Pilot Plant Experiments Research Articles

Process development for advanced simulated moving bed (ASMB) chromatography by parameter refinement using pilot plant experimental data

The advanced simulated moving bed (ASMB) chromatography, which is a new operating strategy in the chromatography process, is proposed and a case study of design and process development is presented. The ASMB strategy divides the operation of the conventional simulated moving bed (SMB) carried out in a single step into five substeps. A detailed analysis based on simulation is carried out, which shows improvement in purity and recovery over the conventional SMB process. The model mismatch in the complex operations is resolved by a novel parameter estimation approach, where multiple data sets obtained from pilot plant experiments refine the model parameters. It was demonstrated in a separation case study of glucose and fructose that the proposed model refinement approach using 20 data sets from ASMB pilot plant experiments improves the prediction from the one obtained only through a single-column chromatography experiment. The refined model will be a powerful tool for the design and control of the ASMB process.

Efficient and Simple Gaussian Process Supported Stochastic Model Predictive Control for Bioreactors using HILO-MPC

Model-based control of biotechnological processes is, in general, challenging. Often the processes are complex, nonlinear, and uncertain. Hence modeling tends to be complex and is often inaccurate. For this reason, non-model-based control strategies developed via fask, bench-scale, or pilot plant experiments are often applied in the biotechnology industry. Model-based control and optimization techniques can increase processes’ performance and automation level, thereby decreasing costs and guaranteeing the desired specifications. These rely on a model of the process to make predictions and optimize the inputs to the plant. To improve the quality of the models, it is often helpful to use combined first principle and data-driven models together in a hybrid modeling approach which increases the model prediction capabilities. The residual uncertainty of the hybrid model should be taken into account in the control level to satisfy the process specifications and constraints. This paper proposes to use a stochastic model predictive control scheme that exploits a hybrid, Gaussian processes-based model. We outline the effectiveness of the stochastic model-based approach in combination with a suitable Kalman filter for state estimation considering an example biotechnological process. Furthermore, we underline that appropriate tools exist that allow the simple application of such methods even for the novice user. To do so, we use an open-source Python package — HILO-MPC, which allows the simple yet efficient formulation and solution of machine learning-supported optimal control and estimation problems.

Bypassing thermodynamic limitations in the Crystallization-based separation of solid solutions

• A new hybrid process to bypass alyotrope. • Process simulation of antisolvent and evaporative crystallization. • Pilot plant experiments guided by simulated data. • Measurements of solubility, and phase diagram of quaternary system. • New graphical method to represent process paths inside a distribution diagram. Separation of solid solution forming systems into their constituents using crystallization processes is very challenging. We demonstrate the separation of L–valine and L–leucine solid solutions using a new hybrid process of evaporation and antisolvent crystallization. This system of two amino acids is characterized by alyotropic behavior. Bypassing the alyotrope via proposed new method is the main feature of the process. The change of pure component solubilities and the composition of the alyotrope with addition of antisolvent (ethanol) is quantified. Based on these solubility measurements, empirical modelling and process simulation the concept was validated in a pilot plant scale. Moreover, Powder X-Ray Diffraction (PXRD), (pseudo)-ternary and Roozeboom diagrams are exploited to deepen process understanding. Additionally, a simple graphical determination of the supersaturation using the Roozeboom diagram is proposed and demonstrated. The successful isothermal bypassing of the alyotrope at larger scale can be directly integrated into a dual counter-current crystallization setup. To achieve further improvements, this concept can be combined with a similar concept based on bypassing the double saturation point by changing temperature.

Pilot Plant Experiments for Extraction Of Inorganic Products from Agro Solid Waste and Cost Estimation of the Products

Pilot Plant Experiments for Extraction Of Inorganic Products from Agro Solid Waste and Cost Estimation of the Products

Wood ash biomethane upgrading system: A case study

In this work, a biomethane fuel was obtained from biogas, using a solid matrix of ashes obtained from a central heating plant fed by wood. Biomethane composition was studied in an experimental pilot plant that treats organic waste through dry anaerobic digestion. European limits were considered and respected for the biomethane injection into the gas grid. The process was able to completely remove carbon dioxide (CO2) during its initial phase. After 50 h of test CO2 concentration started to appear in the outlet gas. This behaviour is related to the ash content, reactive phases (e.g., Ca hydroxides) and fine particle size (<0.2 mm). Coupled with the CO2 removal, European limits for the biomethane injection into the gas grid must consider also trace compounds (Limits for Sulphur 150 mg/Nm3 and CO2 3%vol.). After 95 h of the experimental test, the gas injection limits are still maintained both for total sulphur trace compounds and both for CO2 limits. Uptake of 0.7 g/kg for H2S and 115 gCO2/kgash were registered from the pilot plant.

