Recovery of lactose from simulated delactosed whey permeate by a low-temperature crystallization process.

Delactosed whey permeate is the mother liquor/by-product of lactose manufacture, but it still contains around 20 wt% lactose. The high mineral content, stickiness, and hygroscopic behavior prevent further recovery of lactose in the manufacturing process. Therefore, its use is currently limited to low-value applications such as cattle feed, and more often it is seen as waste. This study investigates a new separation technique operating at sub-zero conditions. At low temperature, precipitation of calcium phosphate is expected to be reduced and the lower solubility at sub-zero temperature makes it possible to recover a large portion of the lactose. We found that lactose could be crystallized at sub-zero conditions. The crystals had a tomahawk morphology and an average size of 23 and 31 µm. In the first 24 h, the amount of calcium phosphate precipitated was limited, whereas the lactose concentration was already close to saturation. The overall rate of crystallization was increased compared with the crystals recovered from a pure lactose solution. Mutarotation was rate limiting in the pure system but it did not limit the crystallization of lactose from delactosed whey permeate. This resulted in faster crystallization; after 24 h the yield was 85%.

Scaling up continuous eutectic freeze crystallization of lactose from whey permeate: A pilot plant study at sub-zero temperatures.

Eutectic freeze crystallization is explored as an alternative to the state-of-the-art evaporation process for the recovery of lactose from whey permeate. At the so-called eutectic freezing point, both water (the solvent) and lactose (the solute) crystallize and can be removed continuously while continuously feeding whey permeate. This continuous process is demonstrated on a pilot scale at sub-zero temperatures. In the first instance, only freeze concentration of whey permeate took place at -4 °C. It was possible to reach a lactose concentration of 30 wt% and hardly any nucleation was observed. The resulting ice had high purity, with a lactose concentration of ±2 wt%. Next, the eutectic phase was reached, and lactose and ice crystallized simultaneously and were continuously removed from the system, the resulting crystals had parallelogram morphology with an average size of 10 µm. Ice was recovered at a rate of 60 kg/h and lactose was recovered at a rate of 16 kg/h, yielding over 80% of the feed lactose. A conceptional design was proposed for an improved yield and reduction of energy. Yields of at least 80% and up till 95% could be achieved. Compared to the state-of-the-art mechanical vapor recompression (MVR), EFC is 80% more energy efficient.

Oil-in-water emulsions based on hydrophobic eutectic systems.

We demonstrate that oil-in-water emulsions can be prepared from hydrophobic eutectic systems (ES). Light microscopy and dynamic light scattering show that droplets are formed and zeta potential measurements indicate sufficient stability against coalescence. We investigate whether Ostwald ripening occurs in these ES-in-water emulsions by following the droplet growth over time and comparing it with an emulsion comprising decane in water. At first sight, the Ostwald ripening rate of the ES-in-water emulsion is expected to be orders of magnitude larger than the ripening of the decane-in-water emulsion due to a much higher solubility of the dispersed phase. However, experimentally we find that the ES-in-water emulsion actually grows a factor of two slower than the decane-in-water emulsion. We attribute this to the two-component nature of the ES, since the growth rate is mainly set by the least-soluble component of the ES. Thus, ESs offer the advantage of creating liquid emulsions of solid components, while setting the emulsion stability through their composition.

Ionic liquids and deep eutectic solvents in natural products research: mixtures of solids as extraction solvents.

Mixtures of solid chemicals may become liquid under certain conditions. These liquids are characterized by the formation of strong ionic (ionic liquids) or hydrogen bonds (deep eutectic solvents). Due to their extremely low vapor pressure, they are now widely used in polymer chemistry and synthetic organic chemistry, yet little attention has been paid to their use as extraction solvents of natural products. This review summarizes the preparation of ionic liquids and deep eutectic solvents with natural product components and recent progress in their applications to the extraction and analysis of natural products as well as the recovery of extracted compounds from their extracts. Additionally, various factors affecting extraction features of ionic liquids and deep eutectic solvents, as well as potential useful technologies including microwave and ultrasound to increase the extraction efficiency, are discussed.

Natural deep eutectic solvents as new potential media for green technology.

Developing new green solvents is one of the key subjects in Green Chemistry. Ionic liquids (ILs) and deep eutectic solvents, thus, have been paid great attention to replace current harsh organic solvents and have been applied to many chemical processing such as extraction and synthesis. However, current ionic liquids and deep eutectic solvents have still limitations to be applied to a real chemical industry due to toxicity against human and environment and high cost of ILs and solid state of most deep eutectic solvents at room temperature. Recently we discovered that many plant abundant primary metabolites changed their state from solid to liquid when they were mixed in proper ratio. This finding made us hypothesize that natural deep eutectic solvents (NADES) play a role as alternative media to water in living organisms and tested a wide range of natural products, which resulted in discovery of over 100 NADES from nature. In order to prove deep eutectic feature the interaction between the molecules was investigated by nuclear magnetic resonance spectroscopy. All the tested NADES show clear hydrogen bonding between components. As next step physical properties of NADES such as water activity, density, viscosity, polarity and thermal properties were measured as well as the effect of water on the physical properties. In the last stage the novel NADES were applied to the solubilization of wide range of biomolecules such as non-water soluble bioactive natural products, gluten, starch, and DNA. In most cases the solubility of the biomolecules evaluated in this study was greatly higher than water. Based on the results the novel NADES may be expected as potential green solvents at room temperature in diverse fields of chemistry.