Processes — Open Access Journal of Chemical and Biological Process Engineering

This paper presents an interactive tool focused on the study of proportional-integral-derivative (PID) controllers. Nowadays, PID control loops are extensively used in industrial applications. However, it is reported that many of them are badly tuned. From an educational point of view, it is essential for undergraduate students in control engineering to understand the importance of tuning a control loop correctly. For this reason, the tool provides different PID tuning methods in the frequency domain for stable open-loop time-delay-free processes. The different designs can be compared interactively by the user, allowing them to understand concepts about stability, robustness, and performance in PID control loops. A survey and a comparative study were performed to evaluate the effectiveness of the proposed tool. Full article

In situ gasification chemical looping combustion (iG-CLC) is a novel and promising coal combustion technology with inherent separation of CO₂. Our previous studies demonstrated the feasibility of performing iG-CLC with a high-flux circulating fluidized bed (HFCFB) riser as the fuel reactor (FR) and a counter-flow moving bed (CFMB) as the air reactor (AR). As an extension of that work, this study aims to further investigate the fundamental effects of the AR coupling on the oxygen carrier (OC) circulation and gas leakages with a cold-state experimental device of the proposed iG-CLC system. The system exhibited favorable pressure distribution characteristics and good adaptability of solid circulation flux, demonstrating the positive role of the direct coupling method of the AR in the stabilization and controllability of the whole system. The OC circulation and the gas leakages were mainly determined by the upper and lower pressure gradients of the AR. With the increase in the upper pressure gradient, the OC circulation flux increased initially and later decreased until the circulation collapsed. Besides, the upper pressure gradient exhibited a positive effect on the restraint of gas leakage from the FR to the AR, but a negative effect on the suppression of gas leakage from the AR to the FR. Moreover, the gas leakage of the J-valve to the AR, which is directly related to the solid circulation stability, was exacerbated with the increase of the lower pressure gradient of the AR. In real iG-CLC applications, the pressure gradients should be adjusted flexibly and optimally to guarantee a balanced OC circulation together with an ideal balance of all the gas leakages. Full article

In this present work, a study of the modelling and simulation for a top-sprayed fluidized bed granulator (SFBG) is presented, which is substantially used by the pharmaceutical industry to prepare granules. The idea is to build a number-based mathematical model using the notion of population balances by dividing a top SFBG into two different zones, namely the wet zone and dry zone. To solve a two-compartment model, an existing accurate and efficient finite volume scheme is implemented. In order to validate the compartmental model, a new class of analytical moments is derived corresponding to various combinations of aggregation and breakage kernels. To verify the accuracy of a modified finite volume scheme, the zeroth and first order moments computed using the finite volume scheme are compared with the newly-derived analytical results. Moreover, the stability of the compartmental model and the numerical scheme is tested by varying the size of the wet zone. It is also shown that the relative errors in both order moments increase with the increase in the size of the wet zone. Full article

This study investigates the effect of carbon nanotube (CNT) dispersion on the mechanical properties and microstructures of ultra-light foamed concrete. A type of uniform and stable CNT dispersion solution is obtained by adding nano-Ce(SO₄)₂. Results show that CNT dispersion increases the compressive and breaking strengths of foamed concrete. CNTs play a nuclear role in the crystallization of C–S–H, and CNT dispersion effectively promotes the grain growth of C–S–H. The effect of CNT dispersion on the compressive and breaking strengths of foamed concrete is predicted through simulation. Full article

Natural gas liquefaction is an energy intensive process where the feed is cooled from ambient temperature down to cryogenic temperatures. Different liquefaction cycles exist depending on the application, with dual mixed refrigerant processes normally considered for the large-scale production of Liquefied Natural Gas (LNG). Large temperature spans and small temperature differences in the heat exchangers make the liquefaction processes difficult to analyze. Exergetic losses from irreversible heat transfer increase exponentially with a decreasing temperature at subambient conditions. Consequently, an accurate and robust simulation tool is paramount to allow designers to make correct design decisions. However, conventional process simulators, such as Aspen Plus, suffer from significant drawbacks when modeling multistream heat exchangers. In particular, no rigorous checks exist to prevent temperature crossovers. Limited degrees of freedom and the inability to solve for stream variables other than outlet temperatures also makes such tools inflexible to use, often requiring the user to resort to a manual iterative procedure to obtain a feasible solution. In this article, a nonsmooth, multistream heat exchanger model is used to develop a simulation tool for two different dual mixed refrigerant processes. Case studies are presented for which Aspen Plus fails to obtain thermodynamically feasible solutions. Full article

