## 3 Results and Discussion  
### SAS1 and SAS2 Experiments  
This study was focused on the variation of the CO\({}_{2}\) flow rate and how the two configurations (SAS1 and SAS2) affected the deposition (see Supplementary Materials). The results of experiments 1-4, in which the co-precipitates are CAP/Q, are provided in Table 1. In these experiments a pressure of 90 bar, a temperature of 313 K, and a constant dissolution rate of 6 mL/min were fixed for all experiments, the CO\({}_{2}\) flow rate varied from 10 to 30 g/min, and the appropriate SAS process configuration. The results measured at the bottom of the precipitation vessel in the experiments are provided in Figure 3. It can be observed that in experiments 1, 3, and 4 there was precipitation on the bottom of the vessel, on the wall, and on the nozzle. However, in experiment 2 there was only precipitation on the wall of the vessel. It is important to note that the silica particles were located on the bottom of the vessel. In these experiments, the bottom of the vessel appeared wet with residual organic solvent. This observation could be due to the fact that the experiments were carried out very close to the MCP, which for DMSO/acetone/CO\({}_{2}\) are 79.7 bar at 313 K and 89.6 bar at 323 K, [35,36] and for ethanol/CO\({}_{2}\) are 79.4 bar at 313.4 K and 89.8 bar at 322.5 K [37]. This situation would cause a subcritical process that cannot remove all of the organic co-solvent. In the experiments carried out with a higher flow rate of CO\({}_{2}\) (exp. 1 and 3), the bottom of the vessel was covered with a large quantity of particles--more than in exp. 2 and 4. This could be caused by an increase in the turbulence near to the jet generating a higher supersaturation [39] and providing a higher efficiency in the micromization. The SEM images for experiments 1-4 (Figure 4) did not show the presence of silica particles, which are spherical particles of around 3-8 \(\upmu\)m (as provided by the manufacturer, the Miyoshi laboratory) [13]. The spherical particles correspond to the precipitation of CAP and the rectangular sticks were identified as precipitated Q. The images of the precipitates on the bottom of the vessel in deposition experiments 5 and 6 are shown in Figure 3 and these correspond to CAP/MNG co-precipitates. It can be observed that almost all compounds were deposited on the bottom of the vessel to form a \"body-mass\". The SEM images of these \"body-mass\" solids (Figure 5) for both configurations showed the presence of silica particles and CAP/MNG co-precipitates. In this case, a slight variation in the morphologies of the particles between SAS1 and SAS2, as observed in a previous study [34], was found. SAS2 co-precipitate particles (exp. 5) showed two different morphologies (quasi-spherical and sticks) against one morphology (quasi-spherical) for the particles observed for co-precipitates with SAS1. It is remarkable that the micromization of MNG also led to quasi-spherical particles and the raw MNG particles are sticks [26]. It can be argued that with the double injection the amorphization of the MNG did not occur and particles similar to the raw material, i.e., with some degree of crystallinity, were formed. In these experiments one could observe the difference between the silica particles, which are spherical particles of 3-8 um, and the spherical particles and sticks corresponding to co-precipitated CAP/MNG, which were smaller. Figure 4: SEM images for deposition experiments 1–4. Figure 3: Deposition images of the bottom of the precipitator vessel, experiments 1–8. Finally, experiments 7 and 8 were carried on the CAP/Q co-precipitates under the same conditions as experiments 5 and 6 due to the successful results obtained with these conditions. In this case, the increase in the pressure from 90-180 bar avoided the possible complications related to being in subcritical conditions and the CO\({}_{2}\) flow rate was fixed at 30 g/min.