Increasing the production efficiency, and reducing the material costs are generally the main goals, both when planning for the improvement of an already existing process, and when developing a brand new one. Process development involves the planning, testing, supervising and optimizing of the procedures, techniques and workflows of a certain process.
There are generally a few different steps in developing a new process. First off, laboratory trials are planned, tested and optimized to ensure satisfactory reaction conditions and product yields. This often includes testing of different materials, solvents, and reaction settings, to reach suitable results. The process is later moved over to a pilot plant for pre-commercial production runs, and further large-scale process optimization. This will offer a chance to study the set-up in a situation resembling the final process. In this step, parameters can be adjusted to ensure a maintained quality of the process at a larger scale. During these two initial phases it is also common to test out partially or complete automation of the process, as well as the incorporation of new tools and technological solutions. After the process has been tested and optimized for satisfactory results, it is ready to be moved on to production.
SpinChem offers help with the development of your heterogeneous processes, from bench-top screening, to full-scale production. Due to the generic design of the SpinChem® rotating bed reactor (RBR), the technology is fully scalable, and performs just as well in liquid phase volumes of a few millilitres (MagRBR), as in several thousand cubic metres of solution (ProRBR). If the existing set-up makes it impractical to use the RBR in-tank for batch processing, SpinChem offers other solutions, such as flow systems, where the RBR is used in a separate vessel connected to the main tank. The SpinChem® RBR can also be used in connected systems of reactor vessels, where the RBR is used in one or more of these vessels.
The efficient mass transfer achieved with the RBR, along with the fact that the solid phase is not exposed to mechanical forces or pressure, makes for quick and clean reactions. Downstream processing is cut to a minimum as there is no need for filtering of solid phase resin or debris from the reaction solution. This makes the SpinChem® RBR a very cost and resource efficient alternative both in research and production.
SpinChem’s fields of expertise include chemistry, engineering, experimental design, solid phase materials, and fluid flow simulations. Through rapid in-house prototyping, testing, simulating, analysis and optimization, SpinChem is able to develop clever, custom-made solutions to fit your processes and applications.
Activated carbon is a common choice for removing impurities or capturing compounds from a product batch. However, the carbon may itself foul the product and be difficult to separate. The rotating bed reactor offers a clean way to deploy activated carbon that removes the need for time-consuming filtration and extends the lifetime of the solid phase.
The rotating bed reactor (RBR) is a combined tool for chemical transformations and liquid transfer operations, reducing or eliminating the need for external pumps. Filled with a catalyst or adsorbent, and rotated by a motor, the RBR brings the liquid to be processed in contact with the solid-phase at high flow rates. Due to the high flow rate generated, the RBR can not only treat the liquid in the reaction vessel, but also transfer it into the vessel for processing.
Automation of large-scale processes is often a requirement for economically viable chemical processes. The benefits of scale are best harvested at high throughputs and 24/7 operation. This leads to the demand for process automation, and the elimination of hands-on work.
Tung Ngoc Pham, Ajaikumar Samikannu, Anne-Riikka Rautio, Koppany L. Juhasz, Zoltan Konya, Johan Wärnå, Krisztian Kordas, Jyri-Pekka MikkolaTopics in Catalysis, 59 (2016) 1165-1177
A performance comparison between a column (fixed bed reactor) and rotating bed reactor (RBR) for de-ionizing 1000 L of tap water. Using best-in-class standard protocols for both technologies, we tested which technology could de-ionize to a desired endpoint conductivity value the quickest. The result show that the RBR is significantly faster, reaching 3.7 times faster a conductivity level of 0.15 µS/cm compared to the column. Keywords: Cleantech, Deionization, Fast reaction, Technology
A fixed bed reactor (FBR), also known as a packed bed reactor or column, is a traditional technology for processes such as adsorption or heterogeneous catalysis. Achieving the required level of purification or conversion means running the liquid through the reactor at a sufficiently low flow rate, and the throughput of a fixed bed reactor is therefore often limited.