A mixture of sandstone and mudstone particles is often used as the main filling material for many agriculture-related and civil engineering projects, including rock-fill dams and foundations. The long-term rheological deformation experienced by rock-fill dams and foundations filled with this mixture is much bigger than that of coarse-grained and cohesive soils, due to the deterioration and softening of the mudstone particles. This study focuses on the rheological deformation of a sandstone-mudstone particle mixture, prepared by mixing sandstone and mudstone particles, based on the content by weight of four mudstone particle types. Confined uniaxial compression tests were performed to test the rheological deformation of 24 samples of the mixture, and a stress-strain curve was obtained for each test. On the basis of compression curves, the rheological process of the mixture was divided into four phases: linear, attenuation rheological, secondary attenuation rheological and stable phases. The three defining features of the curve, namely the rheological attenuation factors, attenuation rheology critical strain and limited rheological strain, were then determined and modeled. A segmented rheological model was then proposed, based on a modified attenuation rheological constitutive model for coarse-grained soil. The modelled results compared well with the experimental data, and the modelled compression-curve prediction was able to describe the two-stage attenuation rheology features (attenuation rheological and secondary attenuation rheological phases) of the sandstone-mudstone particle mixture. Full article

Because of the limitation of mining techniques and economic conditions, large amounts of residual coal resources have been left in underground coal mines around the world. Currently, with mining technology gradually developing, residual coal can possibly be remined. However, when residual coal is remined, caving areas might form, which can seriously affect the safety of coal mining. Hence, grouting technology is put forward as one of the most effective technologies to solve this problem. To study the grouting diffusion in fractured rock mass, this paper developed a visualization platform of grouting diffusion and a three-dimensional grouting experimental system that can monitor the grout diffusion range, diffusion time and grout pressure; then, a grouting experiment is conducted based on this system. After that, the pattern of the grouting pressure variation, grout flow and grout diffusion surface are analyzed. The relationship among some factors, such as the grouting diffusion radius, compressive strength of the grouted gravel, porosity, water-cement ratio, grouting pressure, grouting time, permeability coefficient and level of grout, is quantitatively analyzed by using MATLAB. The study results show that the flow pattern of the grout in fractured porous rock mass has a parabolic shape from the grouting hole to the bottom. The lower the level is, the larger the diffusion range of the grout is. The grouting pressure has the greatest influence on the grouting diffusion radius, followed by the grouting horizon and water-cement ratio. The grouting permeability coefficient has the least influence on the grouting diffusion radius. The grout water-cement ratio has the greatest influence on the strength of the grouted gravel, followed by the grouting permeability. The grouting pressure coefficient has the least amount of influence on the grouting diffusion radius. According to the results, the grouting parameters are designed, and a layered progressive grouting method is proposed. Finally, borehole observation and a core mechanical property test are conducted to verify the application effect. This grouting technology can contribute to the redevelopment and efficient utilization of wasted underground coal resources. Full article

The mechanical properties and seepage characteristics of gas-bearing coal evolve with changes in the loading pattern, which could reveal the evolution of permeability in a protected coal seam and allow gas extraction engineering work to be designed by using the effect of mining multiple protective seams. Tests on gas seepage in raw coal under three paths (stepped-cyclic, stepped-increasing-cyclic, and crossed-cyclic loading and unloading) were carried out with a seepage tester under triaxial stress conditions. The permeability was subjected to the dual influence of stress and damage accumulation. After being subjected to stress unloading and loading, the permeability of coal samples gradually decreased and the permeability did not increase before the stress exceeded the yield stage of the coal samples. The mining-enhanced permeability of the coal samples in the loading stage showed a three-phase increase with the growth of stress and the number of cycles and exhibited an N-shaped increase under the stepped-cyclic loading while it linearly increased under the other two paths in the unloading stage. With the increase of peak stress and the accumulation of damage in coal samples, the sensitivity of the permeability of coal samples to stress gradually declined. The relationship between the damage variable and the number of cycles conformed to the Boltzmann function. Full article

