Process development

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.

Trials and pilot plants

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.

Rotating bed reactors

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.

Application 1008
Activated carbon decolorization, fast and without filtration

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.  

Application 1012
Flexible deployment with the Plug-in rotating bed reactor

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.

Application 1007
Automatic processes for efficient production

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.

Application L1704
Biocatalysis engineering: the big picture

Roger A. Sheldon and Pedro C. Pereira Chem. Soc. Rev., 2017, 46(10), pp. 2678-2691.

Application L1604
Catalytic hydrogenation of d-xylose over Ru decorated carbon foam catalyst in a SpinChem® rotating bed reactor

Tung Ngoc Pham, Ajaikumar Samikannu, Anne-Riikka Rautio, Koppany L. Juhasz, Zoltan Konya, Johan Wärnå, Krisztian Kordas, and Jyri-Pekka Mikkola Top. Catal., 2016, 59, pp. 1165-1177.

Application 1035
Column vs RBR

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  

Application 1024
Decolourization more efficient in rotating bed reactor than fixed bed reactor

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.

Application 1004
High-viscosity applications made faster

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.

Application 1030
Viscous solutions decolourized using a rotating bed reactor and a stirred tank reactor

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.

Application 1034
Decolourization using 79 L of activated carbon in a 7000 L vessel

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

Application L1601
Deconstruction of Nordic hardwood in switchable ionic liquids and acylation of the dissolved cellulose

Valerie Eta and Jyri-Pekka Mikkola Carbohydr. Polym., 2016, 136, pp. 459-465.

Application 1033
Deionizing 7000 L of tap water using the SpinChem® RBR S100

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  

Application L2204
Design of a green chemoenzymatic cascade for scalable synthesis of bio-based styrene alternatives

Philipp Petermeier, Jan Philipp Bittner, Simon Müller, Emil Byström, Selin Kara Green Chemistry, 2022, 24(18), pp. 6889-6899.

Merry Christmas
Effective extraction of spices for mulled wine production using a rotating bed reactor

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

Application 1003
Improving reactions in emulsions using a rotating bed reactor

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.

Application L1301
Efficient biocatalysis with immobilized enzymes or encapsulated whole cell microorganism by using the SpinChem reactor system

Hendrik Mallin, Jan Muschiol, Emil Byström, and Uwe T. Bornscheuer ChemCatChem, 2013, 5, pp. 3529-3532.

Application 1002
Efficient synthesis of chiral lactones by encapsulated cells in a rotating bed reactor

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.

Application L1802
Epoxidation of fatty acids and vegetable oils assisted by microwaves catalyzed by a cation exchange resin

Adriana Freites Aguilera, Pasi Tolvanen, Shuyana Heredia, Marta González Muñoz, Tina Samson, Adrien Oger, Antoine Verove, Kari Eränen, Sebastien Leveneur, Jyri-Pekka Mikkola, and Tapio Salmi Ind. Eng. Chem. Res., 2018, 57(11), pp. 3876-3886.

Application L1605
Fibre stress-strain response of high-temperature chemi-thermomechanical pulp treated with switchable ionic liquids

Ran Duan, Bo S. Westerlind, Magnus Norgren, Ikenna Anugwom, Pasi Virtanen, and Jyri-Pekka Mikkola BioRes., 2016, 11(4), pp. 8570-8588.

Application 1042
How large liquid volumes can a rotating bed reactor process?

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.

Application L1603
In quest for the optimal delignification of lignocellulosic biomass using hydrated, SO2 switched DBU MEASIL switchable ionic liquid

Ikenna Anugwoma, Luis Rujana, Johan Wärnå, Mattias Hedenström, and Jyri-Pekka Mikkola Chem. Eng. J., 2016, 297, pp. 256-264.

Application 1016
In situ filling and emptying of rotating bed reactors

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

Application 1037
In-tank deployment of large scale rotating bed reactor

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  

Application L1903
L-Asparaginase production in rotating bed reactor from Rhizopus microsporus IBBL-2 using immobilized Ca-alginate beads

Anup Ashok and Santhosh Kumar Devarai 3 Biotech, 2019, 9(9), 349.

