Laboratory-scale Equipment Research Articles

Integrated Sono-Fenton ultrafiltration process for 4-chlorophenol removal from aqueous effluents: assessment of operational parameters (Part 1)

Advanced oxidation processes (AOPs) and membrane separation processes are successfully used in the final stages of wastewater treatment for recycling and reuse purposes. This research proposes a new two stage process including in the first step a homogeneous Sono-Fenton process (as an AOP), coupled with ultrafiltration (UF), as a cleaner and safer alternative for advanced wastewater treatment, designed specially to enhance the removal of priority organic pollutants which are difficult to eliminate by means of conventional treatments. The aim of this study is to analyze experimentally the performances of an integrated ultrasonication-UF process for the removal of 4-chlorophenol (4CP) (as a model-pollutant for priority organic compounds from wastewaters), both from the removal efficiency (expressed as phenolic concentration and chemical oxygen demand reduction) and the energy consumption point of view. The most important factors with influence on both stages of the proposed process, such as acoustic amplitude, power density, and operating mode for the Sono-Fenton process and pressure, time, operating mode, and cleaning operations for the UF stage, were assessed in this paper (Part 1). The experimental results indicate that the process can be applied for such aqueous effluents, in laboratory scale equipments and represent the basis for modeling the process steps and scale-up of different process arrangements (Cailean et al. (2014): “Integrated Sono-Fenton UF Process for 4CP Removal from Aqueous Effluents: Process Modeling and Simulation (Part 2)”), with the purpose to analyze and control such a process, under various conditions and to understand better its advantages and disadvantages.

Development and characterization of Li-ion capacitor pouch cells

High energy density Li-ion capacitor (LIC) pouch cell prototypes were assembled with lab-scale equipment using activated carbon cathode and hard carbon/lithium stabilized metal power (SLMP) anode. The specific energy and energy density as high as 30 Wh kg−1 and 39 Wh L−1 have been achieved, respectively. The pouch cells can deliver over 50% of the maximum stored energy at a discharge rate over 100 C-rate. After 10,000 cycles, the LIC pouch cell still has 80% of the initial capacitance. The average leakage current is 0.3 μA cm−2 during the first 72 h.

Robustness Considerations and Effects of Moisture Variations on near Infrared Method Performance for Solid Dosage Form Assay

Quantitative analysis by near infrared (NIR) spectroscopy involves the establishment of the relationship between spectra, related to both physical and chemical information of a sample, and the corresponding parameter(s) of interest. To make a model useful and robust, other sources of variability, not directly related to the element(s) to predict should be included in the calibration set. One of the potential sources of variability is moisture. Raw materials may have different moisture levels as a function of the manufacturing lots, the geographic situation of a plant, storage conditions or the season. In a traditional calibration effort, tablets are often made at the same time and no robustness to moisture is built into the model. The present article investigates how moisture variations affect the predictive ability of a NIR calibration model for active ingredient in solid oral dosage forms. Examples of variable selection and orthogonalisation techniques are presented as an alternative to including the moisture variability in the calibration data. Tablets composed of acetaminophen, lactose, microcrystalline cellulose, hypromellose and magnesium stearate were manufactured using laboratory scale equipment. A full-factorial design was used to vary acetaminophen (five levels) and excipient ratios (three levels) to generate tablets for calibration and test. Tablets were placed in humidity chambers over saturated salt solutions and equilibrated to 11%, 32%, 52% and 75% relative humidity, respectively. Calibration and test tablets were scanned at each moisture level. Following spectral collection, the acetaminophen content was determined by HPLC. From each sample set representing tablets equilibrated at a single relative humidity, individual calibration models for acetaminophen were constructed. Test samples, stored at the alternate relative humidity conditions, were predicted. When the moisture level was different between calibration and test sets, the prediction error increased, indicating a degradation of the model performance when moisture variance was unaccounted for. Models developed using selected variable, orthogonalisation and global approaches gave significantly lower prediction errors for the test set than the individual models applied to all samples. These findings demonstrated the importance of accounting for expected sources of variance, such as moisture in order to achieve robust calibrations.

