A detailed study of the production of polysaccharide aerogel (bio-aerogel) particles from lab to pilot scale is surveyed in this article. An introduction to various droplets techniques available in the market is given and compared with the lab scale production of droplets using pipettes and syringes. An overview of the mechanisms of gelation of polysaccharide solutions together with non-solvent induced phase separation option is then discussed in the view of making wet particles. The main steps of particle recovery and solvent exchange are briefly described in order to pass through the final drying process. Various drying processes are overviewed and the importance of supercritical drying is highlighted. In addition, we present the characterization techniques to analyse the morphology and properties of the aerogels. The case studies of bio-aerogel (agar, alginate, cellulose, chitin, κ-carrageenan, pectin and starch) particles are reviewed. Potential applications of polysaccharide aerogel particles are briefly given. Finally, the conclusions summarize the prospects of the potential scale-up methods for producing bio-aerogel particles.

The production of porous materials based on starch has been explored with supercritical drying—yielding aerogel—and freeze-drying. The two drying procedures were applied on the same gelling solution of amylomaize starch pasted at 140 °C and for two concentrations (5 and 10 wt.%). After gelation and retrogradation, water from the samples to be supercritically dried was exchanged to ethanol. The resulting starch aerogel presented high specific surface area (197 m²/g). Freeze-drying was assessed by investigating the effect of the gelation, retrogradation, freezing temperature, and sublimation pressure. The resulting starch materials were macroporous, with limited specific surface area and limited mechanical integrity. Cohesive open cell foam with pore size of ~20 µm was produced by quenching the hot starch melt in liquid nitrogen. The highest specific surface area obtained with freeze-drying was 7.7 m²/g for the hot starch melt frozen at −20 °C.

Pea and amylomaize starches were used to produce aerogel in form of monoliths and microparticles. The formation of starch gel was investigated, and we showed that each starch needed a different pasting temperature for its complete dissolution. The gelation kinetics was investigated with oscillatory rheometry for both systems as a function of the starch concentration. The gelation and retrogradation temperature of the starch gel were varied and its impact on the final aerogel evaluated. The emulsion gelation was carried out batch wise in a stirred vessel with different impeller geometries, concentrations of surfactant (Span80 and PGPR) and stirring rates. A particle size prediction approach based on idealized flow (Couette, 2D hyperbolic and turbulent) during the emulsification was proposed. A semi-continuous set-up for the emulsion gelation was developed in which the emulsification occurs in a single pass through a colloid mill and the gelation is triggered in-line with a counter-current heat exchanger.

In this work, the ability of several solvents to induce gel formation from amylomaize starch solubilized in dimethyl sulfoxide (DMSO) was investigated. The formed gels were subjected to solvent exchange using ethanol and dried with supercritical carbon dioxide (sc-CO₂) to obtain the aerogels. The influence of starch concentration (3–15 wt%) and solvent content (20–80 wt%) on gel formation was also studied. It was demonstrated that the gelation of starch in binary mixtures of solvents can be rationalized by Hansen Solubility Parameters (HSP) revealing a crucial hole of hydrogen bonding for the gel’s strength, which is in agreement with rheological measurements. Only the addition of water or propylene glycol to starch/DMSO solutions resulted in strong gels at a minimum starch and solvent content of 7.5 wt% and 50 wt%, respectively. The resulting aerogels showed comparably high specific surface areas (78–144 m² g⁻¹) and low envelope densities (0.097–0.203 g cm⁻³). The results of this work indicate that the HSP parameters could be used as a tool to guide the rational selection of water-free gelation in starch/DMSO systems. In addition, it opens up an attractive opportunity to perform starch gelation in those solvents that are miscible with sc-CO₂, avoiding the time-consuming step of solvent exchange.