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In this paper, widely accepted methods of hydrotalcite preparation such as co-precipitation, urea hydrolysis, hydrothermal, sol-gel, microwave irradiation, steam activation and solvothermal have been selected and reviewed. Our review indicates that the nature of the divalent cations, the synthesis method, the calcination temperature and the nature of the interlayer species are determinant factors in shaping the surface properties of the layered double hydoxides. The basic strength of the surface base site and structural changes produced in the mixed oxides can be adjusted conveniently by varying the Al content during the synthesis. The combination of sol-gel with microwave irradiation during the gelling and crystallization steps has also been found to increase the surface area of the hydrotalcite-like compound.