Design and Optimization of a Monomer Processing Reactor

The purpose of this research is to design and to modify a monomer reactor tank in order to achieve higher output production of bio-monomer. The main aspect of this design is based on producing good quality and higher yielding of monomer. The design was started on lab scale process of 2L beaker into a 5L reactor. The most important point of the design is to produce larger amount of monomer as compared to lab scale equipment. Selecting material is vital on the process and cost for fabricating the reactor. It is to prevent chemical corrosion on the reactor and to produce higher yield of monomer with cost effective way. The optimization and analysis of the design and materials of a reactor were based on influence of heat and chemical resistance on the reactor. The design and analysis process were done using Solidworks and chemical resistance were based on the standard chemical chart for common materials used for a reactor. The best material for the reactor is Stainless Steel 316 based on chemical chart, heat resistance and cost effective. The yielding of monomer is more than 100% by lab scale method with predetermined controlled parameters of stirring speed and temperature. There were small differences between every samples. At 80°C, the yielding of monomer is the highest while the by product (water) is the lowest. Meanwhile, at 60°C the monomer yielding is the lowest with highest by-product.

Scaling up Process Output of Monomer Reactor

A monomer processing reactor is a device to process used cooking oil into new substance that can be used for other applications. In this study, used cooking oil was converted to monomer via simple reactor comprised of stirrer started with laboratory scale of 2L to 5L of monomer production. A scale up process is an important process for approaching industrial scale productions. The scale up process was increased to pilot scale before it reaches to industrial scale. The reactor is designed based on lab scale process for producing monomer from used cooking oil. The most important point of the device design is to produce larger amount of monomer compared to lab scale equipment. The device can produce 15liters of monomer per production. The monomer has the same properties and quality of monomer that were produced using laboratory equipment.

Quality by design: scale-up of freeze-drying cycles in pharmaceutical industry.

This paper shows the application of mathematical modeling to scale-up a cycle developed with lab-scale equipment on two different production units. The above method is based on a simplified model of the process parameterized with experimentally determined heat and mass transfer coefficients. In this study, the overall heat transfer coefficient between product and shelf was determined by using the gravimetric procedure, while the dried product resistance to vapor flow was determined through the pressure rise test technique. Once model parameters were determined, the freeze-drying cycle of a parenteral product was developed via dynamic design space for a lab-scale unit. Then, mathematical modeling was used to scale-up the above cycle in the production equipment. In this way, appropriate values were determined for processing conditions, which allow the replication, in the industrial unit, of the product dynamics observed in the small scale freeze-dryer. This study also showed how inter-vial variability, as well as model parameter uncertainty, can be taken into account during scale-up calculations.

Enhancement of Energy Efficiency and Food Product Quality Using Adsorption Dryer with Zeolite

Drying is a basic operation in wood, food, pharmaceutical and chemical industry. Currently, several drying methods are often not efficient in terms of energy consumption (energy efficiency of 20-60%) and have an impact on product quality degradation due to the introduction of operational temperature upper 80oC. This work discusses the development of adsorption drying with zeolite to improve the energy efficiency as well as product quality. In this process, air as drying medium is dehumidified by zeolite. As a result humidity of air can be reduced up to 0.1 ppm. So, for heat sensitive products, the drying process can be performed in low or medium temperature with high driving force. The study has been conducted in three steps: designing the dryer, performing laboratory scale equipment (tray, spray, and fluidised bed dryers with zeolite), and evaluating the dryer performance based on energy efficiency and product quality. Results showed that the energy efficiency of drying process is 15-20% higher than that of conventional dryer. In additon, the dryer can speed up drying time as well as retaining product quality.

FCC testing at bench scale: New units, new processes, new feeds

As the FCC process has evolved over decades, several laboratory scale equipment have appeared to maintain a proper assessment of catalysts activity. Several laboratory equipments are available for simulating the FCC process, from the well known fixed bed, MicroActivity Test to newer, fluid bed or transported bed units. As well, a number of units have been created to simulate other parts of the process such as regenerator or stripper, The increased pressure for treating non-conventional feeds, from reprocessing gasoline to extra-heavy feeds or oils produced from biomass containing large amounts of heteroatoms, increase the needs to have a laboratory test which is as close as possible to the process so that data extraction from the laboratory test are simplified, thus less prone to errors or misunderstanding.

