Scale-up Of Process Research Articles

Novel natural deep eutectic solvent-based supramolecular solvents designed for extracting phytochemicals from pigeon pea leaves and its scale-up and recovery process

In this study, a novel green natural deep eutectic solvent-based supramolecular solvent/equilibrium solution (NADES-SUPRAS/EqS) system was designed. The microstructure and formation processes were characterized, revealing the formation and extraction mechanism of this novel solvent. In combination with vortex-assisted extraction, NADES-SUPRAS/EqS was used to efficiently extract and enrich representative active ingredients of different polarities in Cajanus cajan (Linn.) Millsp leaves. The influencing factors, including auxiliary extraction methods, the type of NADES, the proportion of NADES and ethanol for synthesis, the solid-to-liquid ratio, and the vortex time, were then adjusted utilizing single-factor optimization and response surface methodology. Under ideal extraction parameters, the extraction rates obtained were higher than other conventional organic solvents and had an excellent enrichment effect with only 90 s of vortex-shaking. Ultimately, an integrated multi-stage counter-current extraction and recovery unit was developed, capable of reducing costs and easily recovering solvents and target compounds, exploring the possibility of large-scale applications in the industry. A complete set of extraction, isolation, and recovery from plant material to chemical components offers a new perspective for the development of a high-value industry for plant secondary metabolites.

CFD-response surface methodology to optimize the effective thermal conductivity and homogeneity in tray dryer

Tray dryers are usually designed with simplistic scaling rules that do not account for all the transport phenomena associated with drying. The use of computational fluid dynamics coupled with response surface methodology can be a powerful tool to evaluate how different tray dryer design parameters affect the drying process. In this work, two tray dryers, one with a lateral air inlet and another with a bottom air inlet, were parameterized for the position of the air inlet, the dryer length, and the distance between the trays. A central composite design was chosen to determine the sample points, and the average turbulence viscosity and effective thermal conductivity as well as the homogeneity index were calculated. With these values, a response surface curve was constructed. The effective thermal conductivity and its homogeneity index were improved (80 % and 11 %, respectively) with an increased distance between trays and an air inlet located in the middle of the inlet face in the best scenario. In addition, the reductions in effective thermal conductivity outcomes were minimal due to the scale-up process in terms of the dryer length.

Αpplication of Aspergillus niger for Extracellular Tannase and Gallic Acid Production in Non-sterile Table Olive Processing Wastewaters

Aspergillus niger B60 was screened for the first time toward extracellular tannase and gallic acid production by submerged fermentation using synthetic media supplemented with tannic acid as the sole carbon source at a wide concentration range (5–150 g/L). Maximum tannase (47 IU/mL) and gallic acid production (36 g/L) was obtained at initial tannic acid concentration 100 g/L. For this study, it was of interest to valorize non-sterile table olive processing wastewaters for fungal tannase production. In particular, lye and washing water effluents from Spanish-style green olive processing enriched with 100 g/L tannic acid provided effective alternative substrates for the production of tannase (21 IU/mL and 17 IU/mL, respectively) and gallic acid (22 g/L and 14 g/L, respectively). The fungal growth and tannase production kinetics were described by the Logistic and Luedeking–Piret models, respectively. The maximum dry biomass content and the maximum specific growth rate were more pronounced in the tannic acid-rich effluents (16–18 g/L and 0.5–0.6 1/h, respectively) than in the synthetic medium (11 g/L and 0.4 1/h, respectively) although in all cases tannase production was growth-associated. These novel findings cast a new light on successful biorefinery strategies of the effluents and warrant further investigation via process scaling-up and optimization.Graphical

Optimizing the production of wheat beer by recycling the yeast biomass: perspective for cost reduction with quality maintenance

A considerable investment is being experienced worldwide in the production of artisanal beers of different styles, such as wheat-based Weizen beer. The challenge is to reduce production costs while maintaining the commercially accepted quality. Thus, the improvement of the production process involves the possibility of shortening the fermentation time by reusing the yeast biomass without affecting the yeast vitality and the quality of the end product. In this study, the fermentation parameters of a Weizen beer were measured directly from a scaled-up process in a microbrewing in order to identify the optimum point at which the process might be ended without compromising the final characteristics. The results were confirmed by laboratory studies that compared three different yeast strains in a wheat-based industrial substrate. The results led to the conclusion that the fermentation time was reduced by more than 50% from 7 to 3 days, with less variation in the concentration of the investigated metabolites. By reducing the time of fermentation, the yeast biomass was maintained active to be used up to six consecutive cycles of fermentation. All these improvements might help in reducing the cost of beer processing, which is of paramount interest to microbreweries worldwide.