Liquids with high viscosity create problems for heterogeneous applications in traditional reactors. Packed bed reactors (columns) suffer from huge back pressures, and stirred tank reactors (STR) exhibit reduced reaction rates due to poor mixing. Both issues lead to longer processing times and expensive operations.
Decolorization, pesticide remediation, catalysis, and many other applications involve dealing with viscous liquid that needs to be modified in some way. The rotating bed reactor presents an efficient way to treat viscous liquids, without the challenges of conventional reactors.
A large scale decolourization experiment using the SpinChem® rotating bed reactor (RBR) S100, packed with 79 L of activated carbon. The vessel contained 7000 L of water with added methylene blue dye. In under 40 minutes, 95% of the initial concentration of methylene blue was removed from the water, which shows that the RBR S100 can achieve fast reaction times in large scale processes. Keywords: Activated carbon, Cleantech, Decolouration, Fast reaction
Valerie Eta, Jyri-Pekka MikkolaCarbohydrate Polymers, 136 (2016) 459-465
The SpinChem® rotating bed reactor (RBR) S100, with a solid phase capacity of 100 L, was used to deionize 7000 L of tap water. The RBR S100 was operating at 160 rpm and filled with 36.5 L of mixed bed ion exchange resin. The results show that the RBR S100 can efficiently process large liquid volumes. As shown by the successful deionization, the performance of the RBR remains high even when it is partially filled, which proves the extreme robustness of the RBR technology. Keywords: Ion exchange, Seamless scaleup, Technology
In line with the call for sustainable production, researchers are focusing their efforts on the utilization of renewable resources and the development of environmentally friendly manufacturing methods. Bio-based polymers are emblematic and has potential in terms of polymerization and material characteristics. Many products are using hydroxystyrene monomer these days. Hydroxystyrenes are particularly appealing as a replacement or addition to styrene-based polymer chemistry since they are renewable lignin building blocks. These monomers are made by decarboxylating phenolic acids, and their phenolic hydroxy groups are frequently subjected to chemical changes to enhance polymerization behavior. A straightforward, scalable, and entirely (chemo)catalytic synthesis of acetylated hydroxystyrene is still difficult to come by. With functionalized polystyrene's range and potential, the question arises of how scalable and sustainable the respective monomers are that can be synthesized? Contributing to answering the above question we will discuss a recent research project INTERfaces that developed a green, one-pot, two-step approach to producing acetylated hydroxystyrenes from raw lignin. In this case, the acylated hydroxystyrenes were designed as environmentally friendly monomers for making certain polystyrenes. Also, authors suggestions on a novel chemoenzymatic pathway that uses phenolic acid decarboxylase (PAD) would be discussed. A novel chemoenzymatic pathway Authors suggest a novel chemoenzymatic pathway that makes use of a phenolic acid decarboxylase (PAD). Authors have hypothesized that limitations could be circumvented by a tailored combination of a more active decarboxylation catalyst, milder reaction conditions and a compatible reaction medium. As a renewable, non-toxic, and highly active catalyst, phenolic acid decarboxylase from Bacillus subtilis (BsPAD) was the biocatalyst of our choice to embark on this process development. Herein, we describe our systematic efforts to design an alternative, scalable, chemo-enzymatic route to access bio-based styrene alternatives in an environmentally friendly and efficient manner. An approach to process development entails a computational solvent assessment that provides information on solubilities and feasible reactor operation modes, experimental solvent screening, cascade engineering, heterogenization of biocatalyst, customization of acetylation conditions, and reaction upscale in a rotating bed reactor. Procedure Decarboxylation of phenolic acids, which can be generated from lignin, to the equivalent hydroxystyrene is the initial step. As a green decarboxylation catalyst, phenolic acid decarboxylase from Bacillus subtilis (bsPAD) was