The development of a bio-based economy has its foundations in the development of efficient processes to optimize biomass potential. In this context there are a multitude of molecules that can be either synthetized or recovered from biomass, among those the so-called 12 building-blocks reported by the US Department of Energy. Even if their identification and importance is clearly defined, research efforts concerning the purification or separation of these platform molecules are limited. To fill this gap, different configurations for the purification of levulinic acid recovered from lignocellulosic biomass are examined and compared in this work. In particular, hybrid configurations obtained by the combination of liquid-liquid extraction and distillation have been considered. It was demonstrated how a deep understanding of the subspace including all extraction-assisted simple column distillation configurations represents a fundamental step in the synthesis of different process alternative... [more]

This paper reviews the current technological development of bio-hydrogen (BioH2) generation, focusing on using lignocellulosic feedstock via dark fermentation (DF). Using the collected reference reports as the training data set, supervised machine learning via the constructed artificial neuron networks (ANNs) imbedded with feed backward propagation and one cross-out validation approach was deployed to establish correlations between the carbon sources (glucose and xylose) together with the inhibitors (acetate and other inhibitors, such as furfural and aromatic compounds), hydrogen yield (HY), and hydrogen evolution rate (HER) from reported works. Through the statistical analysis, the concentrations variations of glucose (F-value = 0.0027) and acetate (F-value = 0.0028) were found to be statistically significant among the investigated parameters to HY and HER. Manipulating the ratio of glucose to acetate at an optimal range (approximate in 14:1) will effectively improve the BioH2 generat... [more]

Biomass gasification is one of the most promising routes to produce green hydrogen, power, fuels, and chemicals, which has drawn much attention as the world moves away from fossil fuels. Syngas produced from gasification needs to go through an essential gas cleanup step for the removal of tars and particulates for further processing, which is one of the cost-inducing steps. Existing hot gas cleanup strategies involve the particulate removal step followed by catalytic tar reforming, which could be integrated into a single unit operation using porous ceramics owing to their advantages including high-temperature resistance, high corrosion resistance, flexibility, and robust mechanical integrity. Ceramic filters have proven to be effective at filtering particulates from hot gas streams in various applications including combustion, incineration, gasification, and pyrolysis. These materials have also been evaluated and used to an extent as catalyst support to remove contaminants such as nitr... [more]

Environmentally friendly amino-acid salt solutions are used for the absorption of carbon dioxide from concentrated flue-gas streams via chemical absorption. Process intensification reduces operating and capital costs by combining chemical reactions and separation operations. Here, we present a new process-intensification approach that combines the CO2 capture and the amino-acid regeneration steps into a single process carried out in a slurry three-phase reactor. The absorbed CO2 precipitates as a solid carbonated guanidine compound. The cycle is completed by separation of the solid precipitate to strip the CO2 and regenerate the guanidine compound, while the liquid solution is recycled to the slurry reactor. The process was studied by modifying a model developed by the authors for a gas-liquid bubble column without the presence of the guanidine compound. The guanidine precipitation reaction was accounted for using kinetic parameters calculated by the authors in another study. The propo... [more]

Several carbon sequestration technologies have been proposed to utilize carbon dioxide (CO2) to produce energy and chemical compounds. However, feasible technologies have not been adopted due to the low efficiency conversion rate and high-energy requirements. Process intensification increases the process productivity and efficiency by combining chemical reactions and separation operations. In this work, we present a model of a chemical-electrochemical cyclical process that can capture carbon dioxide as a bicarbonate salt. The proposed process also produces hydrogen and electrical energy. Carbon capture is enhanced by the reaction at the cathode that displaces the equilibrium into bicarbonate production. Literature data show that the cyclic process can produce stable operation for long times by preserving ionic balance using a suitable ionic membrane that regulates ionic flows between the two half-cells. Numerical simulations have validated the proof of concept. The proposed process cou... [more]

