Antisolvent Research Articles

Impact of Additives on Drug Particles during Liquid Antisolvent Crystallization and Subsequent Freeze-Drying.

The impact of single or combinations of additives on the generation of nanosuspensions of two poorly water-soluble active pharmaceutical ingredients (APIs), fenofibrate (FF) and dalcetrapib (DCP), and their isolation to the dry state via antisolvent (AS) crystallization followed by freeze-drying was explored in this work. Combinations of polymeric and surfactant additives such as poly(vinyl alcohol) or hydroxypropyl methyl cellulose and sodium docusate were required to stabilize nanoparticles (∼200-300 nm) of both APIs in suspension before isolation to dryness. For both FF and DCP, multiple additives generated the narrowest, most-stable particle size distribution, with the smallest particles in suspension, compared with using a single additive. An industrially recognized freeze-drying process was used for the isolation of these nanoparticles to dryness. When processed by the liquid AS crystallization followed by freeze-drying in the presence of multiple additives, a purer monomorphic powder for FF resulted than when processed in the absence of any additive or in the presence of a single additive. It was noted that all nanoparticles freeze-dried in the presence of additives had a flat, flaky habit resulting in large surface areas. Agglomeration occurred during freeze-drying, resulting in micron-size particles. However, after freeze-drying, powders produced with single or multiple additives showed similar dissolution profiles, irrespective of aging time before drying, thus attenuating the advantage of multiple additives in terms of size observed before the freeze-drying process.

Sub-micron spherical carbon particles with hollow cores from lignin-based hybrid precursors: preparation, characterization, and electrostatic dissipative application

Novel sub-micron, spherical, bio-based carbon materials with hollow-core characteristics were synthesized from spherical lignin particle (SLP) hybrid precursors via thermo-stabilization and carbonization. Primarily, the mixture of bagasse lignin (BG-L) and palm kernel shell lignin (PKS-L) with an addition of dicumyl peroxide (DCP) at different BG-L:PKS-L:DCP ratios was utilized to prepare SLPs through anti solvent precipitation. Interestingly, as-prepared SLPs having a 250–331 nm diameter contained hollow cores of 41–223 nm inside the spherical particles. A mechanism of hollow-core formation was also proposed. Effects of BG-L:PKS-L:DCP ratio, heating rate (HR), oxygen flow rate (O2 FR), and stabilization time (SBT) on spherical shape retention of SLPs after thermo-stabilization were systematically investigated, and a cross-link pathway was suggested. The spherical aspect of SLPs having hollow cores was successfully maintained at optimal conditions of 250 °C for 1 h with a HR of 0.3 °C/min under O2 FR of 3 L/min using a BG-L:PKS-L:DCP ratio of 1:1:1 by wt. After carbonization at 900–1200 °C, spherical carbon particles (SCPs) with hollow cores were obtained, possessing a high carbon (C) element of ≅ 93–96%, a high specific surface area of ≅ 308–593 m2/g, and a high order of graphitic structure (ID/IG ratio ≅ 1). The average particle size of SCPs and hollow-core dimensions were ≅ 171–224 and 80–107 nm, respectively. The polylactic acid (PLA)/SCP composite films were prepared using SCPs at different carbonization temperatures and loadings via a solution casting technique. The composite film containing 20 wt% of SCPs carbonized at 900 °C (SCPs-900) provided a surface resistance of ≅ 3 × 105 Ω and a tribo-charge voltage of 0 V, appropriate for electrostatic dissipative (ED) applications. The Young's modulus and elongation at break of the PLA/SCP-900 (20 wt%) composite film were ≅ 3.4 MPa and 2.0%, respectively. These findings demonstrate a feasible and effective approach to utilize biomass-based lignin for producing carbon particles with unique features as renewable and sustainable conductive fillers in polymer composites.

Naproxen-bipyridine cocrystallization assisted by pressurized carbon dioxide

Cocrystals of S-naproxen (S-NPX) or RS-naproxen (RS-NPX) and 4,4′bipyridine (BiPY) were prepared by the Gaseous Anti Solvent (GAS) method using CO2 as antisolvent. S-NPX and BiPY cocrystals were also produced by Cocrystallization with Supercritical Solvent (CSS) using CO2 as a solvent though leading to mixtures of cocrystals and homocrystals. Hydrogen-bond networks and stoichiometries of produced cocrystals were identical whatever the mode of preparation (evaporation, grinding and CO2-assisted processes) and matched those already described in literature: S-NPX2:BiPY1 and RS-NPX2:BiPY1. The effects of the NPX:BiPY molar ratio and of the processing conditions were investigated. By GAS, an excess of BiPY in the initial processed mixture was mandatory to produce pure S-NPX2:BiPY1 cocrystals whereas pure RS-NPX2:BiPY1 cocrystals were identically produced from mixtures of 2:2 and 2:1 NPX:BiPY initial ratio. No enrichment of the product in any of the naproxen enantiomer was reached, even when mixtures of S- + RS-NPX were coprocessed with bipyridine.