used. A significant amount of computational and experimental work was put into finding a solvent and water saturation that allowed for high enzyme catalytic activity in the non-conventional media while also offering good solubility of the phenolic acid reactant and hydroxystyrene product. MTBE and CPME that were water-saturated had all required characteristics. The more eco-friendly option was CPME because of higher boiling point, which was beneficial in the second step. The hydroxystyrene intermediate was directly acylated without switching solvents in the second stage of the one-pot, two-step synthesis. The effectiveness of the acylation of the phenol in a wet solvent was confirmed. The ideal parameters for an experiment were found to be low catalyst concentrations (0.03 eq NaOAc), moderate anhydride concentrations (2.0 eq Ac2O), and relatively high temperatures (90°C). The enzyme bsPAD was immobilized to allow for reuse and to stop it from obstructing the second step and work-up. Immobilization on Purolite ECR8415F as a carrier material was the outcome of extensive evaluation of enzyme carrier materials and chemistries for high immobilization yield, enzymatic activity, and longevity. Using the RBR The reaction was scaled up to 1 L to prove its feasibility. SpinChem RBR S3 was used to charge the immobilized bsPAD-8415F enzyme for the reaction. The application of RBR, resulted in a developed clean, one-pot, two-step procedure that makes use of bio-based phenolic acid educts, reusable immobilized PAD, and the renewable solvent CPME. On a 1 L scale, the entire chemoenzymatic reaction casscadded to produce 18.3 g of 4-acetoxy-3-methoxystyrene with a 96% isolated yield. As a result of the rotating bed reactor, the carrier beads were protected and the enzyme could be simply removed between steps one and two, thus preventing the enzyme from interfering with the second step and to be reused in the decarboxylation step. The RBR made the process fast and simple, provided efficient sampling and monitoring of the process and kept the immobilized catalyst safely confined. Interested in the rotating bed reactor? Get in touch with us to understand how the rotating bed reactor technology can simplify or improve your process.
Video showing how to promote holiday spirit by seasoning mulled wine using a rotating bed reactor. Assorted spices and sugar were used to transform white wine mixed with a clear liquor into a festive and flavourful Christmas drink. The temperature of the mixture was kept at 70°C and the outside temperature at -6°C, using a heating jacket and a northern latitude, respectively. Keywords: Behind the scenes
When working with an emulsion (and particularly with a heterogeneous catalyst) the mass transfer between the phases is critical. Insufficient mixing leads to lower interfacial area per volume, and in turn to poor mass transfer across the phases.
Hendrik Mallin, Jan Muschiol, Dr. Emil Byström, Prof. Dr. Uwe T. BornscheuerChemCatChem, 5 (2013) 3529-3532 "...the immobilized transaminase was better protected from mechanical forces in the SpinChem device." Keywords: Alginate, Biotransformation, Encapsulated cells, Immobilized enzymes, Organic molecules, Scientific literature
Whole cell biocatalysis is powerful, but not straightforward. One way of utilizing whole cells is to encapsulate them in a matrix such as alginate to make them easier to separate from a reaction mixture. However, alginate beads are not mechanically stable enough to be packed into columns and are easily destroyed in stirred tank reactors (STR). This makes enzyme recycling ineffective, at the same time as mass transfer limitations may prevail.
Epoxidation reactions with in-situ formed percarboxylic acids were enhanced by heterogeneous catalysis and optimized with respect to product yield. The authors concluded that “SpinChem RBR, was beneficial, in terms of eliminating mass transfer limitations, it enabled a simpler collection and recycling of the catalyst and minimized mechanical wear of the solid catalyst”. Keywords: Easy handling, Ion exchange, Organic molecules, Scientific literature, Synthesis
Large volumes of liquid waste will often accumulate at industrial sites. It may be very time-consuming and resource-intensive to adequately treat these waste streams for release, so the problem often compounds over time.