Multiscale techno-economic analysis of orange hydrogen synthesis

The conversion of hydrogen sulphide into value-added products, hydrogen and elemental sulphur, might be a promising route for the treatment of H2S waste streams and for a circular production of hydrogen. This work investigates the thermal splitting of H2S at different scales: the kinetic scale through dedicated experimental campaigns, the reactor scale with a combined experimental and modelling approach, and the process scale in a commercial simulation environment. The system was tested in a lab-scale reactor at 1 bar and in a temperature range going from 640 °C up to 1100 °C. H2S conversion was measured and used to validate a kinetic scheme implemented in a customized simulation suite. These results were then used for process design and scale-up in Aspen HYSYS, which, considering a feed of 10 t/h of pure H2S, estimated a production of 590.8 kg/h of hydrogen. An economic analysis was performed and the production cost of hydrogen resulted to be 2.23 $/kg.

Lignin extraction from sawdust: optimization of experimental studies, computer-aided simulation and techno-economic analysis of scale-up process design with uncertainty quantification

Lignin extraction from sawdust: optimization of experimental studies, computer-aided simulation and techno-economic analysis of scale-up process design with uncertainty quantification

Intelligent co-design of material, process, and equipment for manufacturing high-quality traditional Chinese medicine preparations

In the context of Pharma 4.0, the design tools that support the pharmaceutical Quality by Design(QbD) are iterating fast toward intelligent or smart design. The conventional development methods for traditional Chinese medicine(TCM) preparations have the limitations such as over dependence on experience, low dimensions for the designed experiment parameters, poor compatibility between the process and equipment, and high trial-and-error cost during process scale-up. Therefore, this paper innovatively proposed the intelligent co-design involving material, process, and equipment for manufacturing high-quality TCM preparations, and introduced the design philosophy, targets, tools, and applications with TCM oral solid dosage(OSD) as an example. In terms of design philosophy, the pharmaceutical design tetrahedron composed of critical material attributes, critical process parameters, critical equipment attributes, and critical quality attributes was developed. The design targets were put forward based on the product performance classification system. The design tools involve a design platform that contains several modules, such a as the iTCM material database, the processing route classification system, the system modeling and simulation, and reliability-based optimization. The roles of different modules in obtaining essential and universal design knowledge of the key common manufacturing units were introduced. At last, the applications of the co-design methodology involving material, process, and equipment in the high shear wet granulation process development and the improvement of the dissolving or dispersion capability of TCM formula granules are illustrated. The research on advanced pharmaceutical design theory and methodology will help enhance the efficiency and reliability of drug development, improve the product quality, and promote the innovation of high-end TCM products across the industry.

Catalytic conversion of n-Dodecane to lower olefins hydrogen carriers over bran-shaped modified MCM-22 zeolite catalyst: SiO2/Al2O3 ratio effects

The demand-supply gap for light olefins and aromatics has been enormous in recent years. This imbalance is anticipated to grow exponentially due to their extensive use in manufacturing plastics, textiles, pharmacological intermediates, climate-neutral synthetic fuels, and hydrogen carriers. Production of light olefins through the catalytic cracking of naphtha is widely regarded as one of the most prestigious methods. Despite this, selecting an effective and efficient catalyst is one of the most challenging aspects of the scaling-up process. In this study, a highly active, modified MCM-22 catalyst has been synthesized by a hydrothermal method. Various techniques are used for the characterization of catalysts, including scanning electron microscopy (SEM), X-ray diffraction (XRD), N2 adsorption-desorption, temperature-programmed desorption of ammonia (NH3-TPD), and solid-state nuclear magnetic resonance experiments (NMR) with Al and Si. The cracking of n-dodecane to lower olefins was performed, and it was found that the conversion rates were highly correlated with the SiO2/Al2O3 ratio of the MCM-22 samples. Sample Si0.5 (SiO2/Al2O3 ∼ 28.9) showed a typical photograph of the MWW phase with a bran or flake shape in a stacking mode. The Si0.5 sample has a superior external surface area than other samples (up to ca. 130 m2/g) caused by a smaller particle with an average crystal size of around 15 nm, resulting in maximum catalytic performance towards light olefins. It was discovered that Si0.5 had a diminishing tendency in the paraffinic selectivity but had a robust selectivity for olefins (propylene and butylene in particular). This research may provide academics and the industry with new prospects for improving the catalytic cracking of n-dodecane into light olefins.