Optimization of Spiral-Wound Microfiltration Process Parameters for the Production of Micellar Casein Concentrate.

A systematic selection of different transmembrane pressures (TMP) and levels of diafiltration (DF) was studied to optimize these critical process parameters during the manufacturing of micellar casein concentrate (MCC) using spiral-wound polymeric membrane filtration. Three TMPs (34.5, 62.1, and 103.4 kPa) and four DF levels (0, 70, 100, and 150%) were applied in the study. The effect of the TMP and DF level on flux rates, serum protein (SP) removal, the casein-to-total-protein ratio, the casein-to-true-protein ratio, and the rejection of casein and SP were evaluated. At all transmembrane pressures, the overall flux increased with increases in the DF level. The impact of DF on the overall flux was more pronounced at lower pressures than at higher pressures. With controlled DF, the instantaneous flux was maintained within 80% of the initial flux for the entire process run. The combination of 34.5 kPa and a DF level of 150% resulted in 81.45% SP removal, and a casein-to-true-protein ratio of 0.96. SP removal data from the lab-scale experiments were fitted into a mathematical model using DF levels and the square of TMPs as factors. The model developed in this study could predict SP removal within 90–95% of actual SP removal achieved from the pilot plant experiments.

Effect of Reaction Time and Hydrothermal Treatment Time on the Textural Properties of SBA-15 Synthesized Using Sodium Silicate as a Silica Source and Its Efficiency for Reducing Tobacco Smoke Toxicity

The synthesis of SBA-15 has been optimized using sodium silicate, an inexpensive precursor of SBA-15. In this work, the influence of synthesis times of the precipitation and the hydrothermal treatment steps, on the textural properties developed as well as for reducing the toxic compounds generated in tobacco smoking, has been studied. The hydrothermal treatment has been proved to be necessary to obtain materials with adequate performance in this particular application. Twenty-four hours of hydrothermal treatment provide materials with the best properties. Although the reaction stage usually involves the mixing of reagents during 24 h, 40 min is enough to obtain a material with stick-like morphology and typical textural properties. Moreover, between 1 and 2 h of reaction time, the material proved to have the best performance for the purpose of reducing the toxicity of the products generated during the tobacco smoking process. These results are of great significance for an eventual scaling up to industrial scale of the SBA-15 manufacturing process. Results of a pilot plant experiment in a batch of 4 kg of SBA-15 are reported.

Pyrolysis yields of tobacco crop residue as a potential alternative fuel source

This study aims to utilize the tobacco crop residue to generate a high economic value for the energy sector. In general notion, tobacco crop is burned as a conventional fuel at low prices; however, in this research, tobacco crop residue was processed through pyrolysis in the form of pyrolysis products (liquid and solid yields) providing a promising alternative fuel fulfilling the standardized fuel properties. The pyrolysis was conducted at a laboratory-scale real pilot plant experiment at a fixed bed reactor and was operated at temperature of around 350 °C to 650 °C for 2 hours to navigate the most optimum product. Further, the products comprising char (solid yield) and tar (liquid yield) were investigated by measuring their properties, which include heating value, flash point, viscosity, density, and char yields’ morphology. The measurement results indicated that the heating value of tobacco crop residue from pyrolysis process significantly escalated to 300% compared to that of tobacco crop residue before pyrolysis process. Similarly, several tar properties indicated the liquid fuel standard such as kerosene. Additionally, another product in the form of solid yields is proved to be utilized as a smart material besides having a higher heating value over coal, due to the high-quality carbon specifications. However, further processing is encouraged to navigate the possibility of solid yields into activated carbon.