Spray Drying Method for Large-Scale and High-Performance Silicon Negative Electrodes in Li-Ion Batteries

Nanostructured silicon electrodes have shown great potential as lithium ion battery anodes because they can address capacity fading mechanisms originating from large volume changes of silicon alloys while delivering extraordinarily large gravimetric capacities. Nonetheless, synthesis of well-defined silicon nanostructures in an industrially adaptable scale still remains as a challenge. Herein, we adopt an industrially established spray drying process to enable scalable synthesis of silicon-carbon composite particles in which silicon nanoparticles are embedded in porous carbon particles. The void space existing in the porous carbon accommodates the volume expansion of silicon and thus addresses the chronic fading mechanisms of silicon anodes. The composite electrodes exhibit excellent electrochemical performance, such as 1956 mAh/g at 0.05C rate and 91% capacity retention after 150 cycles. Moreover, the spray drying method requires only 2 s for the formation of each particle and allows a production capability of ~10 g/h even with an ultrasonic-based lab-scale equipment. This investigation suggests that established industrial processes could be adaptable to the production of battery active materials that require sophisticated nanostructures as well as large quantity syntheses.

기격 습식 방사를 이용한 면 린터 기반 셀룰로스 재생 섬유 제조 및 평가

Compared to the conventional viscose rayon process, Lyocell process using NMMO as a solvent provides a naturally-friendly, less toxic, relatively simple method for producing regenerated cellulose fiber with excellent properties. Existing wood pulp based Lyocell, however, shows some disadvantages such as forest destruction. So, in this study, a novel regenerated cellulose fiber, cotton linter based Lyocell, was prepared by dry jet-wet spinning with a lab scale equipment changing concentration of cellulose/NMMO solution, take-up speed, etc, which are strongly related with fiber properties and its properties were compared with wood pulp based Lyocell fiber. The tenacity and strain at break of the resultant fibers were correlated with the intrinsic fiber properties such as birefringence, crystallinity, and crystalline orientation index.

Towards High speed Inkjet Printed Electronics – Technology Transfer from S2S to R2R Production

An economically successful implementation of printed electronics technologies in industrial production processes requires high throughput and large scale compatible manufacturing techniques. Roll-to-roll inkjet printing and photonic sintering of metal-based conductive inks on flexible plastic substrates is a promising approach in this respect. It is, however, currently mainly applied on a small scale sheet-to-sheet basis, and technology transfer towards roll-to-roll production has proven to be challenging. Presented here is a stepwise strategy, starting with rather basic, laboratory scale equipment and using small amounts of materials. Based on the outcome of these tests, the experimental scale is successively enlarged and the process conditions continuously optimised, until finally industrial applicability is convincingly demonstrated on a pre-pilot roll-to-roll production line with manufacturing rates of up to 20 m/min. Following this stepwise approach, we were able to scale up the production speed by several orders of magnitude in a purposeful and thus cost and labour efficient way.

Improved Plastic-Al Pipe Based System for Refrigeration of Energy Existed in Urban Sewage

In order to recover the urban sewage energy ,a lab-scale equipment for the sewage energy recovery based on water source heat pump was developed and researched experimentally .The technique of indirect heat exchange by the plastic-Al pipe to recover the urban sewage energy, i.e., the corrosion of the heat exchanger, laying the foundation for the practical utilization of sewage energy. The experimental results show that the developed system is favorable to the environment protection and energy conservation, satisfying the cooling duty requirement with the average coefficient of performance 4.15 in the open cycle system and the average coefficient of performance 3.64 in the close cycle system.