The aim of this study was to microencapsulate an optimized extract of purple cactus pear fruit (Opuntia ficus indica), rich in phenolic compounds (PC), betacyanins (BC), and betaxanthins (BX), with antioxidant capacity (AC), by two methodologies: combined water-in-oil-in-water double emulsions-spray drying (W/O/W-SP) and conventional spray drying, studying the effect of spray drying (SP) on PC and AC. Optimal extraction conditions for bioactive compounds were: 52 °C, for 30 min, using aqueous ethanol (40%_w/w) as the solvent, with a 0.85 desirability function, obtaining 17.39 ± 0.11 mg GAE/g_dw (gallic acid equivalents per gram of dry weight) for PC, 0.35 mg BE/g_dw (betanin equivalents per gram of dry weight) for BC, and 0.26 mg IE/g_dw (indicaxanthin equivalents per gram of dry weight) for BX. The best combination of temperatures for conventional SP and W/O/W-SP was 160–80 °C obtaining the highest retention and encapsulation efficiencies for PC. For conventional SP, results were: 107% and 100% PC and AC retention efficiencies (RE-PC and RE-AC), respectively, with 97% of PC encapsulation efficiency (EE-PC), meanwhile for the W/O/W-SP results were: 78% and 103% RE-PC and RE-AC, respectively, with 70% of EE-PC. Microcapsules obtained with W/O/W-SP maintained their structure and integrity and showed a considerable reduction in globule size in the reconstituted W/O/W emulsions due to the spray drying stress. Despite having lower EE-PC than conventional SP, spray dried W/O/W emulsions seem as a promising controlled-delivery vehicle for antioxidant compounds. Full article

The genetic modification of human T lymphocytes with established non-viral methods is inefficient. Linear polyethylenimine (l-PEI), one of the most popular non-viral transfection agents for mammalian cells in general, only achieves transfection rates in the single digit percentage range for these cells. Here, a well-defined 24-armed poly(2-dimethylamino) ethyl methacrylate (PDMAEMA) nanostar (number average of the molecular weight: 755 kDa, polydispersity: <1.21) synthesized via atom transfer radical polymerization (ATRP) from a silsesquioxane initiator core is proposed as alternative. The agent is used to prepare polyplexes with plasmid DNA (pDNA). Under optimal conditions these polyplexes reproducibly transfect >80% of the cells from a human T-cell leukemia cell line (Jurkat cells) at viabilities close to 90%. The agent also promotes pDNA uptake when simply added to a mixture of cells and pDNA. This constitutes a particular promising approach for efficient transient transfection at large scale. Finally, preliminary experiments were carried out with primary T cells from two different donors. Results were again significantly better than for l-PEI, although further research into the response of individual T cells to the transfection agent will be necessary, before either method can be used to routinely transfect primary T lymphocytes. Full article

Multicellular systems play an important role in many biotechnological processes. Typically, these exhibit cell-to-cell variability, which has to be monitored closely for process control and optimization. However, some properties may not be measurable due to technical and financial restrictions. To improve the monitoring, model-based online estimators can be designed for their reconstruction. The multicellular dynamics is accounted for in the framework of population balance models (PBMs). These models are based on single cell kinetics, and each cellular state translates directly into an additional dimension of the obtained partial differential equations. As multicellular dynamics often require detailed single cell models and feature a high number of cellular components, the resulting population balance equations are often high-dimensional. Therefore, established state estimation concepts for PBMs based on discrete grids are not recommended due to the large computational effort. In this contribution a novel approach is proposed, which is based on the approximation of the underlying number density functions as the weighted sum of Gaussian distributions. Thus, the distribution is described by the characteristic properties of the individual Gaussians, like the mean and covariance. Thereby, the complex infinite dimensional estimation problem can be reduced to a finite dimension. The characteristic properties are estimated in a recursive approach. The method is evaluated for two academic benchmark examples, and the results indicate its potential for model-based online reconstruction for multicellular systems. Full article

