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Liquid-Liquid Separators
Zaiput Flow Technologies’ patented liquid-liquid separators enable scalable liquid-liquid extraction/separation in flow. Extraction is conventionally performed in batch, which suffers from slow separation, emulsion formation, and difficulty scaling up.
Zaiput devices exploit membranes and contain an innovative on-board pressure control system to ensure that proper operating conditions for successful separation are always met. The presence of the on-board pressure controller practically decouples the operation of the separator from downstream operations, making the separator a truly modular, plug-and-play unit.
Our separators are rated for high pressure use allowing in-line separation in pressurized flow systems. Finally, our devices have a broad chemical compatibility, easy maintenance and come at an affordable price.
Important features:
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Plug-and-play
Zaiput separators incorporate on-board pressure control so that the separation performance is decoupled from any adjacent processing steps.
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Applicable for systems with negligible density differences
The operating principle behind the technology is based on a liquid’s wettable nature, so it works with any liquid-liquid system regardless of their density difference.
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Resolve your emulsion problems
Instead of using agitation to form microdroplets, we improve mixing by using a flow pattern that has large surface area, thus avoiding emulsions that generally cause separation issues.
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Minimal dead volume
Our device eliminates the need for moving or coalescing parts, so it has a drastically reduced dead volume.
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Excellent chemical compatibility
Machined in materials with excellent chemical resistance, Zaiput SEPs work with a wide range of organic solvents, in acidic and basic solutions. Please contact our technical support team with questions relating to chemical compatibility.
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Allows operation under pressure
The metal shell design allows Zaiput SEPs to be used inline with a pressurized process (up to 300 psi/ 2 MPa).
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Easy and direct scale-up
Our device is well-characterized and directly scalable from lab to pilot to production.
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Green technology
Our device shows excellent separation performance and high extraction efficiency, reducing solvent consumption. It is suitable for any chemical process, anywhere from bulk to high-value chemical industries.
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Inexpensive
Our devices comes at a lower price than competing technologies. Our devices also reduce your operating cost thanks to minimal maintenance and highly efficient performance.
It begins with a membrane’s wettability
Liquid-liquid membrane-based separation operates under the principle that only one phase will wet the membrane while the other phase will be non-wetting and retained.
Let’s see it live!
If the video does not play properly, click here to see our demo.
For further explanation see the image below. The membrane can be wetted by the organic (pink) phase.
Membrane-based separation relies on accurately controlling the pressure on each side of the membrane so that an incoming wetting phase can flow through the membrane pores while the non-wetting phase is retained.
Well, that sounds like an easy operation…
so what makes it challenging to implement?
Yes, that’s correct: membrane separation is relatively easy. However, there is one challenge that users have experienced in the past, which is the pressure difference across the membrane. In other words, we need to control the difference between P1 and P2 to ensure successful separation. Otherwise, if the difference is too high, we will start to see the non-wetting phase in the lower channel. If the pressure difference is too small, then we will start to see the wetting phase in the upper channel.
And that’s what makes Zaiput SEP unique!
In the past, this cumbersome pressure control required users to monitor P1 and P2 independently and carefully. This is especially true when the user operates the membrane separation in combination with other operation units, such as reactors, pumps, etc.
Zaiput Flow Technologies developed and patented a technology which negates all of the need for the pressure control. We integrated a self-tuning element, like the one in the picture below, such that the tedious adjustment of the pressures is no longer needed.
We currently offer three different versions of Zaiput SEP.
| Product | Image | Total Flow Rate (ml/min) | Wetted Parts | Max Operating Pressure (MPa) | Dead Volume | Dimensions (mm) |
|---|---|---|---|---|---|---|
| SEP-10 |  |
0-12 | Perfluorinated polymers | 2 | 400μl | 77 x 71 x 29 |
| SEP-200-SS |  |
20-200 | Stainless Steel 316, Perfluorinated polymers | 2 | 30ml | 206 x 196 x 26 |
| SEP-200-HS |  |
Hastelloy C276, Perfluorinated polymers | ||||
| SEP-3000 |  |
200-3000 | Check back for updates on the release date of this product. | |||
Representative applications:
Examples of liquid-liquid separations that are applicable to Zaiput SEP are shown below. Note that the applications are not limited to this representative list.