Preliminary study of a closed loop vertical ground source heat pump system for an experimental pilot plant (Rome, Italy)

A system for capturing thermal energy is planned for installation at the ENEA-Casaccia centre (Italy). Costs, primary energy requirements, pollutant emissions and seasonal electricity consumption were estimated. The configuration based on four boreholes of different depths and the sizing of the vertical loop (double-U) were performed according to the ASHRAE method. This pilot plant, the first under construction within an Italian research centre, is part of a long-term research project funded by the Italian Ministry of Economic Development. The results of this research could be applied throughout the Italian Tyrrhenian Apennine margin, which is geologically characterised by highly conductive lithotypes.

Application of a wire-mesh sensor for the experimental characterization of liquid distribution in packed columns

Characteristic design parameters for fluid dynamics and mass transfer of packed column internals are usually obtained from laboratory or pilot plant experiments. At this scale, results are often affected by liquid maldistribution. Knowledge of liquid distribution is necessary to quantify the influence of maldistribution on mass transfer efficiency and helps to prevent an overdesign of industrial packed columns. The applicability of a minimally invasive wire-mesh sensor for distribution measurements is investigated and a measuring and evaluation method is developed and applied to investigate liquid distribution for the Pall Ring 25, the Raschig Super Ring 0.6 and the Montz Pak B1.250. The results for both, tracer, and integral liquid distribution, show a high reproducibility and are in good agreement with published liquid distribution behavior. The wire-mesh sensor can provide valuable results as a supplement or alternative to liquid collectors with little additional experimental effort in fluid dynamics and mass transfer measurements.

Adjustment of Olive Fruit Temperature before Grinding for Olive Oil Extraction. Experimental Study and Pilot Plant Trials

Harvesting at high temperatures and bulk transport can negatively influence the quality of olives and lead to undesirable alterations in the extracted oil. Cooling the fruit in the field would be the most logical solution, but it means that the olives arrive too cold at the mill for immediate processing. In this work, the use of warm water in the washing tub to warm up the fruit before grinding instead of flash heat treatment on the paste was assessed in two experiments. In the first one, at the laboratory level, the temperature after milling was determined in three olive cultivars, previously stored at 5 or 10 °C, and then submerged at different water temperatures (25, 30, and 35 °C) for 15, 30, 45, and 60 s. In the second one, two batches of olives were cooled in the field at 5 °C and then conditioned with washing water to obtain a paste at the entrance of the pilot plant malaxer at 27 °C. The temperature of the olives was measured at five points from the discharging up to their entering, as paste, into the malaxer. The results demonstrated the feasibility of the method as the temperature of the ground olives was kept at the desired temperature (28 ± 1 °C). The trials highlight the potential for automating an even more precise adjustment of the temperature of the olives before milling once the washing tub is equipped with a safe heating system.

Combustion Melting Characterisation of Solid Fuel Obtained from Sewage Sludge

Solid fuelization technology can increase the heating value of sewage sludge such that it can be utilised as a fossil fuel substitutes. Reducing landfilling of bottom and fly ash resulting from heavy metals contained in sewage sludge is challenging. Hence, combustion melting technology (CMT), which can discharge bottom ash in the form of slag, has been proposed herein as an alternative to the conventional incineration technology. However, further research is required to improve the flowability of slag. Applicability of CMT for the stable treatment of heavy metals in the ash generated during the energisation of sewage sludge solid fuel has been reviewed. The change in the degree of fluidity was identified via a laboratory-scale fluidity measurement experiment following changes in melting temperature, mixing ratio of sewage sludge and sawdust, and basicity. The pouring index (PI) of sewage sludge solid fuel (pellet) was maintained at a level of about 60% at a basicity index of 0.8. Based on the results, the slagging rates and volume reduction rates, exhaust gas analysis, and heavy metal elution characteristics under oxygen enrichment were derived from a 2 ton/day combustion melting pilot plant experiment; thereafter, the feasibility of combustion melting of sewage sludge solid fuel was determined.

Validation of Differential Temperature Control for a Dividing Wall Distillation Column

A novel dividing wall distillation column (DWC) control strategy was investigated using pilot plant experimentation and commercial scale column dynamic simulation. Results from both indicated that the differential temperature, PID based, control structure successfully rejected flow and composition disturbances. A four-component test system was utilized with three primary components and one trace component. Desired purities were achieved and steady state operation was maintained. The simulation results qualitatively matched the pilot plant data with discrepancies being attributed to equipment-scale dependent heat transfer effects.

