Multistage Extraction

  • Countercurrent extraction
  • Bench top to plant scale
  • PLUG & RUN
  • High extraction efficiency

Description

Multistage Liquid Liquid Extraction (LLE) is a process where multiple extraction steps are repeated in order to increase the recovery of a product. This process is required when, due to a small partition coefficient, the recovery in a single extraction step is insufficient.

In industrial applications, LLE is most often arranged with a “countercurrent extraction scheme” (CC-LLE) that provides the smallest consumption of extractant. In this scheme, the aqueous raffinate from one stage is fed to a former stage as a feed while the organic phase is moved in the opposite direction. Hence, even if the recovery of product in each stage is small, the overall system can achieve a high level of recovery.

In other words, with multistage extraction, selectivity of the extraction and process yield are decoupled as the yield depends on the number of extraction stages used, thus providing greater freedom to the process developer.

Important features:

  • Our lab scale platform (MS-10) is the only existing tool for bench liquid-liquid counter-current extraction process development
  • Minimal internal volume
  • ~3ml per stage at MS-10 scale
  • Easily scalable to pilot (MS-200) and production (MS-3000 or MS-40K)
  • Easy to use and clean
  • Simple to add/remove extraction stages
  • Addresses the most difficult extractions
  • High extraction efficiency
  • Provides a continuous solvent extraction solution

Why is this System Helpful?

Efficiency Counter-current extraction

Fig 1 – Multistage extraction efficiency

  • The power of multistage extraction can be seen in Fig 1 which shows the extraction efficiency of three different systems with a partition coefficient of 1 (50/50 partitioning of solute).
  • As the number of stages increases, extraction efficiency increases, while still using the same amount of material that would be used if only one batch step was performed.
  • Zaiput can assist you in modeling your expected extraction efficiency for different scenarios.

This system addresses 3 key challenges typically encountered in developing multi-stage LLE: lack of information, lack of material and difficulty in scale up.

  • Lack of Information. In Multicomponent Systems, Equilibrium data are generally obtained by thermodynamic models (e.g. UNIQUAC, NRTL) but they are often inaccurate due to (1) lack of equilibrium data, (2) unavailable physical property data, especially for unidentified molecular species. As a result, experimental work is needed.
  • Lack of material. Counter current Extraction is difficult to simulate in laboratory experiments with standard equipment; many experiments and large amounts of material are required. This platform needs 1 to 2 orders of magnitude less material per experiment than any other method.
  • Difficult scale up. Scalability of CC-LLE is challenging with standard equipment (centrifuges, columns, mixer settlers); requires a lot of time and material for optimization. This platform offers seamless scalability up to production.
Technology Mixer Settler
 Columns
 Centrifuges
 Zaiput
Typical Internal Volume per Stage at Lab scale (ml) 25-100 150 100 3

How It Works

Process Description

  • Our counter-current extraction platforms offers an easy to use device to run and optimize Countercurrent extraction processes at the laboratory scale by leveraging our membrane based separation technology and lab scale devices, to then scale-up to production scale separators.
  • Fig 1 outlines the standard plumbing of the system. Interstage pumping is required in multistage countercurrent solvent extraction to allow the solvent of a step to be used upstream as a feed.
  • Each extraction stage is obtained by first contacting the two phases (mass transfer is achieved inside a portion of tube with two phase flow—black lines in fig 1) and then phase separation is obtained with a Zaiput phase separator.
  • Our lab-scale platform MS-10 has been designed with 5 extraction stages; fewer stages can be obtained by excluding some devices, more stages can be obtained by adding another platform in series.

Larger throughput platforms are delivered with the amount of stages needed by your process.