| Liquid 1 | Liquid 2 |
| Water NaCl solution HCl solution Brine liquor |
Light oil Alkanes (hexane, heptane, octane) Acetate (ethyl acetate, isopropyl acetate) Toluene Long-chain alcohols Diethylene glycols (at 60 ˚C) Methyl ethyl ketone Benzene |
NaCl solution
HCl solution
Brine liquor
Alkanes (hexane, heptane, octane)
Acetate (ethyl acetate, isopropyl acetate)
Toluene
Long-chain alcohols
Diethylene glycols (at 60 ˚C)
Methyl ethyl ketone
Benzene
Performance under pressure disturbance:
Zaiput SEP is designed to handle pressure disturbances in the system so that the separation of the liquid multiphase can be achieved without any manual control. To demonstrate this ability, we carried out the following experiments:
Here, we feed the separator with two immiscible liquids (water-hexane, water-ethyl acetate). The separator has a hydrophobic membrane inside. We simulated downstream operations or disturbances by setting a value of back pressure on the outlet of the organic stream. For successful complete separation, water should exit on one side, while the organic exits on the other side. That being said, there are two modes of incomplete separation:
(1) Retention of organic in the aqueous phase
(2) Breakthrough of water through the membrane with the organic phase
The results of experiments with either water-hexane or water-ethyl acetate are shown here (where R represents % of retention and B the % of breakthrough):
The results show that a simple separation (hexane/water, interfacial tension 50 mN/m) runs with complete separation at all of the tested total flow rates, with different ratios of flow rates, and at different levels of disturbances created in the system (with increasing back pressure on the organic side).
The separator has excellent performance also when challenged with a pair of liquids with very low interfacial tension (ethyl acetate/water, interfacial tension 6.8 mN/m). Under these conditions, the separator provided complete separation at different total flow rates and with different ratios of flow rates but tolerated fewer disturbances to achieve complete separation in a single step.
The Zaiput liquid-liquid separator can be used for a wide range of applications. Below are a few examples:
- Liquid-liquid extraction/In-line workup
- Biphasic reaction or quenching system
- Solvent switch (between reactions)
- Homogeneous catalyst recovery
- Separation of hazardous materials after in-situ generation
1. Liquid-liquid extraction/In-line workup
Liquid-liquid extraction is one of the primary purification methods, providing high selectivity and low energy consumption. Zaiput's technology provides the ability to perform the extraction in continuous flow with a simple plug-and-play device. It can be used in conjunction with different chemistries, with applications ranging from pharmaceuticals to polymer synthesis. Alternatively, it can be a standalone unit operating in any laboratory or industrial process.
Selected list of publications
Andrea Adamo, Rachel L. Beingessner, Mohsen Behnam, Jie Chen, Timothy F. Jamison, Klavs F. Jensen, Jean-Christophe M. Monbaliu, Allan S. Myerson, Eve M. Revalor, David R. Snead, Torsten Stelzer, Nopphon Weeranoppanant, Shin Yee Wong, Ping Zhang, On-demand continuous-flow production of pharmaceuticals in a compact, reconfigurable system Science April 2016.
Nicolas Lamborelle, Justine F Simon, Andre LUXEN and Jean-Christophe Monbaliu, Continuous-Flow Thermolysis for the Preparation of Vinylglycine Derivatives Org. Biomol. Chem. Nov 2015.
Irina Sagamanova, Carles Rodríguez-Escrich, István Gábor Molnár, Sonia Sayalero, Ryan Gilmour, and Miquel A. Pericàs, Translating the Enantioselective Michael Reaction to a Continuous Flow Paradigm with an Immobilized, Fluorinated Organocatalyst ACS Catal. Sept 2015.
Leibfarth FA, Johnson JA, and Jamison TF, Scalable synthesis of sequence-defined, unimolecular macromolecules by Flow-IEG Proc. Natl. Acad. Sci. Aug 2015.
2. Biphasic reaction or quenching system
In liquid-liquid reactions, often the reaction stream needs to be quenched by an immiscible phase. Zaiput’s liquid-liquid separator can be used downstream or inline to separate the biphasic reaction.
Selected list of publications
Baptiste Leforestiera and Markus Vögtle, Safe Generation and Direct Use of Chlorine Azide in Flow Chemistry: 1,2-Azidochlorination of Olefins and Access to Triazoles Synlett. June 2016.
Steffen Glöckner, Duc N. Tran, Richard J. Ingham, Sabine Fenner, Zoe E. Wilson, Claudio Battilocchio and Steven V. Ley, The rapid synthesis of oxazolines and their heterogeneous oxidation to oxazoles under flow conditions Org. Biomol. Mol. Oct 2014.
3. Solvent switch (between reactions)
Solvent switching is a common step in multistep synthesis. In general, it is done manually and in a batchwise process that is slow and tedious. Alternatively, Zaiput’s liquid-liquid separator can be inserted between two reactions by simply connecting the streams.
