Mechanochemical synthesis of hydrotalcite and layered double hydroxides was conducted using a horizontal bead mill and passing a wet mixture of mixed metal hydroxides through the mill, followed by thermally ageing all milled material. Hydrotalcite-like layered double hydroxide was successfully synthesised and identified as a mixture of hydrotalcite and meixnerite. The final thermally aged material that was milled for three hours has a particle size distribution in the range 0.5 μm to 12 μm. XRD and FTIR both suggest that the synthesised material is phase-pure LDH but the amorphous halo present in the XRD results suggests that an amorphous compound is present as a contaminant. It is recommended that Mg-Al synthesis experiments be carried out for less than three hours to determine if a smaller particle size distribution and a more LDH-like morphology can be achieved after aging. The total LDH yield should be investigated with Rietveld refinement analysis after autoclaving to crystallise all materials. The optimisation of the Mg-Al mechanochemical synthesis should be investigated to determine if a phase-pure hydrotalcite can be synthesised at a lower cost than the current synthesis methods.