Solid crystal suspensions containing griseofulvin – Preparation and bioavailability testing

The improvement of the bioavailability of poorly soluble drugs has been an important issue in pharmaceutical research for many years. Despite the suggestion of several other technologies in the past, drug particle size reduction is still an appropriate strategy to guarantee high bioavailability of various drugs. A few years ago, the Solid Crystal Suspension (SCS) technology was suggested, in which crystalline drug particles are ground and dispersed in a highly soluble crystalline carrier by a hot melt extrusion process.The current study demonstrates the scale-up of the SCS technology to standard, lab-scale extrusion equipment—a change from previous investigations, which used small batch sizes. A twin-screw extruder was modified to account for the rapid crystallization of the carrier. The screw speed and the barrel temperature were identified as critical process parameters and were varied systematically in several experimental designs. Finally, parameters were identified that produced extrudates with rapid dissolution rates.After extrusion, the extrudates were milled to granules and then tableted. These tablets were investigated with respect to their bioavailability in beagle dogs. It was found that drug particle size reduction in the hot melt extrusion led to 3.5-fold higher bioavailability in these dogs than occurred with the physical mixture of the used substances. The solid crystal suspension formulation had a slightly higher bioavailability than the marked product.In conclusion, the SCS technology was successfully scaled up to lab-scale equipment, and the concept was confirmed by a bioavailability study.

Concentration of liquid whole egg by membrane filtration

One of the most important enriching materials at the processing of alimentary pastes is the egg, which usage is limited because of its water content. Removing water from liquid whole egg with membrane processes, such as ultrafiltration (UF), nanofiltration (NF) and reverse osmosis (RO) was applied for raising the solid content at a temperature of 25 °C at constant flow rate. The separation procedures were carried out on laboratory scale equipments. The initial solid content of the liquid whole egg was 24 refractive (Ref%). The effects of different recirculation flow rates and transmembrane pressure differences were investigated on the permeate flux of the liquid egg. The product had up to 30, 35.5 and 36 Ref% solids in case of UF, NF and RO, respectively. From the resistance data it is obvious, that the polarization layer resistances (RP) determine the values of the permeate flux. The total solid content of permeate was 0.3 and 0.1 Ref% in case of nanofiltration and reverse osmosis, respectively. On the basis of experiments main data of a continuous pilot scale system were calculated and simplified cost estimation was performed using recent economic data of year 2011.

Surface acoustic wave actuated miniaturized lab-on-a-disc (miniLOAD)

Lab-on-a-chip systems offer much potential in next generation diagnostics. Miniaturizing laboratory processes can realize reductions in test times, sample size and cost. This allows for new possibilities such as real time and point of care diagnostic systems. However, lab-on-a-chip systems often require large laboratory scale equipment to drive flow for microfluidic processes. To overcome this challenge, a miniaturized centrifugal based microfluidic platform has been developed. Surface acoustic waves (SAW) are used to generate rotation in a fluid layer, which, in turn, drives the rotation of a disc. Initially, Mylar discs of 5 mm diameter were rotated to greater than 2000 rpm. SU8 discs of dimensions ranging from 250 microns to 10 mm were also actuation and speeds of the order of 10 000 rpm were recorded. The larger 10 mm discs were patterned with various microfluidic structures through the use of photolithography. Common lab-on-a-chip processes are demonstrated including capillary valving, mixing and particle concentration. Currently, work is being carried out to do some basic biological assays on the miniaturized Lab-on-a-disc system.

Scale-Up of a Reaction Chamber for Superhydrophobic Coatings Based on Silicone Nanofilaments

The facile and cheap large-scale production of superhydrophobic surfaces is one of the major challenges to exploit the commercial potential of strongly water-repellent materials. Here, we present the scale-up of a gas-phase reaction process for coating different materials with silicone nanofilaments and rendering them thereby superhydrophobic. As compared to the lab-scale equipment, the chamber volume of the pilot plant is larger by a factor of 1300, and the maximum sample dimension is ∼2 m. Design and technical issues of the pilot plant are presented. The achieved contact angles above 150° and sliding angles below 20° compare well to those achieved on the lab scale. Coated samples with dimensions on the order of meters such as fabric or window glass are presented.