Alkalization of acetylacetonates: A facile and versatile method to prepare Ni-based hydroxides for the electrochemical production of bio-based 2,5-furandicarboxylic acid

A facile and versatile synthesis method is required for the preparation of Ni-based hydroxides, which are efficient electrocatalysts for oxidation of 5-hydroxymethylfurfural (HMF) to high-value added chemical 2,5-furandicarboxylic acid (FDCA). Herein, a preparation strategy for Ni-based hydroxides is provided based on the alkalization of acetylacetonates. With carbon black as the support, ultrathin porous Ni(OH)2 nanosheets (∼1 nm in thickness) are obtained with HMF conversion and FDCA yield reaching ∼100% and 98.1%, respectively. With carbon felt or nickel foam as the substrate, the self-supporting Ni(OH)2 electrode can continuously operate in anion exchange membrane electrolyzer for up to 80 h with the content of FDCA in product between 80% and 100%. After the scale-up of preparation process, the performance of catalyst and electrode is maintained. Moreover, Ni-Co bimetallic hydroxide can be also prepared by this method, which presents enhanced activity for HMF oxidation at low electrode potentials.

Experimental Activities on a Hydrogen-Powered Solid Oxide Fuel Cell System and Guidelines for Its Implementation in Aviation and Maritime Sectors

Solid oxide fuel cell (SOFC) systems are spreading worldwide and, for limited applications, also in the transport sector where high power rates are required. In this context, this paper investigates the performance of a six-cell SOFC stack by means of experimental tests at different power levels. The experimental campaign is based on two different stages: the heating phase, useful for leading the system temperature to approximately 750 °C, and the test stage, in which the experimental activities are properly carried out with varying input parameters, such as the DC current load. In addition, a detailed post-processing activity is conducted to investigate the main performance that could be used in the scale-up processes to design and size a SOFC-based system for transportation. The experimental results concern the electrical power, which reaches 165 W, roughly 27 W for each cell and with 52% electrical efficiency, as well as the theoretical thermal power and efficiency, useful for cogeneration processes, with maximum values of 80 W and 25%, respectively, achieved at maximum load. This discussion then shifts to an in-depth analysis of the possible applications of SOFCs in sustainable mobility, particularly in the maritime and aviation industries. The complexities of the issues presented underscore the field’s multidisciplinary nature, ranging from materials science to system integration, and environmental science to regulatory standards. The findings presented could be useful to scientists, engineers, policymakers, and industry stakeholders working on the development and commercialization of SOFC systems in the sustainable transportation sectors.

Modelling of Nano Silica Formation from Geothermal Silica Using Co-Precipitation Method

Nanosilica is a nanotechnology product with many substantial functions in many industries. Previous research showed that nano silica can be synthesized from geothermal silica, that caused silica scaling in injection well and turbine in geothermal power plant, reducing its power plant capacity by 40%. This research used geothermal silica as a precursor for nanosilica production with co-precipitation to recover amorphous silica from silica geothermal to reduce scaling while also increasing its economic value. The objectives of this study were to determine the model to represent the co-precipitation method for nano-silica by using nucleation and growth modelling, therefore help the scale-up process of nanosilica production. The experiment was conducted in four steps. (1) Silica washing utilized distillate water with a ratio of water to silica of 10:1 and sulfuric acid of 20% with a ratio of acid to silica of 4:1, both as a washing agent. (2) Preparation of HCl with concentrations of 3% and 9%. (3) Preparation of sodium silicate solution by reacting washed silica and NaOH to obtain sodium silicate. (4) Preparation of primary and secondary sodium silicate by diluting sodium silicate by two and four times to obtain primary and secondary sodium silicate, respectively. (5) Precipitation of sodium silicate with HCl consists of two steps using primary and secondary sodium silicate. The result showed that the model fit concentration data, with Sum of Squared Error (SSE) 1.9297.10-4, mass transfer coefficient rate is 9.8.10-3 dm/min, and the average relative error is 3.5%.

