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 decolourization comparing rotating bed reactor and stirred tank reactor

Accelerated video showing the enhanced adsorption rates of methylene blue onto activated carbon using a rotating bed reactor (RBR) compared to a stirred tank reactor (STR). The RBR decolourized the solution almost twice as fast, did not create any visible fines and required no filtration.  Keywords: Activated carbon, Decolouration, Fast reaction, Organic molecules, Simple cleanup, Technology 

Application 1012
An externally connected system for large scale heterogeneous downstream processing

Time lapse video illustrating how an externally connected rotating bed reactor (RBR) can pump and process large liquid volumes by the convective flow created by the spinning RBR. The concept enables handling of volumes at least 10-100 times larger than the external vessel, thus facilitating installation of RBR technology into existing plant equipment.  Keywords: Activated carbon, Continuous flow, Decolouration, Organic molecules, Seamless scaleup, Technology

Application 1007
Automated semi-continuous batch processing system with rotating bed reactor

Video showing the principle of an automated rotating bed reactor system capable of filling a solution, neutralizing it by ion exchange and draining it. By microcomputer control, unattended semi-continuous batch processing was accomplished for many cycles until the ion exchanger was completely saturated.  Keywords: Automation, Ion exchange, Seamless scaleup, Technology

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, Jyri-Pekka MikkolaTopics in Catalysis, 59 (2016) 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
Comparing rotating bed reactor and fixed bed reactor for adsorption purification

Comparison of rotating bed reactor (RBR) technology and fixed bed reactor (FBR) column during activated carbon decolourization. The more efficient use of the adsorbent with a SpinChem® RBR enabled completion of the process within 40% of the time at the same material amount or allowed reduction to 50% material while still being able to finish the process within the same time as the FBR.  Keywords: Activated carbon, Decolouration, Fast reaction, Organic molecules, Purification, Technology  

Application 1004
Consequences of viscous solutions on the reaction rate with rotating bed reactors

Log-log plot of how viscosity affects the reaction time for a mass transfer limited reaction at a fixed rotational speed of a rotating bed reactor (RBR). The RBR behaved very predictably and delivered reaction times that increased linearly with reaction media viscosity up to at least 500 mPa·s.  Keywords: Ion exchange, Organic molecules, Technology, Viscous solutions  

Application 1030
Decolouration of highly viscous solutions using a rotating bed reactor and a stirred tank reactor

The performance of a SpinChem® rotating bed reactor (RBR) in the treatment of highly viscous solutions was compared to that of a conventional stirred tank reactor (STR). Both reactor set-ups were used for the extraction of Allura red dye from a glycerol-dye mixture using an ion exchange resin. The RBR removed 10 times the amount of dye in just over 40 % of the time, compared to the STR. This comparison underlines the efficient mixing and clever design of the SpinChem® RBR, as well as the broad spectrum of applications for which this technology is highly relevant.  Keywords: Decolouration, Fast reaction, Ion exchange, Technology, Viscous solutions    

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, Jyri-Pekka MikkolaCarbohydrate Polymers, 136 (2016) 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  

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
Effective phase-transfer between immiscible liquids and an ion exchange resin

Illustrative video showing how a phenolic colourant is deprotonated and extracted from an organic to an aqueous solvent. Using SpinChem® RBR in a flower-baffled reaction vessel created fine emulsion droplets resulting in effective phase-transfer between the two liquids and the solid phase. Keywords: Immiscible liquids, Ion exchange, Organic molecules, Technology

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

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

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

Comparison of SpinChem® rotating bed reactor (RBR) with traditional reaction set-ups for a demanding biotransformation. SpinChem® RBR matched or outperformed the other systems and gave a 10 to 25-fold more time-efficient recycling of the encapsulated cells.   Keywords: Alginate, Biotransformation, Encapsulated cells, Gas-distribution, Organic molecules, Quick recycling

Application 1028
Enzyme immobilization screening using magnetic rotating bed reactors

The SpinChem® MagRBR ECR screening kit, pre-packed with Purolite® Lifetech™ resins, was used to screen six different enzyme carrier resins in parallel for the immobilization of lipase CalB. Easy sampling and monitoring of the process, together with effortless handling, established the MagRBR as a time and labour efficient screening device. Keywords: Biotransformation, Easy handling, Immobilized enzymes, Rapid screening

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

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

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

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 1001
Optimizing the rotational speed of rotating bed reactors in baffled reaction vessels

Investigation of how rotational speed influences the efficiency of rotating bed reactors (RBR) for a diversity of processes such as adsorption, neutralization and ammonolysis. It was demonstrated how reaction rates could reach a plateau with the SpinChem® RBR when mass transfer efficiency exceeded reaction speed.   Keywords: Activated carbon, Fast reaction, Immobilized enzymes, Ion exchange, Technology

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

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

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 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
Rotating bed reactor setup for in situ formation, loading and handling of alginate beads and whole cell encapsulation

Video showing the formation of alginate beads under conditions mimicking whole cell encapsulation. The use of a SpinChem® rotating bed reactor (RBR) allowed easy collection, maturing and washing of the alginate beads. With the RBR setup, it was possible to immediately continue with filling of the reaction substrate into the same vessel, thus reducing the number of handling steps and facilitating bead recycling. The beads showed no signs of physical wear after use in the RBR.   Keywords: Alginate, Biotransformation, Easy handling, One-pot multistep, Technology

Application 1010
Rotating bed reactors completely avoid grinding of molecular sieves

Photos showing how grinding caused by stirring of molecular sieves can be completely avoided by using a rotating bed reactor (RBR). Molecular sieves contained in a RBR for a 200 mL vessel can theoretically hold 0.23 moles of water. This allows synthesis of product in the range of 100 gram by ester condensation or drying of 25 litres of analytical grade organic solvent. Keywords: Easy handling, Molecular sieve, Purification, Simple cleanup, Synthesis, Technology, Water

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 1009
Simultaneous extraction of two dyes selectively onto different resins

Video illustrating how a mixture of red and blue dyes with different chemical properties can be selectively extracted onto different adsorbents within the same run using a rotating bed reactor (RBR). The dyes were separated based on ionic and hydrophobic interactions, respectively.  Keywords: Cleantech, Decolouration, Extraction, Ion exchange, One-pot multistep, Organic molecules, Polymeric resin, Technology

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

Application 1022
Transfer hydrogenation with catalyst recycling in a rotating bed reactor

Convenient transfer hydrogenation catalysed by palladium-containing beads was performed using a SpinChem® rotating bed reactor (RBR). The set-up resulted in high product conversions throughout more than 10 consecutive batches without any need for filtration to recycle the catalyst.  Keywords: Easy handling, Organic molecules, Palladium on carbon, Quick recycling, Synthesis

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

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