Green Synthesis for Battery Materials: A Case Study of Making Lithium Sulfide via Metathetic Precipitation.

For some future clean-energy technologies (such as advanced batteries), the concept of green chemistry has not been exercised enough for their material synthesis. Herein, we report a waste-free method of synthesizing lithium sulfide (Li2S), a critical material for both lithium-sulfur batteries and sulfide-electrolyte-based all-solid-state lithium batteries. The key novelty lies in directly precipitating crystalline Li2S out of an organic solution after the metathetic reaction between a lithium salt and sodium sulfide. Compared with conventional methods, this method is advantageous in operating at ambient temperatures, releasing no hazardous wastes, and being economically more competitive. To collect the valuable byproduct out of the liquid phases, a "solventing-out crystallization" technique is employed by adding an antisolvent (AS) of low boiling point. The subsequent distillation of the new solution under vacuum evaporates off the AS rather than the high-boiling-point reaction solvent (RS), saving a lot of energy. Consequently, the separated AS and RS containing the unreacted lithium salt can be directly reused. For industrial production, the entire process may be operated continuously in a closed loop without discharging any wastes. Moreover, Li2S cathodes and sulfide-electrolyte Li6PS5Cl derived from the synthesized Li2S show impressive battery performance, displaying the great potential of this method for practical applications.

Formulation Development and Evaluation of Oro-Dispersible Tablets Based On Solid Dispersion of Cimetidine

The most common problem about conventional dosage form is dysphagia (difficulty in swallowing). So, we design a new approach in a conventional dosage form which is oral dispersible tablet. Oral dispersible tablet is also called as mouth dissolving tablet, fast dissolving tablet, or oral disintegrating tablet. Oral dispersible tablet has advantage as it quickly disintegrates into saliva when it is put on the tongue. The faster the drug disintegrates or is dissolved, the faster the absorption and the quicker the therapeutic effect of drug will be attained. The objective of present study was to formulate directly compressible orodispersible tablets of cimetidine with improved solubility and bioavailability by using solid dispersion technique. Cimetidine is a histamine H2-receptor antagonist. It is widely prescribed in active duodenal ulcers, gastric ulcers, Zollinger-Ellison syndrome, gastroesophageal reflux disease and erosive esophagitis. Solid dispersion of cimetidine was prepared by anti-solvent addition method and physical mixture using novel polymer eudragit E 100. Saturation solubility of drug was determined in physical mixture and solid dispersion formulation. The prepared solid dispersion formulations were further characterized by drug contents, HPLC, and encapsulation efficiency. Orodispersible tablets of cimetidine were prepared by direct compression method and blend was evaluated for the pre-compression parameters such as bulk density, compressibility, angle of repose etc. The tablets were prepared by using selected solid dispersion formulation and excipients with sodium starch glycolate as a superdisintegrant and evaluated for hardness, friability, weight variation, content uniformity, wetting time, dispersion time and in-vitro drug release. Orodispersible tablet shows wetting time 27±1 seconds and in-vitro drug release 93.20±3.181%, which is better as compare to tablet containing pure drug (82.36±1.986) within 20min. Thus formulation of orodispersible tablet of cimetidine solid dispersion showed increased solubility and bioavailability with patient complies and convenience.
 Keywords: Cimetidine, Orodispersible tablets, Solid dispersion, Anti solvent addition method, Superdisintegrant

Effect of V-type crystallinity and starch particle structure on the oil loading capacity and anti-oxidation

Starch-based carriers have a great potential in functional oil encapsulation because of their mild preparation conditions, but the oil loading capacity and underlying anti-oxidation mechanism remain unclear. Here V-type starches were applied to fabricate flaxseed oil powder. Particle size analysis and scanning electron microscopy showed a loose aggregation microstructure of normal maize starch (NMS) prepared using the anti-solvent (AS) precipitation method, with an average size of 24.9 μm. Differential scanning calorimetry displayed a good thermo-oxidation resistance of NMS-derived V-type starch prepared via AS precipitation. Principal component analysis revealed that the oil loading capacity, related closely to V-type crystallinity and D50, has a significant positive correlation with the onset oxidation temperature and a negative correlation with the peroxide, thiobarbituric acid, and ρ-anisidine values. Our original study reveals the effects of V-type crystallinity and aggregation microstructure on the oil loading capacity and anti-oxidation, providing theoretical guidance for developing novel, starch-based carriers.