Time-Delay Identification and Validation of a Liquid Film Transport Model based on Pilot Plant Experiments

Abstract The paper presents an identification strategy to obtain relations between time delays of a transport model for an evaporating liquid film and corresponding flow/liquid properties. To this end, step-response based pilot plant experiments referring to the falling film evaporator process are conducted. In this context, the time-delay relations are identified offline by minimizing the output error between the model and experiment. In subsequent validation experiments, we observe that modeled and measured outputs are in good accordance. Within this framework, we conclude that the influence of evaporation on the liquid’s time-delay behavior can be neglected.

Economic Effect of Dust Particles on Photovoltaic Plant Production

The performance of photovoltaic panels decreases depending on the different factors to which they are subjected daily. One of the phenomena that most affects their energy production is dust deposition. This is particularly acute in desert climates, where the level of solar radiation is extreme. In this work, the effect of dust soiling is examined on the electricity generation of an experimental photovoltaic pilot plant, installed at the Solar Energy Research Center (CIESOL) at the University of Almería. An average reduction of 5% of the power of a photovoltaic plant due to dust contamination has been obtained, this data being used to simulate the economic effect in plants of 9 kWp and 1 and 50 MWp. The economic losses have been calculated, and are capable of being higher than 150,000 €/year in industrial plants of 50 MWp. A cleaning strategy has also been presented, which represents a substantial economic outlay over the years of plant operation.

Commissioning of the LPCE and purification systems as front-end of the experimental pilot plant for D-T separation

Abstract Liquid Phase Catalytic Exchange (LPCE) as front-end process and Cryogenic Distillation (CD) as back-end process are key processes in detritiation of heavy water used in Cernavoda CANDU-type Nuclear Power Plant (NPP) from Romania as neutron moderator and in the primary heat transfer system. Same technology is used in the Water Detritiation System (WDS) of International Thermonuclear Experimental Reactor (ITER) from Cadarache, France, in order to recover tritium from moderately tritiated water. The purpose of this paper is to give a detailed overview of the current status for the front-end of the ICSI pilot plant, LPCE and purification systems, including all process components. Additionally, the paper will present the results of the non-radiological commissioning of the actual LPCE. The tests were made using protium and deuterium in order to have the confirmation of fully availability for all systems, to verify the operability in manual and automate mode for all sequences involved by start-up, normal operation and safe shut-down of the installation. The principal results consist in the safety and operability design confirmation. Secondly we present the mass transfer data of LPCE column equipped with catalytic package COMPACK C–P 001 consisting of the structured B7 stainless steel packing manufactured and patented by ICSI and a Pt/C/PTFE hydrophobic catalyst at the commissioning low concentration heavy water tests.

Oxidative removal of soluble divalent manganese ion by chlorine in the presence of superfine powdered activated carbon

Here, we examined the removal of soluble divalent manganese (Mn(II)) by combination treatment with superfine powdered activated carbon (SPAC) and free chlorine in a membrane filtration pilot plant and batch experiments. Removal rates >95% were obtained with 3 mg/L SPAC, 1 mg/L chlorine, and a contact time of 4 min, meeting practical performance standards. Mn(II) was found to be oxidized and precipitated on the surface of the activated carbon particles by chlorine. The Mn(II) removal rate was fitted to pseudo-first-order reaction kinetics, and the rate coefficient changed in inverse proportion to as-is particle size, but not to true particle size. The rate coefficient was independent of both Mn(II) concentration, except at high Mn(II) concentration, and the chlorine concentrations tested. The rate-determining step of Mn(II) removal was confirmed to be external-film mass transfer, not chemical oxidation. Activated carbon was found to have a catalytic effect on the oxidation of Mn(II), but the effect was minimal for conventionally sized activated carbon. However, Mn(II) removal at feasible rates for practical application can be expected when the activated carbon particle diameter is reduced to several micrometers. Activated carbon with a particle size of around 1–2 μm may be the most appropriate for Mn(II) removal because particles below this size were aggregated, resulting in reduced removal efficiency.

