- Dissolution: A wide range of extractors based on green solvents . Equipment to perform solvent extraction from lab scale up to 30 L (extension foreseen to 90 L), Supercritical fluid extraction (kg-scale), Accelerated solvent extraction, pressurized liquid/water extraction.
- Depolymerization: A series of catalytic batch reactors (6) allowing the study of pressurized reactions up to 600 oC. Continuous fix bed reactor at TRL 4, whereby a pilot (TRL 6) will be available Q1-2022. The reactors are suitable for H2 and allow the study of reductive depolymerisation. Work up equipment like filtration, rotavap, (vacuum) oven….
- Upgrading: A wide range of downstream processing equipment for solvent based precipitation, membrane filtration (dead end, cross flow, coupled), specific membrane equipment allowing high temperature filtration, heat stable (functionalized) ceramic membranes. Equipment available till TRL 6.
- Analytical tools: A wide range of analytical tools: GC (TCD, MS, FID), GCxGC (MS) , LC (MS, MSxMS, DAD, PAD, ELSD), benchtop NMR, FT-IR, UV-VIS, GPC, IPC-AAS.
- Material characterization: A wide range of tools to characterize polymers: Rheology, TGA, DSC.
Synthesis and Chemical modification
Labscale batch reactors
Name of the device
High T/P SS reactors
Applications
This lab scale reactor sets with mechanical overhead stirrers allow to perform reactions at high temperature and pressure, using organic solvents - batch and continuous. This set-ups allows closed reactions in vacuum and in inert atmosphere.
Features
The available reaction vessels have a capacity of 100 mL, 200 mL, and 2 L. They can operate at enhanced conditions (150 – 400 oC, -> 600 bar ), (supercritical) CO2-based processes and reactions, and H2-based processes and reactions with extra safety measures.
Name of the device
Glass reactors
Applications
This lab scale reactor sets with mechanical overhead stirrers allow to perform viscous reactions which cannot be performed using a magnetic stirring bar. This set-up allows closed reactions in vacuum and in inert atmosphere.
Features
The available reaction vessels have a capacity of 100 mL, 250 mL, 6 L and 30 L. The small reactors do not contain a bottom valve. The mechanical stirrer has a maximum rotation speed of 2000rpm (IKA RW20).
Labscale Continuous reactor
Labscale Continuous reactor
Name of the device
Mini - pilot
Applications
This lab scale set-up allows continuous processing with different units: a feed vessel, a continuous reactor, and a collection vessel. This set-up allows reactions/extractions in inert atmosphere, or with hydrogen; with and without catalyst.
Features
The available reaction feed vessel has a capacity of 1L (feed vessel, stirred), the catalytic bed is 40 mL; The reactor runs up to 325 oC, and up to 150 bar.
Chemical analysis
Attenuated total reflectance-fourier transfor infrared (ATR-FTIR)
Name of the device
Nicolet iS10 spectrometer.
Applications
FTIR is a classical technique for the characterization of chemical molecules and materials, specially organic based. The theory behind FTIR is the vibration of the bonds of the molecules. Therefore, different functional groups give different signal or peaks in a FTIR spectra. This technique is useful for several applications.
- Characterization of organic molecule and materials.
- Monitoring reactions in terms of chemical conversion
- Curing/reaction kinetics
- Impurities detection (qualitative)
Features
ATR device which allows to measure solid and liquid samples without any additional sample preparation.
Heating device, allows to heat up the sample while measuring.
Physical analysis
Benchtop NMR 80 MHz
Name of the device
Magritek Benchtop Spinsolve 80 MHz ULTRA spectrometer
Description
NMR spectroscopy is one of the most used and powerful techniques for molecular characterization. It allows the detection of mainly 1H, 13C, 31P and 19F nuclei, among others. By studying the peaks of nuclear magnetic resonance spectra, chemists can determine the structure of many organic compounds.
Applications
- Structural characterization of organic molecules and polymers.
- Purity of compounds
- 31P for the quantification of OHs groups (crucial in lignin developments).
- Determination of compounds ratio in mixtures
- In-line detection and reaction monitoring in real time (using the Spinsolve device)
Features
- Probe for 1H NMR analysis
- Probe for 31P NMR analysis
Thermal and mechanical analysis
Name of the device
TA Discovery DSC 250
Applications
DSC measures temperatures and heat flows associated with thermal transitions in a material.
- Glass transitions, Melting & Crystallization
- Heat Capacity
- Crosslinking & Curing
- Solid-solid transitions
- Oxidation
Features
-
Autosampler.