Kinetic modelling and improvement of methane production from the anaerobic co-digestion of swine manure and cassava bagasse

Anaerobic co-digestion (AcoD) is a promising biotechnological approach for the management of livestock and agro-industrial wastes with the concomitant production of renewable energy. This study investigated methane production during batch AcoD of swine manure (SM) and different amounts of cassava bagasse (CB), using Na2CO3 to adjust initial pH (8.0) and as buffering agent. The highest methane yield of 41,129 ± 1783.6 mL CH4 L−1 (157,04 ± 6,81 mL CH4 g VSinitial−1) was observed with 90.6 g total solids (TS) L−1, in systems containing 16.87 g TS L−1 from cassava bagasse. At this condition and in comparison, with the control (C1), the reactor R4 presented a superior removal of 83.8% for TS, 101.1% for VS, 42.1% for COD, and 161.6% for CODS. Nevertheless, methane production was inhibited at higher CB additions (22.48–33.72 g TS L−1). Methane production kinetics was well explained by including the first order specific growth rate with metabolism as the limiting step for two different substrates (SM and CB) and the linear buffering capacity behavior from CB. This novel proposed model describes the phenomenon of acid inhibition and inactivation of cell biomass caused by the insufficient buffering capacity. The developed model might apply to other similar systems where acid failure could occur, and can be used for a rational scale-up of batch and continuous processes.

Analysis of powder behaviour in bin blending processes at different scales using DEM

Obtaining a desired content uniformity with satisfactory flowability is one of the main challenges during blending process of the pre-mixture with lubricants. In this study, Discrete Element Method (DEM) simulations were implemented to examine blending time and mixing behaviour during the blending process on the lab and industrial scales. The main goal was to investigate the possible influence of operational conditions on the blending behaviour and the change in powder cohesivity during the scale-up process. The effects of rotational speed and filling mass on the particles' travelled distance, velocity, shear stress and blending time were studied in the simulations. Based on the simulations, blending time and particle exposure to shear during the blending process were calculated for different scales. It was observed that the system's mass significantly influences them, and the effect of rotational speed could be neglected. The novelty of this paper is connecting particle exposure to shear from DEM to the flow function coefficient (ffc) of powder from experiments. It was done to define a critical range of exposure to shear that changes the powder flowability in different scales.

A rapid, high-yield and bioinspired synthesis of colloidal silver nanoparticles using Glycyrrhiza glabra root extract and assessment of antibacterial and phytostimulatory activity.

Silver nanoparticles (AgNPs) have emerged as highly effective antimicrobial agents against multidrug-resistant (MDR) pathogens. This study aims to employ green chemistry principles for AgNP synthesis involving phytochemical-rich extract from Glycyrrhiza glabra roots. The approach highlights using renewable feedstocks, safer chemicals, minimum byproducts, and process scale-up. The synthesis of AgNPs was assessed using a surface plasmon resonance band at 420 nm, and structural properties were characterized using TEM, x-ray diffraction, Fourier-transform infrared spectroscopy, and X-ray photoelectron spectroscopy. This method enables the production of high-yield dispersions of AgNPs with desired physicochemical characteristics, including dark yellow solution, size (~20 nm), spherical to an oval shape, crystal structure, and stable colloidal properties. The antimicrobial activity of AgNPs was investigated against the MDR bacteria strains of gram-positive (Staphylococcus aureus) and gram-negative (Escherichia coli). This work reveals that the antimicrobial activity of AgNPs can be influenced by bacterial cell wall components. The results demonstrate the strong interaction between AgNPs and E. coli, exhibiting a dose-dependent antibacterial response. The green approach facilitated the safer, facile, and rapid synthesis of colloidal dispersions of AgNPs, providing a sustainable and promising alternative to conventional chemical and physical methods. Furthermore, the effect of AgNPs on various growth parameters, including seed germination, root and shoot elongation, and dry weight biomass, was assessed for mung bean seedlings. The results revealed phytostimulatory effects, suggesting the promising prospects of AgNPs in the nano-priming of agronomic seeds. RESEARCH HIGHLIGHTS: Glycyrrhiza glabra root extract enabled rapid, high-yield, and eco-friendly synthesis of silver nanoparticles (AgNPs). Spectrophotometric analysis examined the optical properties, scalability, and stability of AgNPs. Transmission electron microscopy provided insights into the size, shape, and dispersity of AgNPs. Scanning electron microscopy revealed significant damage to gram-negative bacterial cell morphology and membrane integrity. AgNPs were found to enhance seed germination, seedling growth, and biomass yield of Vigna radiata.