Formation of Curcuma xanthorrhiza extract microparticles using supercritical anti solvent precipitation

Curcuma xanthorriza (C. xanthorrizha) is one of the most medicinal plant used in pharmacy and have many scientifically proven health benefits. In this work, C. xanthorrhiza extract was used as starting material to form microparticles. To prevent the rapid oxidation and to enhance stability, bioavailability, and solubility in water, C. xanthorrhiza extract was combined with polyvinylpyrrolidone (PVP) to form microparticles using supercritical anti solvent (SAS) precipitation. Acetone was used as solvent while supercritical CO2 was used as the antisolvent. The effects of pressure and extract-PVP ratio on the particle size and morphology of particles formed were evaluated. The characterization of microparticles included the particles morphology and functional group of bioactive compounds. SAS process was carried out at various pressures of 8, 12, and 16 MPa, various extract/PVP ratios of 1:0, 1:10, and 1:20, constant CO2 flow rate of 15 mL/min, and constant solution flow rate of 0.5 mL/min. The result showed that nanoparticles were successfully produced with particle sizes ranging from 175 ± 95 nm to 376 ± 137 nm. Scanning electron microscopy (SEM) images described that irregular shape particles were precipitated from C. xanthorrizha extract solution, and spherical shape particles were formed from C. xanthorrizha/PVP solution. Computational Fluid Dynamic (CFD) simulation has successfully applied to realize the internal flow of the nozzle in micronization of SAS process. The results of this work are expected to improve the applications of the bioactive compounds from natural products in pharmaceutical industry.

Preparation and characterization of nanoparticles from field pea starch by batch versus continuous nanoprecipitation techniques

Starch nanoparticles (SNPs) were produced by batch nanoprecipitation (BNP) and continuous techniques such as flash nanoprecipitation (FNP) and microfluidic nanoprecipitation (MNP). Water and absolute ethanol were used as solvent (S) and antisolvent (AS), respectively, while they can be mixed either dropwise or direct mixing at once. The effects of processing parameters on SNPs properties were investigated including antisolvent/solvent (AS/S) ratio, starch concentration, mixing technique and flow rate. Field emission scanning electronic microscopy (FE-SEM), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectrophotometry were used to characterize the nature of molecular interactions and structure within SNP. The results indicated that BNP can be successfully achieved in a shorter time with a smaller particle size and narrower particle size distribution, even at AS/S ratio as low as 1:1, using direct mixing at once method than the dropwise technique. Increasing the starch concentration at a fixed AS/S ratio of 1:1, initially decreased the average particle size from 135 (2.5 mg/mL) to 123 nm (10 mg/mL), and then increased to ~430 nm (50 mg/mL). Based on the optimized conditions for BNP, continuous methods (FNP and MNP), were investigated in the commercial prospective for potential scale up processing. Under the same conditions, FNP involving confined impinging jet mixer (CIJM) at an overall flow rate of 60 mL/min, had a uniform spherical shape with particle size of ~100 nm, which was superior to all other techniques investigated. Regardless of the techniques used, all SNPs had an amorphous structure with short-range molecular order.

Optimization of processing parameters to produce nanoparticles prepared by rapid nanoprecipitation of pea starch

Field pea starch was thermally solubilized in water and subsequently ultrasonicated and then used to produce starch nanoparticles (SNPs) via a rapid nanoprecipitation method with the addition of the antisolvent (AS) ethanol into the starch solution (solvent, S). The spherical shape of SNPs with a small mean particle size was visualized by dynamic light scattering (DLS) and field emission-scanning electron microscopy (FE-SEM), which demonstrated a narrow size distribution (PSD) and good water dispersibility. Processing parameters, such as duration and amplitude of ultrasonication, AS/S ratio, starch concentration, separation and drying techniques, were investigated in relation to their effect on SNPs properties. There is an optimal AS/S ratio (1:1) and starch concentration (10 mg/mL) which gives rise to smaller SNPs with a narrower PSD. The formation of SNPs was found to follow a kinetically controlled nucleation-growth/aggregation mechanism in which amylose molecules formed the initial critical nuclei. The ultrasonication amplitude and separation and drying techniques significantly affected the size and morphology of SNPs. Moderate shear facilitated rapid starch aggregation and SNPs precipitation, enabling easy recovery by centrifugation and subsequent freeze drying. The freeze-dried SNPs were able to be dispersed quickly to form a SNP suspension in Milli-Q water. The dispersed SNPs showed good thermal stability in water and retained their particle characteristics at a temperature range of 25–60 °C. Further research exploring the potential of these SNPs as nutraceutical carriers for applications in both health and nutrition industries is warranted.