Selected list of publications
Trevor A. Hamlin, Gillian M. L. Lazarus, Christopher B. Kelly, and Nicholas E. Leadbeater, A Continuous-Flow Approach to 3,3,3-Trifluoromethylpropenes: Bringing Together Grignard Addition, Peterson Elimination, Inline Extraction, and Solvent Switching. Org. Process Res. Dev. Aug 2014.
4. Homogeneous catalyst recovery
A biphasic homogeneous-catalyzed reaction refers to catalysis that takes place at the interface between the two immiscible phases. Despite its high selectivity, it is difficult to operate at a large scale because it requires highly active mixing to keep the two liquids in contact. Even at small scale, homogeneous catalysis is rarely used because it poses problems with catalyst recovery via phase separation. Zaiput’s separator offers an easy and flexible way to separate the two phases and recover the catalyst.
Selected list of publications
Maryam Peer, Nopphon Weeranoppanant, Andrea Adamo, Yanjie Zhang, and Klavs F. Jensen, Biphasic catalytic hydrogen peroxide oxidation of alcohols in flow: Scale up and extraction Org. Process Res. Dev. Aug 2016.
Javier Guerra, David Cantillo and C Oliver Kappe, Visible-Light Photoredox Catalysis using a Macromolecular Ruthenium Complex: Reactivity and Recovery by Size-Exclusion Nanofiltration in Continuous Flow Catal. Sci. Technol. Feb 2016.
5. Separation of hazardous materials after in-situ generation
Flow synthesis becomes very useful for handling hazardous intermediates. This is because the compounds can be consumed directly into another flow synthesis without isolation. A recent example (e.g., Lehman, Dec 2016) includes the safe and scalable preparation of diazomethane, which involves the generation of a N-methyl-N-nitrosourea intermediate. At the end of diazomethane synthesis, Zaiput’s SEP is used to separate the desired product and waste. Alternatively, Zaiput’s SEP can be used for inline extraction of the hazardous intermediate in order to avoid a potentially unsafe off-line/batch-wise workup (e.g., Cantillo D et al, 2016).
Selected list of publications
Hansjoerg Lehmann, A scalable and safe continuous flow procedure for in-line generation of diazomethane and its precursor MNU. Green Chemistry. Dec 2016.
David Cantillo, Bernd Wolf, Roland Goetz, and C. Oliver Kappe, Continuous Flow Synthesis of a Key 1,4-Benzoxazinone Intermediate via a Nitration/Hydrogenation/Cyclization Sequence Org. Process Res. Dev. Dec 2016.
Scientific research articles using our separator:
Liquid-Liquid Separation
Gas-Liquid Separation
Hannes P. L. Gemoets, Gabriele Laudadio, Kirsten Verstraete, Prof. Dr. Volker Hessel, Dr. Timothy Noël, A Modular Flow Design for the meta-Selective C−H Arylation of Anilines Angew. Chem. Int. Ed. May 2017.
Nopphon Weeranoppanant, Andrea Adamo, Galym Saparbaiuly, Eleanor Rose, Christian Fleury, Berthold Schenkel, and Klavs F. Jensen, Design of Multistage Counter-Current Liquid–Liquid Extraction for Small-Scale Applications Ind. Eng. Chem. Res. Apr 2017.
C. Battilocchio, G. Iannucci, S. Wang, E. Godineau, A. Kolleth, A. De Mesmaeker and S. V. Ley Flow synthesis of cyclobutanones via [2 + 2] cycloaddition of keteneiminium salts and ethylene gas React. Chem. Eng. Mar 2017.
Joshua Britton and Colin L. Raston, Multi-step continuous-flow synthesis Chem. Soc. Rev. Jan 2017.
David Cantillo, Bernd Wolf, Roland Goetz, and C. Oliver Kappe, Continuous Flow Synthesis of a Key 1,4-Benzoxazinone Intermediate via a Nitration/Hydrogenation/Cyclization Sequence Org. Process Res. Dev. Dec 2016.
Hansjoerg Lehmann, A scalable and safe continuous flow procedure for in-line generation of diazomethane and its precursor MNU. Green Chemistry. Dec 2016.
Maryam Peer, Nopphon Weeranoppanant, Andrea Adamo, Yanjie Zhang, and Klavs F. Jensen, Biphasic catalytic hydrogen peroxide oxidation of alcohols in flow: Scale up and extraction Org. Process Res. Dev. Aug 2016.
Franz J. Strauss, David Cantillo, Javier Guerrac and C. Oliver Kappe, A laboratory-scale continuous flow chlorine generator for organic synthesis React. Chem. Eng. Aug 2016.
Baptiste Leforestiera and Markus Vögtle, Safe Generation and Direct Use of Chlorine Azide in Flow Chemistry: 1,2-Azidochlorination of Olefins and Access to Triazoles Synlett. June 2016.
