Magnesium silicates combining acidic and basic surface properties are known to be interesting as heterogeneous catalysts. Nevertheless, their catalytic performances are highly dependent on the synthesis method used. In this study, a series of magnesium silicates was synthesized for the first time using a coprecipitation method with a micromixer. It is first shown that changes in synthesis/precipitation pH led to magnesium silicates with different Mg/Si ratios: the higher the synthesis pH, the higher the Mg/Si ratio. Moreover, prepared silicates with a final Mg/Si ratio greater than 0.7, thus prepared at high pH, exhibit negligible specific surface area, whereas relatively high values (>180 m2/g) have been obtained for lower Mg/Si ratios. A set of experimental characterization data obtained by N2 physisorption, SEM, XRD, TGA-DTA as well as Raman and 29Si NMR spectroscopies are presented and discussed. They show the existence of two distinct families with a similar Magnesium Silicate Hydrate (MSH) phase, but they reveal different aggregation states and textural properties. Finally, the surface acid–base reactivity of the co-precipitated magnesium silicates was determined using the model reaction of 2-methylbut-3-yn-2-ol (MBOH) conversion. The results obtained suggest that it is possible to prepare silicates with a wide range of surface acid–base properties, from purely basic solids to those with both acidic and basic properties, by adjusting the final Mg/Si ratio via the control of the synthesis parameters.