The objective of the research was to compare the flotation performance of medical waste incinerator fly ash (MWIFA) by considering two methods: the cyclonic-static micro-bubble flotation column (FCSMC) method and conventional flotation cell (CFC) method. The results indicated that for FSCMC, the optimum parameters were kerosene = 3.5 g/kg·ash, methyl isobutyl carbinol (MIBC) = 0.2 g/kg·ash, Tween 80 = 7.5% of kerosene concentration, slurry concentration = 100 g/L, and pump speed = 380 r/min. The optimized conditions resulted in a higher dioxin removal efficiency (90.98%), carbon removal efficiency (91.88%) and lower loss on ignition (LOI) (4.96%). The data obtained from the CFC under different optimum operating conditions were 88.65%, 90.63% and 5.68%, respectively. FSCMC was proven to be more efficient for the flotation of MWIFA than CFC. Full article

Porous medium burners are characterized by high efficiency and good stability. In this study, a new burner was proposed based on the combustion mechanism of the methane-air mixture in the porous medium and the preheating effect. The new burner is a two-section and double-deck porous medium with gas inlets at both ends. A mathematical model for the gas mixture combustion in the porous medium was established. The combustion performance of the burner was simulated under different equivalence ratios and inlet velocities of premixed gas. The methane combustion degree, as well as the temperature and pressure distribution, was estimated. In addition, the concentrations of emissions of NO_x for different equivalence ratios were investigated. The results show that the new burner can not only realize sufficient combustion but also save energy. Furthermore, the emission concentration of NO_x is very low. This study provides new insights into the industrial development and application of porous medium combustion devices. Full article

Bioprocesses for the production of renewable energies and materials lack efficient separation processes for the utilized microorganisms such as algae and yeasts. Dissolved air flotation (DAF) and microflotation are promising approaches to overcome this problem. The efficiency of these processes depends on the ability of microorganisms to aggregate with microbubbles in the flotation tank. In this study, different new or adapted aggregation models for microbubbles and microorganisms are compared and investigated for their range of suitability to predict the separation efficiency of microorganisms from fermentation broths. The complexity of the heteroaggregation models range from an algebraic model to a 2D population balance model (PBM) including the formation of clusters containing several bubbles and microorganisms. The effect of bubble and cell size distributions on the flotation efficiency is considered by applying PBMs, as well. To determine the sensitivity of the results on the model assumptions, the modeling approaches are compared, and suggestions for their range of applicability are given. Evaluating the computational fluid dynamics (CFD) of a dissolved air flotation (DAF) system shows the heterogeneity of the fluid dynamics in the flotation tank. Since analysis of the streamlines of the tank show negligible back mixing, the proposed aggregation models are coupled to the CFD data by applying a Lagrangian approach. Full article

Model-based design principles have received considerable attention in biotechnology and the chemical industry over the last two decades. However, parameter uncertainties of first-principle models are critical in model-based design and have led to the development of robustification concepts. Various strategies have been introduced to solve the robust optimization problem. Most approaches suffer from either unreasonable computational expense or low approximation accuracy. Moreover, they are not rigorous and do not consider robust optimization problems where parameter correlation and equality constraints exist. In this work, we propose a highly efficient framework for solving robust optimization problems with the so-called point estimation method (PEM). The PEM has a fair trade-off between computational expense and approximation accuracy and can be easily extended to problems of parameter correlations. From a statistical point of view, moment-based methods are used to approximate robust inequality and equality constraints for a robust process design. We also apply a global sensitivity analysis to further simplify robust optimization problems with a large number of uncertain parameters. We demonstrate the performance of the proposed framework with two case studies: (1) designing a heating/cooling profile for the essential part of a continuous production process; and (2) optimizing the feeding profile for a fed-batch reactor of the penicillin fermentation process. According to the derived results, the proposed framework of robust process design addresses uncertainties adequately and scales well with the number of uncertain parameters. Thus, the described robustification concept should be an ideal candidate for more complex (bio)chemical problems in model-based design. Full article