An innovative approach for resin infusion and impregnation processes of a commercial resin-impregnated paper bushing

In the present analysis, a new experimental pilot plant system for exploring resin-impregnated paper (RIP) bushing technology was conducted. Experimental and numerical studies were carried out on the resin infusion and impregnation processes in the paper condenser core of a RIP bushing. An innovative approach for the molding process (named molding method B) of a commercial RIP bushing was implemented. For this method, the homogeneity of the paper winding process was controlled precisely. The filling process was conducted by gravity due to the difference of heights between two vacuumed chambers and from bottom to top in the mold. The flow front position and infusion time were measured experimentally and used to obtain the axial permeability of the paper condenser core analytically and numerically. The results indicate that the molding methods have a significant effect on the RIP bushing quality, homogeneous filling, and impregnating process time. Also, it was found that homogeneity of the paper winding process and, consequently, uniform axial velocity of resin flow in the radial direction is the most effective factor to eject the air. Finally, it was recognized that the determination of axial permeability in the case of transient flow is novel in comparison with conventional procedures such as Darcy relation of steady flows. By decreasing the paper thickness from 0.3 to 0.2 mm, the permeability decreased from 8.84 × 10−10 to 4.52 × 10−10 m2. The microstructure of the core illustrates that the axial permeability of the crepe paper condenser core is considerably affected by the variation of the paper thickness.

Accurate voidage prediction in fluidisation systems for full-scale drinking water pellet softening reactors using data driven models

In full-scale drinking water production plants in the Netherlands, central softening is widely used for reasons related to public health, client comfort, and economic and environmental benefits. Almost 500 million cubic meters of water is softened annually through seeded crystallisation in fluidised bed reactors. The societal call for a circular economy has put pressure on this treatment process to become more sustainable. By optimising relevant process conditions, the consumption of chemicals can be reduced, and raw materials reused. Optimal process conditions are feasible if the specific crystallisation surface area in the fluidised bed is large enough to support the performance of the seeded crystallisation process. To determine the specific surface area, crucial variables including voidage and particle size must be known. Numerous models can be found in the literature to estimate the voidage in liquid-solid fluidisation processes. Many of these models are based on semi-empirical porous-media-based drag relations like Ergun or semi-empirical terminal-settling based models such as Richardson-Zaki and fitted for monodisperse, almost perfectly round particles. In this study, we present new voidage prediction models based on accurate data obtained from elaborate pilot plant experiments and non-linear symbolic regression methods. The models were compared with the most popular voidage prediction models using different statistical methods. An explicit model for voidage estimation based on the dimensionless Reynolds and Froude numbers is presented here that can be used for a wide range of particle sizes, fluid velocities and temperatures and that can therefore be directly used in water treatment processes such as drinking water pellet softening. The advantage of this model is that there is no need for applying numerical solutions; therefore, it can be explicitly implemented. The prediction errors for classical models from the literature lie between 2.7 % and 11.4 %. With our new model, the voidage prediction error is reduced to 1.9 %.

Preoperational Monitoring of an Experimental Pilot Plant for Tritium and Deuterium in Surface Water at Valcea, Romania

The paper reports the monitoring of the surface water radioactivity variations in the region surrounding the Experimental Pilot Plant for Tritium and Deuterium Separation for an experimental period with a duration of one year. The primary goal of the radioactivity monitoring of the environmental factors in the preoperative stage is to establish the baseline levels of radioactive concentrations present in the environment. Two surface water sampling points in the Olt River, Valcea, Romania were selected. The first was upstream of the discharge point of the “Deversor Olt” as the background location and the second was downstream of the liquid effluent discharge point as the indicator location. The activity concentration measurements were carried out on surface water samples from locations established on the Olt River in the vicinity of the magistrate channel “Deversor Olt” on a weekly basis. The employed analytical methodology was high resolution gamma ray spectrometry with the use of a high purity germanium detector. The observed activity concentration for 40K was less than 1.17 Bq·l−w. The activities of the analyte radionuclides, including 7Be, 51Cr, 60Co, 65Zn, 137Cs, 226Ra, 235U, were below the detection limits. The results recorded for the background location were slightly different compared with the values recorded in the indicator location, but the differences were statistically insignificant. The nuclear activity in the preoperational stage of the Experimental Pilot Plant for Tritium and Deuterium Separation facility has not had any impact on the environment to date. This study creates a unique database that may be relevant for further operational monitoring of the Experimental Pilot Plant for Tritium and Deuterium Separation.