Revisiting heat losses in lab-scale distillation columns: Quantification, improvement, and influence on miniaturized 3D-printed packings

Lab-scale distillation columns with a diameter of 50 mm (DN50) are widely established for experimental investigations during process development and scale-up. In recent years, the diameter was successfully reduced to 20 mm (DN20) by utilizing additive manufacturing to attain new miniaturized packings that attend to the specific miniaturization obstacles. However, since heat losses have a higher influence in a DN20 column, this publication investigates their impact on the operation and data obtained from an additively-manufactured laboratory distillation column. A comparison is provided between the state-of-the-art DN50 size and a miniaturized DN20 size. The heat loss rate is estimated by simulations and experimentally measured for both column diameters with and without thermal insulation. The impact on the internal flow variation and the gas load (F-factor) uncertainty is presented. The findings provided motives for further improvement to minimize the heat loss rate in the DN20 column. This led to the development of a novel active insulation system where custom-dimensioned flexible silicon heaters are utilized for external heat compensation. The system reduces the heat losses significantly and led to a decrease in the F-factor uncertainty from ± 0.09 Pa0.5 to 0.04 Pa0.5 compared to the passively insulated case. Finally, the effect of the heat loss reduction on the mass transfer efficiency is discussed using two additively-manufactured packings, a 3D-printable version of the Rombopak 9M structure (RP9M-3D) and a new miniaturized packing (XW-Pak). The RP9M-3D showed a decrease in separation performance with heat loss reduction while the performance of the XW-Pak remained unaffected.

Improvement of the Mechanical Properties of Silica Aerogels for Thermal Insulation Applications through a Combination of Aramid Nanofibres and Microfibres.

Reinforcement of silica aerogels, remarkable lightweight mesoporous materials with outstanding insulation performance, is still a challenging research topic. Among the strategies used to overcome their brittleness, one of the most effective is the manufacturing of aerogel composites with embedded fibres. In this work, the incorporation of nanofibres together with microfibres in a tetraethoxysilane-vinyltrimethoxysilane matrix is investigated for the first time for the development of novel aerogel nanocomposites. The nanofibres, synthesized from different aramid fibres, including Kevlar® pulp, Technora®, Teijinconex® and Twaron® fibres, were used in different combinations with microaramids and the resulting nanocomposites were thoroughly investigated for their physicochemical and thermomechanical features. The properties depended on the type and amount of the nano/microfibre used. While the microfibres exhibited low interaction with the silica matrix, the higher surface of the nanofibres ensured increased contact with the gel matrix. A low bulk density of 161 kg m-3 and thermal conductivity of 38.3 mW m-1 K-1 (Hot Disk®) was achieved when combining the nanofibres obtained from Kevlar® pulp with the Technora® or Teijinconex® long fibres. The nanofibres showed higher dispersion and random orientation and in combination with microfibres led to the improvement by a factor of three regarding the mechanical properties of the aerogel nanocomposites reinforced only with microfibres. The scale-up process of the samples and simulated tests of thermal cycling and vacuum outgassing successfully conducted indicate good compliance with space applications.

Estimation of selectivities in the lipase-catalyzed esterification of trimethylolpropane with fatty acids

Interest has increased in using enzyme-catalyzed esterification to produce fatty acid esters of trimethylolpropane for use as biolubricants. Mathematical models of this process can be used to guide the design and scale-up of production processes. The selectivities of the enzyme for the various trimethylolpropane species (unesterified, mono-esterified, di-esterified and tri-esterified) are important parameters of such models. Previous attempts to estimate selectivities in the esterification of trimethylolpropane have not produced accurate estimates. In the current work, we show that the fingerprinting method can be used to obtain accurate estimates. We apply the method to various data sets from the literature, using Bayesian techniques for model fitting. We show that, depending on the reaction conditions, different versions of the model are necessary: (i) A model that treats the reactions as irreversible; (ii) an “irreversible model” that recognizes mass transfer limitations, but treats them using a pseudoprocessive model; and (iii) a model that treats the first reaction as reversible and is appropriate for systems in which water is added at the beginning of the reaction.