Can the cavi-precipitation process be exploited to generate smaller size drug nanocrystal?

Objective Cavi-precipitation has the potential to generate drug nanocrystals very efficiently. Achieving smaller than 100 nm particle size for organic drug substances still remained a challenge. The objective of this study was to demonstrate if cavi-precipitation technology can be used to generate smaller than 100 nm drug nanocrystal particle. Significance This study demonstrates that cavi-precipitation process can be used to generate drug nanocrystals of the model compound resveratrol (RVT) consists of crystallites of 30–50 nm size. Method RVT was dissolved in different organic solvents to prepare the solvent phase (S-phase). Several stabilizers were tested for the organic phase. A combination of SDS and PVP was used stabilizer system in the aqueous anti-solvent phase (AS-phase). The S-phase was added to the AS-phase inside the Emulsiflex C5 homogenizer. Nanosuspension was characterized by laser diffractometry (LD), photon correlation spectroscopy (PCS) and scanning electron microscopy (SEM). The solid state of the suspended particles was investigated by powder X-ray diffractometry (PXRD) and differential scanning calorimetry (DSC). Results It was found that DMSO, alone or in combination with acetone in the S-Phase generated the smallest size RVT nanocrystals. The optimum solvent (S) antisolvent (AS) ratio (S:AS) was found to be 3.6:56.4 (v:v). Span 20 was identified as the best stabilizer for the organic phase at a ratio (w:w) of 1:3 (Span 20:RVT). The particles precipitated from different solvents were predominantly crystalline. Conclusions The best sample had a mean particle size (LD) of 167 nm [d(0.5)] which was composed of smaller crystallites having 30–50 nm size (SEM).

A crystal engineering design to enhance the solubility, dissolution, stability and micrometric properties of omeprazole via Co-crystallization techniques

Introduction: Omeprazole, a proton-pump inhibitor used in peptic ulcers, gastro-oesophageal-reflux disorder, Zollinger-Ellison syndrome and in H.pylori infections. The omeprazole is unstable at acidic pH, undergoes degradation in stomach. To prevent the degradation in stomach, dosage forms are supplied as enteric-coated tablets or granules encapsulated in gelatin capsules. The efficiency of such dosage forms depends upon the extent of coating, solubility of coating material, type of dosage forms; in addition this it is insoluble in water, having poor bioavailability. To overcome these major drawbacks of omeprazole, an novel technique: co-crystallization was attempted, to produce a stable, enhancement in solubility and improved micromeritic properties of omeprazole. Co-crystals consists of API and a stoichiometric amount of a pharmaceutically acceptable co-crystal former. Pharmaceutical Co-crystals are non-ionic supramolecular complexes and can be used to address physical property issues such as solubility, stability and bioavailability in pharmaceutical development without changing the chemical composition of the API. Co-crystal is a crystalline entity formed by two different or more molecular entities where the intermolecular interactions are weak forces like hydrogen bonding and π-π stacking. Materials and methods: As omeprazole is unstable in acidic pH, very hygroscopic character, photosensitive and thermolebility in nature, Anti solvent addition method was used for preparation of crystals. Poly Vinyl Pyrrolidone is taken as co-former, magnesium chloride and sodium bicarbonate as basic substances. Further prepared crystals were characterized by Powder X-ray Diffractometer (PXRD), Differential scanning colorimeter (DSC), Fourier Transformation Infra-red Spectroscopy (FTIR).Moreover they were studied for melting point determination, flow property studies (micromeritic properties), dissolution studies, solubility test and stability tests. Results and discussion: FTIR revealed that there is no formation of hydrogen bonding between drug and co-former; hence it states that co-crystals are not formed, but XRD and DSC states that there is a formation of some physical interaction, partial crystalline and amorphous form which is a new crystal lattice. Conclusion: Formed crystals produce moderate improvement in micromeritic properties, solubility, stability and dissolution behaviour of drug. Thus physicochemical properties of omeprazole were improved via crystal engineering technique-co-crystallization.