Video showing how a SpinChem® rotating bed reactor (RBR) was charged with solid particles, followed by draining and replacing the reaction liquid without escape of solids. Lastly, the solid phase was removed without opening the RBR. This procedure illustrates a concept for automatic handling of solid phases in production scale equipment without opening the reaction vessel. Keywords: Easy handling, Seamless scaleup, Technology
To further demonstrate the use of RBR:s at process scale, a decolorization using ion exchange resin was performed at 7500 L scale. An RBR S14 was filled with strongly acidic cationic resin NRW1160 from Purolite and used to remove blue dye from an aqueous solution in a stainless steel tank of 7500 L volume. The solid-to-liquid ratio is a fraction of percent, showing the efficiency of the RBR technique for convectional mass-transfer and global mixing. The RBR was spun at 340 rpm while the transmittance at 663 nm was monitored for ca 4 h at which point the transmittance had recovered the baseline value for colorless de-ionized water. Keywords: Ion exchange, Cleantech, Nuclear, Scale-up
The present work reports on the production of extracellular l-asparaginase from Rhizopus microsporus IBBL-2 using submerged fermentation (SmF) process free of glutaminase and urease activities. Scale-up studies involving 200-mL and 1-L rotating bed reactor (RBR) using immobilized beads were done and the results obtained are 20.21 U mL-1 and 19.13 U mL-1, respectively, the increased activity with immobilization accounts for reduced shear on cells due to increased stability as compared to the free-flowing cells.
Learn how SpinChem rotating bed reactors (RBR) can eliminate poor mass transfer in heterogeneous reactions during chemical synthesis and biotransformations. Preserve activity and facilitate recycling of solid phases with the RBR. This brochure shows technology and applications. Keywords: Biotransformation, Brochure, Fast reaction, Immobilized enzymes, Molecular sieve, Preserved activity, Simple cleanup, Synthesis, Technology
In the American Institute of Chemical Engineers, AIChE Journal, the authors of this paper highlights the use of Rotating Bed Reactor (RBR) with two different immobilized enzymes at the same time in a cascade reaction. In the flow chart above of the miniplant consisting of a continuously stirred tank reactor (CSTR) equipped with an RBR (highlighted in orange) (a), a buffer tank (b), an extractive centrifuge (c) and a fixed bed reactor (d) In the reaction scheme the complete multi-enzyme cascade is shown with the two enzymes placed in the RBR is highlighted. If you would like to get in contact with us give us a call or fill in the form.
Many heterogeneous processes are limited by mass transfer at typical laboratory or industrial conditions. When using a rotating bed reactor, the mass transfer is most easily controlled using the rotational speed.
In biotransformations, obstacles commonly encountered are product inhibition, product toxicity, and reaction equilibria that prevents complete conversion. Enzyme engineering has made tremendous progress in alleviating these problems. The concept of in situ product removal (ISPR) may still be an attractive alternative or complement. The authors have demonstrated concurrent enzymatic reaction and ISPR, referred to as 'extractive biocatalysis'. For the ISPR, the authors evaluated the use of aqueous micellar two-phase systems (ATPMS) as an extraction medium. For the model reaction, Penicillin G hydrolysis by CalB lipase, the demonstrated process was thus a continuous, heterogeneous extractive biocatalysis with cloud point extraction. An RBR was used during the process development work to determine the Michaelis-Menten kinetics of the CalB immobilized in gel coatings on column packing material. Also, the particles were easily re-used in stability experiments.