A Soft Skin Adhesive (SSA) Patch for Extended Release of Pirfenidone in Burn Wounds.

As much as half or more of deep partial-thickness burn wounds develop hypertrophic scarring and contracture. Once formed, treatments are only minimally effective. Pirfenidone (Pf), indicated for treatment of idiopathic pulmonary fibrosis, is an anti-inflammatory and anti-fibrotic small molecule that potentially can be repurposed as a preventative against scarring in burn wounds. We present a drug-in-matrix patch with a soft skin adhesive (SSA) wound-contacting layer for multi-day drug delivery of Pf into burn wounds at the point of injury. Our patch construction consists of an SSA adhesive layer (Liveo™ MG7-9850, Dupont, Wilmington, DE, USA) for wound fixation, an acrylic co-polymer drug matrix (DURO-TAK 87-2852, Henkel, Düsseldorf, Germany) as the drug (Pf) reservoir, and an outermost protective polyurethane backing. By employing a drug-in-matrix patch design, Pf can be loaded as high as 2 mg/cm2. Compared to the acrylic co-polymer adhesive patch preparations and commercial films, adding an SSA layer markedly reduces skin stripping observed under scanning electron microscopy (SEM). Moreover, the addition of varying SSA thicknesses did not interfere with the in vitro release kinetics or drug permeation in ex vivo porcine skin. The Pf patch can be easily applied onto and removed from deep partial-thickness burn wounds on Duroc pigs. Continuous multi-day dosing of Pf by the patches (>200 μg/cm2/day) reduced proinflammatory biomarkers in porcine burn wounds. Pf patches produced by the manual laboratory-scale process showed excellent stability, maintaining intact physical patch properties and in vitro biological activity for up to one year under long-term (25 °C at 60% RH) and 6 months under accelerated (40 °C at 75% RH) test conditions. To manufacture our wound safe-and-extended-release patch, we present scale-up processes using a machine-driven automated roll-to-roll pilot scale coater.

The imidazole ionic liquid was chemically grafted on SBA-15 to continuously catalyze carbon dioxide to prepare propylene carbonate

The massive emission of carbon dioxide has led to the greenhouse effect. The preparation of propylene carbonate from carbon dioxide and propylene oxide can alleviate the environmental problems caused by carbon dioxide. In this paper, the supported ionic liquid (NMImBr-SBA-15) was prepared by chemical grafting with SBA-15 as the carrier, and NMImBr-SBA-15 was characterized by XRD, N2 adsorption-desorption, TGA, TEM and FT-IR. The effects of operating conditions on product yield and selectivity were investigated in a batch reactor, including CO2 pressure, catalyst dosage, reaction time and reaction temperature. The continuous catalytic performance of NMImBr-SBA-15 was systematically studied in a fixed bed reactor, which has guiding significance for the reaction design and scale-up process. In addition, the possible reaction mechanism was deduced by DFT calculation.

A Novel One-Step Reactive Extrusion Process for High-Performance Rigid Crosslinked PVC Composite Fabrication Using Triazine Crosslinking Agent@Melamine-Formaldehyde Microcapsules.

In this work, we propose, for the first time, a simple, fast, and efficient strategy to fabricate high-performance rigid crosslinked PVC composites by continuous extrusion. This strategy improves the poor processing fluidity of composites and solves the impossibility of conducting extrusion in one step via using microcapsule-type crosslinking agents prepared by in situ polymerization to co-extrude with PVC blends. The results demonstrate that the PVC/microcapsule composites were successfully prepared. Within the studied parameters, the properties of crosslinked PVC gradually increased with the addition of microcapsules, and its Vicat softening temperature increased from 79.3 °C to 86.2 °C compared with pure PVC. This study shows the possibility for the industrial scale-up of the extrusion process for rigid crosslinked PVC.