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
Dramatically improved deionization with a rotating bed reactor

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.

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

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.

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, and Selin Kara Green Chemistry, 2022, 24(18), pp. 6889-6899.

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.

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

To underscore the use of rotating bed reactors (RBR:s) on scale, a decolorization was performed in a 7500 L tank using ion exchange resin.

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.

Application Brochure
Mass transfer revolutionized

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.

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

Oliver Fellechner and Irina Smirnova Can. J. Chem. Eng., 2021, 99, pp. 1035-1049.

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 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 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.

Application 1032
Rotating bed reactor for immobilized enzymatic reactions

This case study presents a lipase-mediated stereoselective acetylation of a racemic amine in a rotating bed reactor.

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 cooperation 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.

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.

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

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.

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.

Application L2005
Solvent and rotating bed reactor extraction with one- and two-phase solvents applied to bilberries (Vaccinium myrtillus) for isolating valuable antioxidants

Josefina Nyström, Ulla-Britt Östman, Torgny Mossing, Leif Hed, and Paul Geladi Food Anal. Methods, 2020, 13, pp. 933-941.

Application 1022
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.

Application 1041
Treatment of 7.5 m3 with a 50 L 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 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.

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 in the long run. The need for new equipment may inflict delays and affect your 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, and Mikelis Kirpluks J. Polym. Environ., 2022, 30, pp. 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 L2116
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.

Application L2111
Streamlining design, engineering, and applications of enzymes for sustainable biocatalysis

Roger A. Sheldon and Dean Brady ACS Sustainable Chem. Eng., 2021, 9(24), pp. 8032–8052.

Application L2106
Interaction of intrinsic kinetics, catalyst durability and internal mass transfer in the oxidation of sugar mixtures on gold nanoparticle extrudates

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.

Application L2008
Probing batch and continuous flow reactions in organic solvents: Granulicella tundricola hydroxynitrile lyase (GtHNL)

José Coloma, Yann Guiavarc'h, Peter-Leon Hagedoorn, and Ulf Hanefeld Catal. Sci. Technol., 2020, 10(11), pp. 3613-3621.

Application L2201
A critical review on ibuprofen removal from synthetic waters, natural waters, and real wastewaters by advanced oxidation processes

Enric Brillas Chemosphere, 2022, 286, Part 3, 131849.

Application L2208
Process intensification in oxidative biocatalysis

Guillem Vernet, Markus Hobisch, and Selin Kara Curr. Opin. Green Sustainable Chem., 2022, 38, 100692.

Application 1069
Cellulose-bead immobilized enzymes as biodegradable and renewable catalysts

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.

Application 1070
Decolourization of product residues

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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