A traditional stirred tank reactor setup was compared to a rotating bed reactor (RBR) for the biocatalytic synthesis of the anti-inflammatory drug (S)-naproxen. Both setups performed well during five repetitive bathes giving an enantiomeric excess of 99% and an isolated yield of 92%, but the RBR was easier to handle and the authors concluded that “… the rotating bed reactor concept can be regarded as a promising option for industrial applications”. Keywords: Biotransformation, Immobilized enzymes, Organic molecules, Scientific literature
Immobilized catalyst recycling using a SpinChem® rotating bed reactor (RBR) and a Mettler-Toledo EasyMax™ 102 Advanced synthesis workstation. The process proved very time efficient as no filtration steps were needed between cycles, or for the samples extracted for analysis during each run. Washing of the resin between runs was fast, simple and robust, without running the risk of material loss. Keywords: Biotransformation, Immobilized enzymes, Mettler-Toledo, Organic molecules, Preserved activity, Quick recycling
The versatility of the ProRBR IBC add-on (picture below) was demonstrated by mounting it on a high-integrity container (HIC) (picture above) and running a sample reaction. The ProRBR IBC add-on can be placed on most reasonably stable supports. In this case, the RBR add-on was placed over the HIC opening by support of a common construction scaffold. A common ion-exchange reaction, de-ionization by 7 L of mixed-bed resin to 3000 L of municipal water, was carried out to measure the performance. The ion concentration/ conductivity was halved after ca 30 min and after 2 h it was down to our LOQ.
Poster on a case study of applying the rotating bed reactor for the lipase-mediated stereoselective acetylation of a racemate amine as a model reaction for the manufacturing of pharmaceutical building blocks. The results showed that enzyme recycling and synthesis scale up was easy to achieve with preserved yield, enantioselectivity and catalytic activity. Keywords: Biotransformation, Easy handling, Immobilized enzymes, Quick recycling, Seamless scaleup
Stirred vessels tend to damage soft heterogeneous catalysts, like enzymes immobilized in agarose or alginate beads, with activity loss and tedious workup as consequence. In a fixed bed reactor, these materials are easily compressed by the pressure gradient, leading to a loss of flow rate. Overcoming these challenges opens up the possibility to use biocatalysis as a tool for greener processes and more sustainable manufacturing.
When using of solid-phase catalysts or adsorbents in reactors, the physical degradation of the materials is a common problem. The traditional stirred tank reactor inflicts mechanical damage to the particles, which causes attrition, fines that are difficult to separate, and loss of the functionality of the solid-phase.
In co-operation with ZHAW, two students screened various types and sizes of activated carbon using the SpinChem® RBR S2. Five different carbons were screened by decolorizing solutions of methylene blue in distilled water. The decolorization process was monitored using inline UV-Vis spectrometry (PAT). The results show the importance of choosing the correct media for your application. In this case of activated carbon, the source and type of the activation was shown to have a major impact on performance. Keywords: Activated carbon, Decolouration, Fast reaction, Rapid screening, Technology
Research and development quickly takes new directions, and the requirements on a laboratory may vary with every new project. Limiting yourself to equipment with a narrow scope of conditions and applications may become expensive, since new equipment must be acquired for anything out of scope. With budgets quickly consumed by other projects, the need for new equipment may mean significant delays and a reduced capability to take on emerging opportunities. Many heterogeneous processes (e.g. adsorption or catalysis) are made faster by increasing the solid-to-liquid ratio. Studying scale-up effects can also help to predict full-scale performance. For these reasons it’s wise to invest in equipment that can handle different operating conditions such as liquid volume, solids loading, pH and temperature. The RBR S3 Plus is the most modular rotating bed reactor for laboratory use. Made from two stacked rotating bed reactors, the S3 Plus quickly converts to a single RBR S3 for use with smaller liquid volumes. When used in the dedicated glass reactor system, this yields an operating range of 250 - 1500 mL of liquid and 0 - 140 mL of solids. This application note investigates the effect of solids loading on the reaction rate of two applications: the adsorption of a dye and a biocatalytic esterification reaction. These two reactions are mass-transport limited and relatively fast. In the first case, an RBR S3 and an RBR S3 Plus were filled with 50 mL and 100 mL respectively of the ion-exchange resin Purolite® NRW1160. Methylene blue was dissolved in water, and the solution was decolorized by spinning an RBR at 600 RPM (reaction conditions in the details below). The results were clear; each case followed 1st order kinetics with a rate constant for the RBR S3 Plus that was twice that of the RBR S3. Note that the solid-to-liquid ratio for the RBR S3 Plus was also twice that of the RBR S3. For the enzymatic esterification, the same rotating bed reactors (RBR S3 and RBR S3 Plus) were filled with 40 mL and 80 mL respectively of the biocatalyst Purolite® immo PS. The rotating bed reactors were used in separate reactions in mixtures of lauric acid, 1-propanol and water. Also in this case the reaction rate was proportional to the solid-to-liquid ratio, yielding twice the productivity with the RBR S3 Plus compared to the RBR S3. The conclusion is that with a rotating bed reactor you are making the most out of the solid-phase. Doubling the amount of catalyst or adsorbent will generally double the reaction rate constant, which makes scaling up straightforward. Contact us today to discuss how we can scale your process.
