Extraction and separation of nickel and cobalt from saprolite laterite ore were studied by using a method of microwave-assisted hydrothermal leaching and chemical deposition. The effects of leaching temperature and time on the extraction efficiencies of Ni2+ and Co2+ were investigated in detail under microwave conditions. It is shown that the extraction efficiencies of Ni2+ and Co2+ from the ore pre-roasted at 300 C for 5 h were 89.19% and 61.89% when the leaching temperature and time were about 70 C and 60 min, respectively. For the separation process of Ni and Co, the separation of main chemical components was performed by adjusting the pH values of sulfuric leaching solutions using a NaOH solution based on the different pH values of precipitation for metal hydroxides. The final separation efficiencies of Ni and Co were 77.29% and 65.87%, respectively. Furthermore, the separation efficiencies of Fe of 95.36% and Mg of 92.2% were also achieved at the same time. Extraction and separation of nickel and cobalt from saprolite laterite ore were studied by using a method of microwave-assisted hydrothermal leaching and chemical deposition. The effects of leaching temperature and time on the extraction efficiencies of Ni2 + and Co2 + were investigated in detail under microwave conditions. It is shown that the extraction efficiencies of Ni2 + and Co2 + from the ore pre-roasted at 300 C for 5 h were 89.19% and 61.89% when the leaching temperature and time were about 70 C and 60 min, respectively. For the separation process of Ni and Co, the separation of main chemical components was performed by adjusting the pH values ​​of sulfuric leaching solutions using a NaOH solution based on the different pH values ​​of precipitation for metal hydroxides. The final separation efficiencies of Ni and Co were 77.29% and 65.87 %, respectively. Furthermore, the separation efficiencies of Fe of 95.36% and Mg of 92.2% were also achieved at the same time.