CO2 mineralization is a promising method for the resource utilization of low-grade limestone and calcium-containing solid waste. Therein, adopting the acetic acid medium to achieve indirect mineral carbonation process to fixing CO2 is considered as an innovative and environmentally sustainable method owing to the reusability of the acetic acid medium. Nevertheless, the conversion efficiency of carbonation in this technique remains limited, with less than 20% efficiency at pressure of 5 MPa. Even with the addition of an extractant for acetic acid, the conversion efficiency of carbonation is still below 30%, significantly impeding the industrial applicability of this technology. In order to address the low conversion efficiency of carbonation in the acetic acid system, this study developed a new method for the preparation of calcium carbonate nanoparticles by microbubble-enhanced carbonation. The impacts of various factors such as medium calcium concentration, reaction temperature, reaction time, the value of pH, and aperture size of aerator on the efficiency of the carbonation reaction were systematically investigated. The results showed that: (1) Under optimal conditions (reaction time of 1 hour, reaction temperature of 80℃, initial pH of 7.2, initial calcium content of 70.07 g/L, and aperture size of aerator of 0.22 μm), the conversion rate of carbonation can reach 19.17% under atmospheric pressure, equivalent to the conversion rate achieved under 3 MPa. Meanwhile the regeneration cycle of the acetic acid medium can avoid wastewater generation at the source. (2) By integrating tributyl phosphate (TBP) with microbubble technology, the conversion efficiency of carbonation was improved to 57.5%, marking a 13.4 percentage point improvement over the reported pressurized extraction process. (3) At atmospheric pressure, rod-like aragonite nano-calcium carbonate products were synthesized with length of 400~800 nm and width less than 100 nm.