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.
Roger A. Sheldon and Pedro C. Pereira Chem. Soc. Rev., 2017, 46(10), pp. 2678-2691.
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.
Removing ions from liquids is common in industry and society. Ions are remediated in applications ranging from the production of pharmaceuticals to the treatment of communal waste streams. Likewise, the nuclear energy sector deals with the removal of ionic radioactive substances from water on a daily basis.
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.
Valerie Eta and Jyri-Pekka Mikkola Carbohydr. Polym., 2016, 136, pp. 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.
Philipp Petermeier, Jan Philipp Bittner, Simon Müller, Emil Byström, and Selin Kara Green Chemistry, 2022, 24(18), pp. 6889-6899.
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, Emil Byström, and Uwe T. Bornscheuer ChemCatChem, 2013, 5, pp. 3529-3532.
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.
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.
Ran Duan, Bo S. Westerlind, Magnus Norgren, Ikenna Anugwom, Pasi Virtanen, and Jyri-Pekka Mikkola BioRes., 2016, 11(4), pp. 8570-8588.
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.
Ikenna Anugwoma, Luis Rujana, Johan Wärnå, Mattias Hedenström, and Jyri-Pekka Mikkola Chem. Eng. J., 2016, 297, pp. 256-264.
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.
How can this process be scaled up? This is perhaps the most important question to consider when developing a chemical process. If it cannot be done on large scale, all the time and resources invested in laboratory work will be unrewarded. Pumping liquids through massive columns or separating solids from a large batch can be unsurmountable challenges that bring a halt to a new project before it has even left the starting blocks.
Anup Ashok and Santhosh Kumar Devarai 3 Biotech, 2019, 9(9), 349.
Carl-Johan Aurell, Staffan Karlsson, Fritiof Pontén, and Søren M. Andersen Org. Process Res. Dev., 2014, 18(9), pp. 1116-1119.
The SpinChem rotating bed reactor (RBR) can eliminate poor mass transfer in heterogeneous reactions during chemical syntheses and biotransformations, preserve catalyst activity, and facilitate recycling of solid phases. This brochure presents our technology and its applications.
Jens Johannsen, Francesca Meyer, Claudia Engelmann, Andreas Liese, Georg Fieg, Paul Bubenheim, and Thomas Waluga AIChE J., 2021, 67(4), e17158.
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.
Oliver Fellechner and Irina Smirnova Can. J. Chem. Eng., 2021, 99, pp. 1035-1049.
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.
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 of 3000 L municipial water by 7 L of mixed-bed resin, was carried out to assess performance. The conductivity was halved after only about 30 min and after 2 h it reached the LOQ.
This case study presents a lipase-mediated stereoselective acetylation of a racemic amine 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.
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.
Contaminations in liquids can often be removed using an adsorbent, such as granular activated carbon (GAC). The best choice of adsorbent is unique for each contaminant, and the effectiveness depends on many parameters. Failing to investigate these can lead to unnecessarily high material costs and long processing times.
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.
The synthesis of products, such as active pharmaceutical ingredients (APIs), often involves multiple steps using heterogeneous catalysts or adsorbents. Thus, the simultaneous use of multiple solid phases either during synthesis or downstream processing is frequently highly advantageous.
Synthesis typically involves multiple reaction steps and the isolation of intermediate products. Any incomplete conversion at the end of each step will compound to an overall lower yield. To make things worse, the work-up of each intermediate can be very time-consuming. This has made one-pot cascade synthesis (the simultaneous execution of multiple steps in a single reactor) a desirable target for chemists. This approach aims to minimize intermediate work-up, reduce the risk of material loss, and enhance overall process efficiency.
Josefina Nyström, Ulla-Britt Östman, Torgny Mossing, Leif Hed, and Paul Geladi Food Anal. Methods, 2020, 13, pp. 933-941.
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 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.
Heterogeneous reactions involving viscous solutions put high demands on equipment and materials. Columns face high pressure drops and require powerful pumps and durable solid phase particles. Stirred tank reactors do not face the same problem, but the high liquid viscosity and low particle density will have a negative impact on reaction kinetics and require tedious filtration to separate the solids afterwards.
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 in the long run. The need for new equipment may inflict delays and affect your 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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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.
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Adriana Freites Aguilera, Roosa Hämäläinen, Kari Eränen, Pasi Tolvanen, and Tapio Salmi J. Chem. Technol. Biotechnol., 2021, 96(7), pp. 1874-1881.
Tapio Salmi, Kari Eränen, Pasi Tolvanen, J.-P. Mikkola, and Vincenzo Russo Chem. Eng. Sci., 2020, 215, 115393.
Roger A. Sheldon and Dean Brady ACS Sustainable Chem. Eng., 2021, 9(24), pp. 8032–8052.
Maria Herrero Manzano, Kari Eränen, Kari, Adriana Freites Aguilera, Johan Wärnå, Sebastian Franz, Markus Peurla, Juan García Serna, Dmitry Murzin, and Tapio Salmi Ind. Eng. Chem. Res., 2021, 60(18), pp. 6483-6500.
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Environmentally benign and safe synthesis is enabled by highly active biocatalysts. To bolster economic and ecological aspects, catalyst reuse is essential and achieved by heterogenization of otherwise soluble enzymes onto solid supports. Here, this is demonstrated on novel renewable and non-polluting cellulose beads.
In the manufacture of liquid products, they may be coloured with appealing and brand-building colourants. During changes of batches, downtimes, or other regular day-to-day operations, coloured product residues are washed out of the process line. These are ideally recycled to minimize waste and maximize utility. For this, however, they need to undergo decolourization. Below we present a customer story in which the SpinChem RBR technoloy was deployed to decolourize viscous product residues.
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