Ultrathin polymeric films for interfacial passivation in wide band-gap perovskite solar cells

Wide band-gap perovskite solar cells have the potential for a relatively high output voltage and resilience in a degradation-inducing environment. Investigating the reasons why high voltages with adequate output power have not been realized yet is an underexplored part in perovskite research although it is of paramount interest for multijunction solar cells. One reason is interfacial carrier recombination that leads to reduced carrier lifetimes and voltage loss. To further improve the Voc of methylammonium lead tri-bromide (MAPbBr3), that has a band-gap of 2.3 eV, interface passivation technique is an important strategy. Here we demonstrate two ultrathin passivation layers consisting of PCBM and PMMA, that can effectively passivate defects at the TiO2/perovskite and perovskite/spiro-OMeTAD interfaces, respectively. In addition, perovskite crystallization was investigated with the established anti-solvent method and the novel flash infrared annealing (FIRA) with and without passivation layers. These modifications significantly suppress interfacial recombination providing a pathway for improved VOC’s from 1.27 to 1.41 V using anti solvent and from 1.12 to 1.36 V using FIRA. Furthermore, we obtained more stable devices through passivation after 140 h where the device retained 70% of the initial performance value.

Preparation of All-Trans-Retinoic Acid-Loaded mPEG-PLGA Nanoparticles Using Microfluidic Flow-Focusing Device for Controlled Drug Delivery

In recent years, microfluidic devices present unique advantages for the development of a new generation of nanoparticle synthesis method compared to bulk methods. In this study, we report a microfluidic flow-focusing method for the production of all trans retinoic acid (ATRA)-loaded methoxy poly(ethylene glycol)-poly(lactide-coglycolide) (mPEG-PLGA) nanoparticles (NPs). Box–Behnken experimental design (BBD) was applied to optimize of formulation ingredients and process conditions with minimum particle size, maximum drug loading% (DL%) and encapsulation efficiency% (EE%). Polymer concentration, drug concentration and flow rates of solvent (S) and antisolvent (AS) were selected as independent variables. Based on optimization strategy, minimum particle size achieved shows average (SD) particle size of [Formula: see text][Formula: see text]nm with DL of [Formula: see text][Formula: see text]wt.% and EE of [Formula: see text][Formula: see text]wt.%, respectively. While maximum DL has been reported to be [Formula: see text][Formula: see text]wt.% with particle size of [Formula: see text][Formula: see text]nm and EE of [Formula: see text][Formula: see text]wt.%, respectively. Moreover, the results have shown that the AS/S ratio represents the most significant effect on particle size. Indeed, increasing the AS flow rate directly results in generating smaller particles. The AS/S ratio represents the least significant effect on DL%, such that, at fixed flow rates, higher DL was observed at high concentration of drug and lower concentration of polymer. In conclusion, optimization of the ATRA-loaded mPEG-PLGA NPs by BBD yielded in a favorable drug carrier for ATRA that could provide a new treatment modality for different malignancies.

Experimental study on the reduction of loratadine particle size through confined liquid impinging jets.

The confined liquid impinging jets (CLIJ) technique was applied as a simple and effective approach to reducing the particle size of loratadine to enhance its solubility. The effect of anti-solvent (AS) to solution (S) flow rate ratio, organic phase concentration, Reynolds number (Re), and stabilizer concentration was investigated in this reduction process. After the synthesis, the chemical and physical properties of loratadine nanoparticles were determined through different characterization and analytical techniques. The results indicated that the particle size of loratadine decreases from 320nm to 80nm by increasing the AS/S ratio from 1 to 25. It was found that the particle size of loratadine was unchanged at the higher AS/S ratios. The loratadine nanoparticle size was optimized by changing the solution concentration, Re, and Tween 80 as a stabilizer. The finest loratadine nanoparticle size of about 53nm was obtained with a narrow size distribution, which corresponds to solution concentration of 35mg/mL, Re of 5687, and 0.1% (w/v) stabilizer concentration. It was revealed that the optimized loratadine nanoparticles completely dissolved after 11min, indicating the loratadine nanoparticle dissolution rate 50 times faster than raw loratadine.