  • Counter-current Liquid Liquid Extraction

 

Fig 1. Schematic of the standard system plumbing

Device Description

MS-10 (fig 2) captures the process shown in (fig 1) using five SEP-10s and a variety of components outlined below:

  • Interstage pumping is achieved using a small diaphragm pump in conjunction with Zaiput ’s Pulsation Dampener (DMP-10) to achieve smooth flow in a compact space.
  • Tube coils for mass transfer are wound onto supports and can be replaced; their length can be optimized to achieve full equilibrium at each stage (as a result the process efficiency will approach theoretical values).
  • Electrical Switches allow pump exclusion (if less than 5 stages are in use), a knob allows control of the interstage pump flow rate to help eliminate air at system start-up.
  • The unit has also quick release bays for hot-swapping and to facilitate system maintenance.
  • The system frame is made of Stainless Steel to provide solvent resistance and excellent durability.
  • The utilization of standard fittings allows the user to customize the process scheme, if needed.
  • For operation it needs only external metering pumps to supply aqueous and organic. External metering pumps are not provided with the lab-scale device (MS-10), but can be provided with the larger devices.
  • The very small internal volume (~3ml per stage) results in a quick time to steady state and low consumption of material for process optimization/ experimental data collection. Its internal volumes are 1 to 2 orders of magnitude less than alternative LLE extraction technologies.

 

MS-10 Zaiput CCLLE

Fig 2. Multistage Liquid-Liquid Extraction Platform

Process Scale Up

  • A process that has been optimized at the laboratory/bench scale can be scaled up using our pilot plant units (SEP-200) or production scale units (SEP-3000 and SEP-40K).
  • Set up for the larger units is typically customized for the specific application/ process developed at the MS-10 scale. Contact us for assistance.

 

MS-200

multistage liquid liquid separation using Zaiput liquid liquid separators

MS-3000

 

multistage liquid liquid separation at production scale using Zaiput liquid liquid separators

Literature

C. Heiduk, I. Hohlen, and S. Scholl, Multi-Stage Liquid/Liquid Extraction with a Zaiput Apparatus, SPhERe – 4rd International Symposium on Pharmaceutical Engineering Research, 15. – 17. Sept 2021.

Nopphon Weeranoppanant and Andrea Adamo, In-Line Purification: A Key Component to
Facilitate Drug Synthesis and Process Development in Medicinal Chemistry, ACS Med. Chem.
Lett., Dec 2019.

René Lebl, Trevor Murray, Andrea Adamo, David Cantillo, C. Oliver Kappe, Continuous Flow
Synthesis of Methyl Oximino Acetoacetate: Accessing Greener Purification Methods with Inline Liquid-Liquid
Extraction and Membrane Separation Technology, ACS Sustainable Chem. Eng., Nov 2019.

Scientific research articles relating to our multistage extraction platform:

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.

Yi Shen, Nopphon Weeranoppanant, Lisi Xie, Yue Chen, Marcella R. Lusardi, Joseph Imbrogno, Moungi G. Bawendi and Klavs
F. Jensen, Multistage extraction platform for highly efficient and fully continuous
purification of nanoparticles Nanoscale Mar 2017.

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.

Specifications

Contact us if you need more than 5 stages. Platforms can be easily connected together.

Part Number MS10-5
Width 500 mm (19.7 inches)
Depth 400 mm (15.7 inches)
Height 155 mm (6.1 inches)
Total flow rate 0-10 ml/min
Wetted parts:
Separators ETFE, PFA, FEP, PTFE
Tubing/ flow sensors PFA
Interstage pumps FFMK, PVDF
Ports 1/4-28 Flat bottom
Max temperature of operation 80°C
Hold-up volume per stage ~3 ml

MS-200 Platforms are custom-built to our customers’ specifications

 Part Number MS200
Dimensions

Dimensions depend on number of stages specified

but platforms fit in a lab hood
Total flow rate 5 – 200 ml/min
Wetted parts:
Separators 316-SS, ETFE or Hastelloy C-276

PFA, FEP, PTFE
Tubing/ flow sensors PFA
Interstage pumps FFMK, PVDF
Ports Swagelok for 1/4” OD
Max temperature of operation 80°C
Hold-up volume per stage ~45 ml—Depends on Setup.

 

MS-3000 Platforms are custom-built to our customers’ specifications

 Part Number MS3000
Dimensions Dimensions depend on number of stages specified
Total flow rate 200 – 3000 ml/min
Wetted parts:
Separators 316-SS, ETFE or Hastelloy C-276

PFA, FEP, PTFE
Ports Swagelok for 3/8” OD
Max temperature of operation 80°C
Hold-up volume per stage ~500 ml – Depends on Setup
Contact us if you are interested in a MS-40K (40 L/min) platform

Ordering Information