Downstream processing

The manufacturing of pharmaceuticals, cosmetics and food items consists largely of altering the structure or function of chemicals and chemical compounds. To reach a satisfactory quality of the end-products, there is often also a need for downstream processing, including purification, extraction and polishing. Two solid materials commonly used for such heterogeneous procedures are activated carbon and ion exchangers.

Activated carbon is produced by exposing carbon-rich material to high temperatures under certain conditions; the source material is either pre-treated with chemicals, or exposed to hot gases to achieve a porous structure. The resulting material has a vast surface area (>3000 m²/g) due to the tiny pores having been created between the carbon atoms. The excessive porosity makes activated carbon a suitable material for adsorption, where molecules adhere to a surface by van der Waals forces. Due to this, activated carbon is commonly used in the chemical industry to remove organic impurities in the production of pharmaceuticals and fine chemicals. Other areas of usage include metal extraction, mercury scrubbing, and the purification of various liquids and gases, including polluted water and air.

Ion-exchangers are used to purify, separate, decontaminate and catalyse a wide variety of chemical compounds and processes. These polymeric matrices are typically cross-linked into porous microbeads in the size range of 200-500 µm. The properties of ion-exchange resins are determined by the functional groups attached to the internal and external surfaces of the beads. The two most common types of ion exchange resins are anion and cation exchangers, which attract negatively and positively charged ions, respectively. During an ion exchange process, the resin beads acts as a medium to which charged compounds bind, as the loosely bound ions originally attached to the resin are released into the solution. Ion exchangers are not physically altered by the process, and are, by definition, insoluble acids or bases with equally insoluble salts.

Rotating bed reactors

In downstream processing, the soluble compound of interest must come in contact and interact with the solid particles conducting the purification, extraction or polishing. The mass transfer in these cases can be mediated by packed columns, also known as fixed bed reactors (FBR), or by stirred tank reactors (STR). However, these methods have their drawbacks, such as low flow rate, high back pressure, limited mass transfer and mechanical stress on the solid phase particles.

With the SpinChem® rotating bed reactor (RBR), the solid phase is kept inside a rotating stainless-steel cylinder. As the cylinder spins, solution is pushed through the filters of the cylinder and through the packed bed within by centrifugal forces. Simultaneously, new solution enters the cylinder through the centre hole to subsequently be pushed through the bed, thus repeating the process. This allows every liquid parcel to do multiple passages through the bed, optimizing the resin utilization. By increasing the rotational speed of the RBR, the process can be sped up without risking degradation of the solid phase, which is kept well-protected from mechanical forces. The SpinChem® RBR works perfect with ion-exchange resins and granular activated carbon in downstream processing applications. Due to the enhanced mass transfer, the SpinChem® RBR allows for the use of larger, more manageable solid phase particles, without suffering from reduced reaction speed or inferior efficiency.

Application 1015
A remote controlled raft for treatment of surface water using rotating bed reactor technology

Time lapse video demonstrating a prototype vehicle capable of processing two cubic metres of coloured water within five minutes. The raft was carrying two rotating bed reactors that neutralized the basic surface water in a square pond by ion exchange.  Keywords: Cleantech, Ion exchange, Seamless scaleup, Technology

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 L1801
Advanced oxidation process for the removal of ibuprofen from aqueous solution: A non-catalytic and catalytic ozonation study in a semi-batch reactor

Degradation of the pharmaceutical compound ibuprofen by ozone, was optimized in batch type reactors with and without zeolite based heterogeneous catalysts. The rotating bed reactor technology increased the concentrations of dissolved gas compared to traditional stirred tank reactors and allowed convenient handling of the catalyst particles without any filtration.  Keywords: Fast reaction, Gas-distribution, Organic molecules, Scientific literature, Zeolite

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 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 1006
Comparison of reaction speed with rotating bed reactor and stirred tank reactor

Video revealing the efficient mass transfer and resulting shorter reaction time with a rotating bed reactor (RBR) during ion-exchange neutralization of a base. The reaction with the RBR finished 30% faster and left a completely clear solution without any particles. Keywords: Fast reaction, Ion exchange, 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 1031
Decolourization in an IBC tank using the ProRBR IBC add-on

Adsorption of methylene blue (3 g, 5 mg/L) onto Purolite® NRW1160 (4.2 L) placed in a SpinChem® S5 RBR operated at 147 rpm. The SpinChem® S5 RBR was placed within a 600 L IBC tank, using the ProRBR IBC add-on, where the tank was filled with water. The data was acquired using a UV-VIS spectrophotometer.  

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 1026
Decolourization with activated carbon in a production scale rotating bed reactor

Accelerated video showing the removal of methylene blue from 50 L volume of liquid, by adsorption onto activated carbon in a production scale rotating bed reactor (RBR). The decolouration process removed 99.96% of the dye within 10 minutes with a logarithmic decline of concentration as documented by analysis of withdrawn samples.  Keywords: Activated carbon, Decolouration, Organic molecules, Purification, Seamless scaleup, Technology

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 1021
Demonstration of loading, reaction and unloading in a production scale rotating bed reactor

Video showing how a SpinChem® rotating bed reactor (RBR) for use in 20-300 L vessels was charged with solid particles, used for pH neutralization, drained from reaction liquid and finally emptied from solid phase without opening the RBR. This procedure illustrates one approach to using RBR in production scale equipment without opening the reaction vessel.  Keywords: Easy handling, Ion exchange, Seamless scaleup, 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 L1402
Lipase catalyzed regioselective lactamization as a key step in the synthesis of N-Boc (2R)-1,4-oxazepane-2-carboxylic acid

A synthesis of N-Boc (2R)-1,4-oxazepane-2-carboxylic acid was developed in 39% yield over seven steps starting from methyl (2R)-glycidate. The key step was a lipase-catalyzed regioselective lactamization performed using SpinChem® rotating bed reactor that simplified work up and recycling of the enzyme. Carl-Johan Aurell*, Staffan Karlsson, Fritiof Pontén, and Søren M. Andersen Keywords: Biotransformation, Immobilized enzymes, Organic molecules, Quick recycling, 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 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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