No unified electromagnetic anti-fouling mechanism is currently available. Most research has focused on the effects of structural parameters and water quality parameters on electromagnetic fields; variations in water quality parameters under the influence of electromagnetic fields have not been reported. A variable-frequency vertical electromagnetic field is proposed in this study. Relationships between conductivity, pH value, dissolved oxygen, turbidity, fouling resistance, and magnetic acting time were carefully analyzed using statistical analysis. Results show that the conductivity difference was the most explanatory predictive variable on magnetic acting time in the multiple stepwise regression model. Magnetic acting time has a greater impact on conductivity than pH value and dissolved oxygen. Conductivity is used as an adaptive feedback control parameter for the optimum anti-fouling state. Fouling resistance on the heat-exchanging surface of the magnetic experiment was smaller than that of the contrast experiment. The anti-fouling efficiency in 1 kHz and 5 kHz magnetic and contrast experiments was 91.23% and 46.97%, respectively. Better anti-fouling performance was realized under the influence of low-frequency electromagnetic fields, confirming that physical water treatment is an effective and environmentally friendly method to eliminate heat exchanger fouling. This research serves as a reference for the development of an electromagnetic-adaptive closed-loop water treatment device. Full article

In this study, process integration for crystallization of a priori purified Artemisia annua L. is investigated. For this total process, the integration operation boundaries and behavior of the crystals are studied. This is performed focusing on a conceptual process design study for artemisinin, aiming towards the development of a crystallization step under given parameters by process integration. At first, different crystallization systems consisting of ethanol-water or acetone-water mixtures are compared. In subsequent steps, the metastable zone width and the behavior of the crystals regarding agglomeration and breakage are checked. Furthermore, the sensitivities of process variables based on several process parameters are investigated. Additionally, the final process integration of crystallization as a combined purification and isolation step is studied. Full article

In this study, the purification of an extract from Artemisia annua L. using chromatographic methods is studied. In a first step, a screening of different phases and solvents using thin-layer chromatography (TLC) was performed. Then, a laboratory-scale high performance liquid chromatography (HPLC) method was developed and transferred to a pilot scale. A reproducibility study based on 120 injections was carried out. The batch process that was developed and the results from a designed continuous simulated moving bed (SMB) chromatography were compared based on characteristic process numbers and economy. Full article

Liquid-liquid extraction (LLE) is an established unit operation in the manufacturing process of many products. However, development and integration of multistage LLE for new products and separation routes is often hindered and is probably more cost intensive due to a lack of robust development strategies and reliable process models. Even today, extraction columns are designed based on pilot plant experiments. For dimensioning, knowledge of phase equilibrium, hydrodynamics and mass transport kinetics are necessary. Usually, those must be determined experimentally for scale-up, at least in scales of DN50-150 (nominal diameter). This experiment-based methodology is time consuming and it requires large amounts of feedstock, especially in the early phase of the project. In this study the development for the integration of LLE in a new manufacturing process for artemisinin as an anti-malaria drug is presented. For this, a combination of miniaturized laboratory and mini-plant experiments supported by mathematical modelling is used. System data on extraction and washing distributions were determined by means of shaking tests and implemented as a multi-stage extraction in a process model. After the determination of model parameters for mass transfer and plant hydrodynamics in a droplet measurement apparatus, a distributed plug-flow model is used for scale-up studies. Operating points are validated in a mini-plant system. The mini-plant runs are executed in a Kühni-column (DN26) for extraction and a packed extraction column (DN26) for the separation of side components with a throughput of up to 3.6 L/h, yield of up to 100%, and purity of 41% in the feed mixture to 91% after washing. Full article