Regenerating sodium hydroxide from the spent caustic by bipolar membrane electrodialysis (BMED)

An experimental study was carried out on regeneration sodium hydroxide (NaOH) from the spent caustic by bipolar membrane electrodialysis (BMED). The effects of operation parameters, such as concentration of electrolyte, current density and initial base concentration, on regeneration were investigated. The results indicate that low energy consumption and high current efficiency can be achieved with the concentration of electrolyte in the range of 0.20–0.30mol/L, initial concentration of the base in range of 0.10–0.25mol/L and current density in the range of 30–60mA/cm2. The process cost is estimated to be USD 0.97 for regenerating 1kg NaOH with the laboratory-scale equipment, showing economically competitive.

A novel precursor route for the production of Si―B―N ceramic fibers

A novel polymeric precursor to SiBN ceramic fiber was synthesized by reaction of tetramethylaminosilane ((CH 3NH) 4Si) and trimethylaminoborane ((CH 3NH) 3B). It was shown that the polymer contains an Si―N―B bridge bond connecting the linear silicon and borazon ring parts. This structure imparts sufficient viscosity for the material to be processed by melt spinning, so that for the first time it was easily spun into green fibers using laboratory scale equipment. SiBN ceramic fibers with diameter 35 μm were obtained after pyrolysis at 1600 °C in an NH 3 atmosphere. The thermal decomposition behavior of the polymer during pyrolysis was also investigated.

Simple guidelines for a self-built laboratory-scale supercritical anti-solvent system

A technique to generate supercritical fluid (SCF) particles has gained attention in pharmaceutical, cosmetic and paint applications. However, the scarcity of information on the design of this type of laboratory-scale equipment is a significant obstacle to its technological progress. Therefore, the purpose of this study was to design and develop a laboratory supercritical anti-solvent (SAS) system for producing microparticles and microcapsules of acetaminophen. The designed SAS system was operated at 110 bars of pressure, 35 °C, 35 mg/ml polymer concentration and 1.75 ml/min feed flow rate. The morphological, thermal and crystallographic properties of the microparticles and microcapsules were characterised using scanning electron microscopy, thermogravimetric analysis and X-ray powder diffraction, respectively. The in vitro drug release by the microparticles and microcapsules was also investigated. Following the SAS process, a more homogenous microparticle size distribution was observed in addition to a change in the crystallinity, and the drug thermal stability was maintained. Furthermore, the microcapsules significantly prolonged the drug release during the in vitro study. These results demonstrate that the designed SAS system successfully produced microparticles and microcapsules of the selected drug.

Realization of Power Modules by Chip Embedding Technology

The continuous miniaturization of silicon dies and the need for a further package size reduction, with an equal or better performance and reduced manufacturing cost, are the main drivers for new packaging concepts. The embedding of active and passive components offers a wide range of benefits and potentials. With the use of laminate based technology concepts, components can be moved from surface mount into the build-up layers of substrates by embedding and by that, the third dimension will be available for further layers or assemblies. This paper will briefly discuss the necessary process steps of the embedded chip technology, which is based on printed circuit board manufacturing processes, and will also demonstrate the transfer of the technology from a smaller size lab scale equipment environment to an industrial comparable process line, capable of processing large panel formats up to 18” x 24”. The paper will also briefly describe this development and categorize today's embedding technologies. First modules with embedded chips are in production in Asia, mainly for telecom and computer applications. In Europe embedding has gained a strong interest for power modules, especially in automotive applications. Main drivers are the capability for compact and thin packaging, the high reliability and cost saving potential. In a number of European cooperation projects with partners from industry and research, embedding of power chips, like IGBTS and power MOSFET, is of high interest. In this paper current achievements of these projects will be shown, especially examples of realized devices and their characteristics. The dominating technology for power chip embedding is a face-up technology. Chips are bonded with their backside (drain contact) to a Cu substrate using highly conductive adhesive or solder. Using the face up assembly, a direct contact to the backside of the die is possible, allowing a lot of benefits for driving high currents and applying an efficient thermal management for the power devices. Then Chips are embedded by vacuum lamination of prepreg or RCC (resin coated copper) layers. Via holes to the top contacts (gate and source) are formed by laser drilling. The vias are metallized using conventional Cu plating. Finally conductor structures are etched in the top Cu layer, finalizing the circuit. Details will be given about device manufacturing, related yield issues and strategies to overcome them. Finally scenarios for the implementation of embedding technology and concepts for future applications will be discussed.