Propylene glycol monomethyl ether acetate (PGMEA) is a commonly used solvent in the rapidly developing semiconductor industry. Ultra-high purity PGMEA is required for this ultra-precision industry and to satisfy the current strict waste management regulations. The traditional PGMEA production process consumes considerable energy and has a high production cost. In this study, a novel heat integrated and intensified design, which applies a dividing wall column, reactive distillation, and pressure swing techniques, was proposed for improving the energy efficiency and reducing the cost of PGMEA production. Heat integration was applied to maximize the heat recovery of the process. All processes were simulated using the commercial simulator Aspen Plus V11. The economic and environmental parameters of the process alternative were assessed for a fair comparison with the conventional process. The results showed that heat integration of the optimal pressure swing-based reactive distillation and... [more]

The greatest challenge of our times is to identify low cost and environmentally friendly alternative energy sources to fossil fuels. From this point of view, the decarbonization of industrial chemical processes is fundamental and the use of hydrogen as an energy vector, usable by fuel cells, is strategic. It is possible to tackle the decarbonization of industrial chemical processes with the electrification of systems. The purpose of this review is to provide an overview of the latest research on the electrification of endothermic industrial chemical processes aimed at the production of H2 from methane and its use for energy production through proton exchange membrane fuel cells (PEMFC). In particular, two main electrification methods are examined, microwave heating (MW) and resistive heating (Joule), aimed at transferring heat directly on the surface of the catalyst. For cases, the catalyst formulation and reactor configuration were analyzed and compared. The key aspects of the use of... [more]

N2O has a global warming potential about 300 times higher than CO2, and even if its contribution to the greenhouse effect is underrated, its abatement in industrial production’s tail gas has become imperative. In this work, we investigate the feasibility of the microwave (MW)-assisted regeneration of a 13X zeolite bed for N2O capture from tail gases. Several consecutive adsorption−desorption cycles were performed to verify the microwave heating effect on the zeolite’s adsorption properties. The results of the experimental tests, performed at N2O concentrations of 10, 20 and 40% vol, highlighted that (i) the steps are perfectly repeatable in terms of both adsorbed and desorbed amount of N2O, meaning that the MWs did not damage the zeolite’s structure, (ii) the presence of both H2O and O2 in the feed stream irreversibly reduces the adsorbent capacity due to nitrites and nitrates formation, and (iii) the presence of H2O alone with N2O still reduces the adsorbent capacity of the zeolites,... [more]

Freeze-drying is a common process to extend the shelf life of food and bioactive substances. Its main drawback is the long drying time and associated high production costs. Microwaves can be applied to significantly shorten the process. This study investigates the effects of modulating the electromagnetic field in microwave-assisted freeze-drying (MFD). Control concepts based on microwave frequency are evaluated using electromagnetic simulations. The concepts are then applied to the first part of primary drying in a laboratory-scale system with solid-state generators. Targeted frequency modulation in the electromagnetic simulations enabled an increase in energy efficiency or heating homogeneity throughout MFD while having negligible effects on the power dissipation ratio between frozen and dried product areas. The simulations predicted the qualitative effects observed in the experimental proof of concept regarding energy efficiency and drying homogeneity. Additionally, shortened drying... [more]

This study aims to investigate, from a technical and an environmental perspective, various alternatives for acetic acid concentration for maximizing acetic acid production, its purity, and in the meantime, minimizing the energy usage and the environmental impact. Liquid−liquid extraction followed by azeotropic distillation using different solvents such as: (i) ethyl acetate, (ii) isopropyl acetate, and (iii) a mixture containing isopropyl acetate and isopropanol were first explored, using process flow modeling software. The three cases were compared considering various technical key performance indicators (i.e., acetic acid flow-rate, acetic acid purity, acetic acid recovery, power consumption, thermal energy used, and number of equipment units involved) leading to the conclusion that the usage of the isopropyl acetate—isopropanol mixture leads to better technical results. The isopropanol-isopropyl acetate mixture was furthermore investigated in other two cases where process intensific... [more]