-
Modulated DSC (MDSC) for the separation of complex thermal event.
Name of the device
TA Discovery DMA 850
Applications
DMA measures the mechanical properties of materials as a function of time, temperature, and frequency. DMA is commonly used to measure glass transition temperatures and secondary transitions, orientation caused by processing, cold crystallisation, cure optimization, filler effect in composites,… DMA provides an accurate measure of material stiffness (modulus) but also other important mechanical properties such as damping, creep and stress relaxation.
- Viscoelastic properties (E’, E’’, tan δ)
- Glass transition
- Frequency effects
- Creep and recovery
- Stress relaxation
- Secondary transitions
- Softening and melting temperature
- Time-temperature superposition
- Aging
- Curing of networks
- Crosslinking density
- Orientation effects
- Stress-strain curves
Features
-
Force range: 0.0001 to 18N.
-
Temperature range: -150 °C to 600 °C.
Name of the device
TA Discovery Hybrid Rheometer 2
Applications
Rheology is the study of flow and deformation, or stress-strain relationship of materials. Rheometers measure materials from low viscosity liquids to stiff solids in terms of viscosity, modulus, and elasticity or damping.
Most industrially relevant materials exhibit complex rheological behavior that determines processability and end-use performance. A rheometer can be used to measure and understand how rheological properties influence every stage of industrial production.
- Understand formulation based on rheological properties
- Make predictions of material performance based on known use conditions without specifically mimicking application conditions
- Optimize properties such as spreading, pourability, stability during storage
Accessories
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Advanced Peltier plate.
-
Cone and parallel plate accessory.
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Environmental test chamber.
Name of the device
Tensile Instron machine model 5582
Applications
Tensile allows a wide range of mechanical properties testing. Simple changes of setup allow for measurement of tensile, flexural and compressive properties.
- Elongation measurements
- Tensile stress-strain data
- Young’s modulus
Operations Range
-
Load: 100 kN
-
Speed: 0.05 to 500 mm/min
Material development
Name of the device
WS-650 Series spin processor (Laurell Technologies Corporation)
Applications
Spin coating is a procedure used to deposit uniform thin films to flat substrates. Usually a small amount of coating material is applied on the center of the substrate, which is either spinning at low speed or not spinning at all. The substrate is then rotated at high speed in order to spread the coating material by centrifugal force.
Features
This 650-series coater system will accommodate up to ø150mm wafers and 5" × 5" (127mm × 127mm) substrates, and features a maximum rotational speed of 12,000 RPM (based on a ø100mm silicon wafer).
Pilot facility
Name of the device
Reactor Solvent-Based Dissolution/Extraction. PILLAR II
Description
- A flexible, multi-purpose extraction unit for: Dissolution of lignin in an organic solvent (solvolysis)
- Compatible with Lignovalue as feed reactor.
Applications
Extraction of biobased components from lignin using organic solvents
Features
-
Stainless steel and/or Hastelloy
-
1.5 m³ reactor vessel
-
Capacity: Lignin solvolysis: 1.8 – 18 kg/h of solubilized lignin (compatible with capacity range LignoValue). Extraction of lignin from biomass: only downscale production in the range of 2.5-5 kg/h of lignin
-
Design phase ongoing; PILLAR II unit ready for start-up Summer 2022 (with reservation)
Accessories
- A flash vessel is included to evaporate the solvent after reaction.
- Feeding system (hopper) to supply lignin powder and wood chips to the reactor.
Registration Parameters
Temperature, pressure and circulation flow, pH
Name of the device
Catalytic Reactor. LIGNOVALUE
Description
Catalytic conversion (fixed bed) of lignin
Applications
Depolymerisation of lignin via catalytic conversion of lignocellulosic/lignin in solvents with a heterogeneous metal catalyst under reductive (hydrogen) atmosphere.
Features
-
Material of construction: Stainless steel; Hastelloy C material for high pressure/high temperature equipment/instruments
-
Content: 4 fixed bed reactors, 0.1 m³ each; Reactors can be applied in series or in parallel
-
Capacity: 1-10 kg/h of lignin oil (without solvent); For the downscale scenario (1 kg/h), only 1 reactor will be used
Accessories
-
A flash vessel is included to tune the lignin-to-solvent ratio in the final product lignin oil.
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Recirculation line over the reactors is included to increase residence time in the reactors if needed.
Registration Parameters
Temperature, pressure and circulation flow, pH