Andrea Adamo, Rachel L. Beingessner, Mohsen Behnam, Jie Chen, Timothy F. Jamison, Klavs F. Jensen, Jean-Christophe M. Monbaliu, Allan S. Myerson, Eve M. Revalor, David R. Snead, Torsten Stelzer, Nopphon Weeranoppanant, Shin Yee Wong, Ping Zhang, On-demand continuous-flow production of pharmaceuticals in a compact, reconfigurable system Science April 2016.
L Osorio-Planes, C Rodríguez-Escrich, MA Pericas, Removing the superfluous: a supported squaramide catalyst with a minimalistic linker applied to the enantioselective flow synthesis of pyranonaphthoquinones Catalysis Science & Technology Mar 2016.
Lorenzo Di Marco, Dr. Morgan Hans, Prof. Lionel Delaude and Dr. Jean-Christophe M. Monbaliu, Continuous-Flow N-Heterocyclic Carbene Generation and Organocatalysis Chem. Eur. J. Feb 2016.
Javier Guerra, David Cantillo and C Oliver Kappe, Visible-Light Photoredox Catalysis using a Macromolecular Ruthenium Complex: Reactivity and Recovery by Size-Exclusion Nanofiltration in Continuous Flow Catal. Sci. Technol. Feb 2016.
Nicolas Lamborelle, Justine F Simon, Andre LUXEN and Jean-Christophe Monbaliu, Continuous-Flow Thermolysis for the Preparation of Vinylglycine Derivatives Org. Biomol. Chem. Nov 2015.
Irina Sagamanova, Carles Rodríguez-Escrich, István Gábor Molnár, Sonia Sayalero, Ryan Gilmour, and Miquel A. Pericàs, Translating the Enantioselective Michael Reaction to a Continuous Flow Paradigm with an Immobilized, Fluorinated Organocatalyst ACS Catal. Sept 2015.
Leibfarth FA, Johnson JA, and Jamison TF, Scalable synthesis of sequence-defined, unimolecular macromolecules by Flow-IEG Proc. Natl. Acad. Sci. Aug 2015.
Chunhui Dai, David R. Snead, Ping Zhang, and Timothy F. Jamison, Continuous-Flow Syn and Purification of Atropine with Sequential In-Line Separations of Structurally Similar Impurities J. Flow Chem. July 2015.
Steffen Glöckner, Duc N. Tran, Richard J. Ingham, Sabine Fenner, Zoe E. Wilson, Claudio Battilocchio and Steven V. Ley, The rapid synthesis of oxazolines and their heterogeneous oxidation to oxazoles under flow conditions Org. Biomol. Mol. Oct 2014.
Trevor A. Hamlin, Gillian M. L. Lazarus, Christopher B. Kelly, and Nicholas E. Leadbeater, A Continuous-Flow Approach to 3,3,3-Trifluoromethylpropenes: Bringing Together Grignard Addition, Peterson Elimination, Inline Extraction, and Solvent Switching. Org. Process Res. Dev. Aug 2014.
Andrea Adamo, Patrick L Heider, Nopphon Weeranoppanant, and Klavs F. Jensen, Membrane-Based, Liquid-Liquid Separator with Integrated Pressure Control. Ind. Eng. Chem. Res. July 2013.
Jisong Zhang, Andrew R. Teixeira, Lars Thilo Kögl, Lu Yang, and Klavs F. Jensen Hydrodynamics of gas–liquid flow in micropacked beds: Pressure drop, liquid holdup, and two-phase model AIChE Journal June 2017.
Everett J. O’Neal, Chang Ho Lee, Julian Brathwaite, and Klavs F. Jensen, Continuous Nanofiltration and Recycle of an Asymmetric Ketone Hydrogenation Catalyst ACS Catal. March 2015.
Reference to separator’s theory:
Kralj, J. G.; Sahoo, H. R.; Jensen, K. F., Integrated continuous microfluidic liquid-liquid extraction. Lab Chip.2007, 7, (2), 256-263.
Reference to examples of use of liquid–liquid separators:
Sahoo, H. R.; Kralj, J. G.; Jensen, K. F., Multistep Continuous-Flow Microchemical Synthesis Involving Multiple Reactions and Separations. Angew. Chem. Int. Ed. 2007, 46, (30), 5704-5708.
Cervera-Padrell, A. E.; Morthensen, S. T.; Lewandowski, D. J.; Skovby, T.; Kiil, S.; Gernaey, K. V., Continuous Hydrolysis and Liquid–Liquid Phase Separation of an Active Pharmaceutical Ingredient Intermediate Using a Miniscale Hydrophobic Membrane Separator. Org. Process Res. Dev. 2012, 16, (5), 888-900.