This work presents an experimental and modelling evaluation of the preferential oxidation of CO (CO PROX) from a H2-rich gas stream typically produced from fossil fuels and ultimately intended for hydrogen fuel cell applications. A microchannel reactor containing a washcoated 8.5 wt.% Ru/Al2O3 catalyst was used to preferentially oxidise CO to form CO2 in a gas stream containing (by vol.%): 1.4% CO, 10% CO2, 18% N2, 68.6% H2, and 2% added O2. CO concentrations in the product gas were as low as 42 ppm (99.7% CO conversion) at reaction temperatures in the range 120−140 °C and space velocities in the range 65.2−97.8 NL gcat−1 h−1. For these conditions, less than 4% of the H2 feed was consumed via its oxidation and reverse water-gas shift. Furthermore, a computational fluid dynamic (CFD) model describing the microchannel reactor for CO PROX was developed. With kinetic parameter estimation and goodness of fit calculations, it was determined that the model described the reactor with a confide... [more]

Dividing-wall columns (DWCs) are intensified processes that have attracted industrial and academic attention due to the reduction in operating and installation costs compared to traditional distillation systems. Several methodologies are available for the design of DWCs. Most of them consist of three parts: an analysis of operating variables; an analysis of the structural design (topology); and an optimization of the resulting preliminary design. This paper aims to study three widely used design methodologies reported in the literature for DWCs, i.e., Triantafyllou and Smith (T&S), minimum vapor (Vmin), and Sotudeh and Shahraki (S&S) methods, along with their implementation on process simulators. A proposed modification to the S&S methodology is also presented. A comparison of the methods is carried out and rated against designs with minimum total annual costs. The analysis considers the effect of different structural design variables to initialize the design procedure with each method... [more]

A current focus of biopharmaceutical research and production is seed train process intensification. This allows for intermediate cultivation steps to be avoided or even for the direct inoculation of a production bioreactor with cells from cryovials or cryobags. Based on preliminary investigations regarding the suitability of high cell densities for cryopreservation and the suitability of cells from perfusion cultivations as inoculum for further cultivations, an ultra-high cell density working cell bank (UHCD-WCB) was established for an immunoglobulin G (IgG)-producing Chinese hamster ovary (CHO) cell line. The cells were previously expanded in a wave-mixed bioreactor with internal filter-based perfusion and a 1 L working volume. This procedure allows for cryovial freezing at 260 × 106 cells mL−1 for the first time. The cryovials are suitable for the direct inoculation of N−1 bioreactors in the perfusion mode. These in turn can be used to inoculate subsequent IgG productions in the fed-... [more]

Biocatalytic processes often provide an ecological alternative to many chemical processes. However, further improvements in terms of the economic efficiency are required. In order to achieve that, the concept of process integration is a promising option. Applying this within a biocatalytic process, a highly integrated apparatus working as a reactive extraction centrifuge was developed and operated. For this purpose, a commercially available extraction centrifuge was modified to implement a biocatalytic reaction. The novel apparatus was used within a multi-enzyme cascade for the production of a natural flavor and fragrance, namely cinnamic ester. The characterization of the reactive extraction centrifuge and the suitable operation conditions for the inlet streams and the rotational speed for a stable operation were determined. Furthermore, different initial substrate concentrations were applied to prove the reaction. The results provide a successful proof of concept for the novel reacti... [more]

Computational fluid dynamics (CFD) have been extensively used to simulate the hydrodynamics of multiphase flows (MPFs) in rotating machinery. In the presence of a granular dense phase, the Kinetic Theory of Granular Flow (KTGF) is usually coupled to Eulerian multi-fluid models to obtain tractable computational fluid models. In the present work, the hydrodynamic behavior of a three dimensional, industrial scale, and rotating drum granulator with gas−solid flows is assessed using the Eulerian−Eulerian approach coupled with the k-ε standard turbulence model. A Eulerian−Eulerian Two-Fluid Model (TFM) is used with the KTGF model for the granular phase. The sensitivities to different operating parameters, including the rotational speed (8, 16, and 24 rpm), inclination degree (3.57∘, 5.57∘, and 7.57∘), and degree of filling (20%, 30%, and 40%) are studied. Moreover, the impact of the drag model on the simulation accuracy is investigated. The flow behavior, regime transitions, and particle dis... [more]