The synthesis of products, such as active pharmaceutical ingredients, often involve multiple steps using heterogeneous catalysts or adsorbents. The need often arises for simultaneous use of multiple solid phases.
Two dyes were selectively extracted onto different adsorbents within the same run using a SpinChem® rotating bed reactor (RBR) and an EasyMax™ 102 Advanced synthesis workstation. This experiment illustrates performing cascade reaction for one-pot multi-step synthesis. Keywords: Cleantech, Decolouration, Extraction, Ion exchange, One-pot multistep, Organic molecules, Polymeric resin, Technology
Hydrogenation reactions using hydrogen gas are usually efficient and clean. Drawbacks are the safety issues of handling hydrogen gas, need for reactors made for pressurized reactions, and the necessity of vigorous stirring to make these solid-liquid-gaseous reactions work well.
A small rotating bed reactor (RBR) system deployed in an external loop to the customer’s regular reaction vessel. Even though RBR technique has been identified as offering advantages for a particular process, deploying it in existing an existing reaction vessel may prove difficult for practical reasons. This is were “plug-in” mode deployment of the RBR can offer a solution. The RBR and associated vessel is attached in an external loop by inlet and outlet connections to the regular vessel. The “plug-in” RBR system is typically small compared to the regular vessel. Alternatively, the RBR system can be deployed in a vessel → RBR → 2nd vessel mode. A proof-of-concept demonstration of an RBR in “plug-in” mode by a decolorization. The volume of the “plug-in” vessel is ca 0.7% of the regular vessel it is attached to.
Blue dye was removed from a highly viscous liquid using a SpinChem® RBR S2 in an EasyMax™ 102 Advanced Synthesis Workstation. Monitoring of the reaction was easily recorded as no freely suspended ion exchange resin beads or resin debris interfered with the readings. This demonstrates that the RBR technology is extremely well suited for in-line monitoring. The viscosity of the solution was determined to ca 230 cP at 25°C, showing that it is possible to absorb dye even from a highly viscous solution. Keywords: Decolouration, Extraction, Ion exchange, Mettler-Toledo, Viscous solutions
Research and development quickly takes new directions, and the requirements on a laboratory may vary with every new project. Limiting yourself to equipment with a narrow scope of conditions and applications may become expensive, since new equipment must be acquired for anything out of scope. With budgets quickly consumed by other projects, the need for new equipment may mean significant delays and a reduced capability to take on emerging opportunities.
Biocatalysis offers many benefits in the production of chemicals and active pharmaceutical ingredients. One major challenge has been the deployment of immobilized enzymes in an efficient way on large scale. The rotating bed reactor offers a convenient way to scale a biocatalytic process.
Catalyst recovery is an important step in downstream processing. Using an appropriate scavenger resin and a rotating bed reactor to deploy it, the recovery is straightforward and effective.
Sometimes you don’t want to pack the entire rotating bed reactor full with your solid-phase material. Fully loading might simply be wasteful, or you may want to experiment with your reaction conditions. But how does the amount of solids in the rotating bed reactor influence the reaction performance? Can you use only 10% of the full capacity?
Scavenging of soluble undesirable compounds and substances onto solid phase is used in a wide range of applications. In this example, a rotating bed reactor (RBR) is used to capture low concentrations of a phenol onto readily available Strong Anion Exchange (SAX) resin as a scavenger.
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