di-esters are measured and their structures have been characterized by 1H NMR、13C NMR and IR spectra. Compared with conventional synthesis method, the microwave method can achieve excellent yield of 95%-～99.4% within 6.5 min -～12 min. The reaction time has a reduction by a factor of 7.1 to 11.4 and the yields of didodecyl adipate, didodecyl azelate, di-(2-ethylhexyl) adipate and di-(2-ethylhexyl) azelate are 3%, 6%, 11.5% and 29% higher than the conventional yields, respectively. Moreover, the color of products is colorless or white. Microwave synthesis method is a rapid, highly efficient and novel synthetic approach for lubrication oil di-esters.