Application L1402
Lipase catalyzed regioselective lactamization as a key step in the synthesis of N-Boc (2R)-1,4-oxazepane-2-carboxylic acid

Carl-Johan Aurell, Staffan Karlsson, Fritiof Pontén, and Søren M. Andersen Org. Process Res. Dev., 2014, 18(9), pp. 1116-1119.

Brochure
Mass transfer revolutionized

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

Application L2117
Multi‐enzyme cascade reaction in a miniplant two‐phase‐system: Model validation and mathematical optimization

Jens Johannsen, Francesca Meyer, Claudia Engelmann, Andreas Liese, Georg Fieg, Paul Bubenheim, and Thomas Waluga AIChE J., 2021, 67(4), e17158.

Application 1001
How to find the optimal rotational speed when using a rotating bed reactor

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.

Application L2110
Process design of a continuous biotransformation with in situ product removal by cloud point extraction

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.

Application L1703
Reaction engineering of biocatalytic (S)-naproxen synthesis integrating in-line process monitoring by Raman spectroscopy

M. Aßmann, A. Stöbener, C. Mügge, S. K. Gaßmeyer, L. Hilterhaus, R. Kourist, A. Liese, and S. Kara React. Chem. Eng., 2017, 2(4), pp. 531-540.

Application 9001
Recycling of Immobilized Enzymes – Simple and Streamlined Biocatalysis

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

Application 1039
Remediation of wastewater stored in High Integrity Container

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.

Application 1032
Rotating bed reactor for immobilized enzymatic reactions

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

Application 1025
Soft alginate beads used in a rotating bed reactor

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.

Application 1010
Rotating bed reactors completely avoid grinding of molecular sieves

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.

Application 1036
Screening of activated carbon using the SpinChem® RBR S2

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

Application 1044
Simple scale-up using flexible reactors

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.

Application 1009
Multistep synthesis or simultaneous extraction simplified in a rotating bed reactor

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.

Application 9003
Simultaneous Selective Decolouration – Illustrating a Concept for Cascade Reactions

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

Transfer hydrogenation with catalyst recycling in a rotating bed reactor

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.

Treatment of 7.5 m3 with a 50L Plug-in system

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.

Application 9004
Treatment of Viscous Solutions – Simple Extraction and In-line Monitoring

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

Application 1043
Using a rotating bed reactor in different liquid volumes

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.

Application 1050
Lipase-catalyzed hydrolysis in 750 L using a rotating bed reactor

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.

Application 1054
Palladium catalyst recovery using scavenger resin

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.

Application 1051
How the loading of solids influences reaction speed

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?

Application 1053
Phenol scavenging using ion-exchange resin

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.

Application L2212
Epoxidation of Tall Oil Fatty Acids and Tall Oil Fatty Acids Methyl Esters Using the SpinChem Rotating Bed Reactor

Krzysztof Polaczek, Eliza Kaulina, Ralfs Pomilovskis, Anda Fridrihsone, Mikelis Kirpluks Journal of Polymers and the Environment, Volume 30 (2022), pages 4774–4786

Application L2302
Fatty Acid Epoxidation on Enzymes: Experimental Study and Modeling of Batch and Semibatch Operation

Wilhelm Wikström, Adriana Freites Aguilera, Pasi Tolvanen, Robert Lassfolk, Ananias Medina, Kari Eränen, and Tapio Salmi Ind. Eng. Chem. Res., 2023, 62(23), pp. 9169-9187.

Application L2120
Rotating bed reactor packed with heterofunctional structured silica-supported lipase. Developing an effective system for the organic solvent and aqueous phase reactions

Daria Kowalczykiewicz, Katarzyna Szymańska, Danuta Gillner, and Andrzej B. Jarzębsk Microporous Mesoporous Mater., 2021, 312, 110789.

Application 2116
Prilezhaev epoxidation of oleic acid in the presence and absence of ultrasound irradiation

Adriana Freites Aguilera, Roosa Hämäläinen, Kari Eränen, Pasi Tolvanen, and Tapio Salmi J. Chem. Technol. Biotechnol., 2021, 96(7), pp. 1874-1881.

Application L2002
Determination of kinetics and equilibria of heterogeneously catalyzed gas-phase reactions in gradientless autoclave reactors by using the total pressure method: Methanol synthesis

Tapio Salmi, Kari Eränen, Pasi Tolvanen, J.-P. Mikkola, and Vincenzo Russo Chem. Eng. Sci., 2020, 215, 115393.

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