The effect of forced periodic modulation of several input parameters on the rate of photocatalytic decomposition of formic acid over a TiO2 thin film catalyst has been investigated in a continuously stirred tank reactor. The kinetic model was adopted based on the literature and it includes acid adsorption, desorption steps, the formation of photocatalytic active sites and decomposition of the adsorbed species over the active titania sites. A reactor model was developed that describes mass balances of reactive species. The analysis of the reactor was performed with a computer-aided nonlinear frequency response method. Initially, the effect of amplitude and frequency of four input parameters (flowrate, acid concentration, temperature and light intensity) were studied. All single inputs provided only a minor improvement, which did not exceed 4%. However, a modulation of two input parameters, inlet flowrate and the acid molar fraction, considerably improved the acid conversion from 80 to 9... [more]

An experimental study was conducted in this work to investigate the effect of different configurations on bubble cutting and process intensification in a micro-structured jet bubble column (MSJBC). Hydrodynamic parameters, including bubble size, flow field, liquid velocity, gas holdup as well as the interfacial area, were compared and researched for a MSJBC with and without mesh. The bubble dynamics and cutting images were recorded by a non-invasive optical measurement. An advanced particle image velocimetry technique (digital image analysis) was used to investigate the influence of different configurations on the surrounding flow field and liquid velocity. When there was a single mesh and two stages of mesh compared with no mesh, the experimental results showed that the bubble size decreased by 22.7% and 29.7%, the gas holdup increased by 5.7% and 9.7%, and the interfacial area increased by more than 34.8% and 43.5%, respectively. Significant changes in the flow field distribution cau... [more]

The growing interest in intensified process units that improve efficiency by combining several phenomena into one unit, has led to a loss in degrees of freedom when addressing the control scheme of these units. Previous work demonstrated that a novel module-based design approach to membrane reactors could improve the operability index of membrane reactor systems. This approach sought to decouple the phenomena to regain some degrees of freedom for the control system. However, the computational time to determine such an optimal module design made this class of design problems intractable to solve in a reasonable amount of time. This work proposes a set of design heuristics for a new module-based design approach for membrane reactors. These heuristics are used in combination with a genetic algorithm formulation to produce a novel, two-staged algorithm for the design and control of membrane reactor systems. This algorithm is developed in Python and uses rigorous membrane reactor models bui... [more]

Process Intensification (PI) is a vast and growing area in Chemical Engineering, which deals with the enhancement of current technology to enable improved efficiency; energy, cost, and environmental impact reduction; small size; and better integration with the other equipment. Since process intensification results in novel, but complex, systems, it is necessary to rely on optimization and control techniques that can cope with such new processes. Therefore, this review presents some advancements in the field of process intensification that are worthy of exploring in detail in the coming years. At the end, several important open questions that can be taken into consideration in the coming years are listed.

This paper intends to propose options for climate neutrality concepts by taking non-German international experiences and decisions made into account. Asia-Pacific and Arabic countries do have already same lessons learned by large-scale projects with regard to economic evaluations. Quite a few conceptual studies to generate the climate neutrality of the chemical−pharmaceutical industry in Germany have been published recently. Most of the studies differ even in magnitude but do not refer to or evaluate the other ones. These are all first theoretical feasibility studies. Experimental piloting is not far developed; only few and only stand-alone parts are operated, with no overall concepts. Economic evaluation is missing nearly completely. Economic analysis shows a factor 3 more expensive green technologies. Even if a large optimization potential of about 30% during manufacturing optimization is assumed as significant, cost increases would result. To make green products nevertheless competi... [more]