Preparation, in vitro and ex-vivo Evaluation of Mirtazapine Nanosuspension and Nanoparticles Incorporated in Orodispersible Tablets

The objective of the present investigation was to enhance the solubility of practically insoluble mirtazapine by preparing nanosuspension, prepared by using solvent anti solvent technology. Mirtazapine is practically insoluble in water which act as antidepressant .It was prepared as nano particles in order to improve its solubility and dissolution rate. Twenty formulas were prepared and different stabilizing agents were used with different concentrations such as poly vinyl pyrrolidone (PVPK-90), poly vinyl alcohol (PVA), poloxamer 188 and poloxamer 407. The ratios of drug to stabilizers used to prepare the nanoparticles were 1: 1 and 1:2. The prepared nanoparticles were evaluated for particle size, entrapment efficiency, dissolution study, Fourier transform infrared spectroscopy, differential scanning calorimetry, and atomic force microscopy. The percentage of drug entrapment efficiency of F1-F20 was ranged from 78.2% ± 1 to 95.9 % ± 1. The release rate and extent of mirtazapine nanoparticles were inversely proportional to the particle size of the drug i.e. it decreased when particle size increase. It is concluded that the nanoprecipitation have potential to formulate homogenous nanosuspensions with uniform-sized stable nanoparticles of mirtazapine. The prepared nanosuspension showed enhanced dissolution which may lead to enhanced solubility of mirtazapine.

Crystal Orientation and Grain Size: Do They Determine Optoelectronic Properties of MAPbI3 Perovskite?

Growing large, oriented grains of perovskite often leads to efficient devices, but it is unclear if properties of the grains are responsible for the efficiency. Domains observed in SEM are commonly misidentified with crystallographic grains, but SEM images do not provide diffraction information. We study methylammoinium lead iodide (MAPbI3) films fabricated via flash infrared annealing (FIRA) and the conventional antisolvent (AS) method by measuring grain size and orientation using electron back-scattered diffraction (EBSD) and studying how these affect optoelectronic properties such as local photoluminescence (PL), charge carrier lifetimes, and mobilities. We observe a local enhancement and shift of the PL emission at different regions of the FIRA clusters, but we observe no effect of crystal orientation on the optoelectronic properties. Additionally, despite substantial differences in grain size between the two systems, we find similar optoelectronic properties. These findings show that optoelectronic quality is not necessarily related to the orientation and size of crystalline domains.

Solubility, Solubility Modeling, and Antisolvent Precipitation of 1,3-Bis(9-carbazolyl)benzene in Organic Solvents

The solubility of 1,3-bis(9-carbazolyl)benzene (mCP) in 12 kinds of organic solvents, including methanol, ethanol, isopropanol, n-butanol, ethyl acetate, n-hexane, dichloromethane, toluene, acetoni...

Electron-Beam-Induced Nucleation in an Antisolvent

Electron-Beam-Induced Nucleation in an Antisolvent

Flash infrared annealing as a cost-effective and low environmental impact processing method for planar perovskite solar cells

Abstract For successful commercialization of perovskite solar cells, straightforward solutions in terms of environmental impact and economic feasibility are still required. Flash Infrared Annealing (FIRA) is a rapid method to fabricate perovskite solar cells with efficiencies >18% on simple, planar architecture, which allows a film synthesis in only 1.2 s, faster than the previous report based in a meso architecture and all of them without the usage of antisolvent. In this work, through a comparative study with the common lab-scale method, the so-called antisolvent (AS), the main photovoltaic parameters and working mechanisms obtained from impedance spectroscopy (IS) measurements show similar device features as for FIRA. However, from the life cycle assessment (LCA) comparison study, the FIRA method has only 8% of the environmental impact and 2% of the fabrication cost of the perovskite active layer with respect to the AS for the perovskite film synthesis. These results denote that FIRA is a low-impact, cost-effective fabrication approach that can be directly adapted to perovskite planar configuration that is compatible with industrial up-scaling.

Recovery of 3-hydroxypropionic acid from organic phases after reactive extraction with amines in an alcohol-type solvent

Reactive extraction is a well-known method for the recovery of organic acids from dilute streams. The extraction through complex formation with amines is followed by its back-extraction. Their affinity for amine extractants makes their back-extraction a limiting step. The case of 3-hydroxypropionic acid is addressed here. Three methods were compared: salts additions, diluent swing and temperature swing. Mineral bases led to complete 3-HP recovery but as a salt. Diluent swing was tested using n-hexane as the anti–solvent. Results showed that increasing the n-hexane content led to a great increase of 3-HP recovery. However, high recovery yields are associated with high dilutions. The temperature was varied from 4 to 140 °C and it led to a high decrease of the acid-amine complex formation. Our thermochemical study showed an apparent heat of reaction of −25.3 kJ/mol and, at 140 °C, 78% of 3-HP can be recovered in a single step.