Global primary energy consumption has increased tenfold over the course of the 20th Century, the availability of non-renewable energy is becoming scarce, and the burning of fossil fuels is leading to global warming. Climate change has now become tangible. The will to act against fossil fuels has become apparent in the western world, and in Germany in particular. This poses a particular challenge for the chemical and pharmaceutical industry, since, in the future, not only will the energy input, but also the feedstock, have to come from non-fossil sources. They must be replaced by carbon capture and utilization, and the exploitation of a circular economy. Concepts for a climate-neutral chemical−pharmaceutical industry have been developed and evaluated. Due to a high predicted consumption of renewable energies and an insufficient expansion of these, Germany will remain an energy importer in the future. The largest consumer in a climate-neutral chemical−pharmaceutical industry will be elec... [more]

For the purpose of the intensification of an industrial-scale gas-liquid process, the implementation in an alternative reactor concept is investigated at Hamburg University of Technology (TUHH) in cooperation with Ehrfeld Mikrotechnik GmbH. Existing process operation data from a bubble column hint at a mass transfer limitation of the gas-liquid reaction. In the project, a jet loop reactor (JLR) is chosen to increase the specific interfacial area between gas and liquid, and thus increase mass transfer, while keeping the reactor system mechanically simple and low-maintenance. For the investigation, a laboratory scale reactor has been designed on the basis of an existing industrial scale process and scaled according to a pilot scale reactor available at TUHH. For scaling, geometric similarity is desired, while specific energy dissipation rate and volumetric gas input are kept constant for the chosen scale-up strategy. Between the two different scales, the reactors are successfully charact... [more]

Ethanol and starch are the main products generated after the processing of corn via dry grinding and wet milling, respectively. Milling generates byproducts including stover, condensed distillers’ solubles, gluten meal, and the dried distillers’ grains with solubles (DDGS), which are sources of valuable compounds for industry including lignin, oil, protein, carotenoids, and phenolic compounds. This manuscript reviews the current research scenario on the valorization of corn milling byproducts with supercritical technology, as well as the processing strategies and the challenges of reaching economic feasibility. The main products recently studied were biodiesel, biogas, microcapsules, and extracts of enriched nutrients. The pretreatment of solid byproducts for further hydrolysis to produce sugar oligomers and bioactive peptides is another recent strategy offered by supercritical technology to process corn milling byproducts. The patents invented to transform corn milling byproducts incl... [more]

Simulated moving bed technology is applied in the field of pharmaceutical, petrochemical and fine chemistry. It shows capability in separating multicomponent mixtures up to high purities. In this work, an attempt was made to optimize the production of 1,1-diethoxybutane (DEB), using the simulated moving bed technology. A fixed bed model is made with good agreement with experimental results. This fixed bed model was expanded to a simulated moving bed model. This model was used to determine the optimum conditions regarding the switching time and flowrates in each section. From this model, the optimum switching time was found to be 2.4 min, and the ratio of liquid flowrate over the solid flowrate in Section 1Section 2Section 3 and Section 4 of the SMBR was found to be 4.24, 1.77, 3.03 and 1.35, respectively. Under those conditions, the productivity was 19.8 kg DEB per liter of adsorbent per day, and the desorbent consumption was 6.1 L of ethanol per kg of DEB. The results were obtained wi... [more]

Spinning disc technology is capable of achieving intensified micromixing within thin liquid films created through large shear rates, typically of the order of 103 s−1, generated by means of fast disc surface rotation. In this study the effect of the high shear on solvent−antisolvent mixing and starch nanoparticle precipitation is reported. Rheological studies of starch solutions at 2% w/v and 4% w/v have demonstrated their shear-thinning behaviour at the large shear rates experienced on the spinning disc surface. The effect of such high shear rate on starch nanoparticle precipitation is investigated alongside solute concentration and several other operating parameters such as flow rate, disc rotational speed, and solvent/antisolvent ratio. A reduction in nanoparticle size has been observed with an increase in starch concentration, although agglomeration was found to be more prevalent amongst these smaller particles particularly at larger flow rates and disc rotational speeds. Micromixi... [more]