Special Condition Syntheses
The laboratory for special condition syntheses is equipped with a series of Anton Parr reactors permitting running processes under high pressure and in high temperatures. They offer a possibility to perform processes in solvents in supercritical state. The instrument unique in the country is a laboratory fluidal reactor permitting investigation and optimisation of processes in the fluid phase, under high pressure and in high temperatures, with the use of nitrogen, carbon oxide or hydrogen. The laboratory also has a glove box in which up to four persons can work simultaneously in controlled atmosphere.
Glovebox AMB-200 MOD (1800/1200) NAC, M. Braun Intergas-System
MB-200B modular platform is designed with the capability of adding further box tops onto the original workstations. MB-200B can also connect directly to your choice of any standard MBRAUN gas purification system. Like pieces of a puzzle the MB-200B glovebox system can be “pieced together” to form the solution for countless applications and system configurations. Systems incorporating MB-200B modules typically feature additional equipment ranging from laboratory instruments and deposition systems to fully automated processing lines.
Fluid Bed Reactor System
Three reactant feed lines are included. Each has a shut-off valve, filter, bypass valve, electronic mass flow controller (MFC), and a reverse-flow check valve. The MFC’s are calibrated for 0 – 20000 sccm flow of H2, CO, and N2, respectively. Reactor is made of T316SS, is rated for use to 500 psi at 350°C and has a 1” ID and 36” inner length that expands to 2.5” ID in the uppermost 2” segment. The software provides for control and monitoring of three temperature zones, pressure, and the gas flow rates as well as displaying, monitoring, and data logging of all gas flows, temperatures, and pressure readings.
High-pressure and high temperature reactor
High-pressure and high temperature reactor made of HC Alloy C-276; can work under pressures up to 345 bar and in temperatures up to 500°C, its capacity is 1000 mL and it is equipped with a stirrer and automatic control unit.
Reaction setup for processes in supercritical CO2
It can work with pressures up to 350 bar and temperatures up to 350°C, its capacity is 100 mL and it is fully automated. The setup permits running of flowthrough and cyclic processes. Thanks to the use of sapphire windows the processes can be controlled by spectroscopic methods. The setup includes a pump for carbon dioxide and a pump for dosing reagents under high pressure.
Our process development and scale up laboratories offers You an access to the most advanced and precise equipment allowing for full insight to the wide range of chemical processes by measuring heat profiles, enthalpies, chemical conversion and heat transfer under process-like conditions and their optimization. Possessed automated lab reactors (Mettler Toledo EasyMax and OptiMax synthesis workstations) provide a simple platform for organic synthesis in chemical and process development that ensure high level of measurements repeatability and accuracy in laboratory scale (from 25 mL to 1 L). Our synthesis workstations can be equipped with heat flow calorimetry (HFCal) and in-situ FT-IR (ReactIR 15) modules to offer simultaneous benefits of an easy-to-work-with synthesis workstation, reaction calorimeter collecting heat data for scale-up and safety studies and IR data for kinetic analysis.
The RC1e reaction calorimeter provides information, such as heat profiles, chemical conversion, and heat transfer, under process-like conditions using either heat flow or real-time calorimetry supported by iC Safety which converts the information into safety relevant information for process carried out in much bigger scale (up to 15 L).
Data obtained from mentioned above reactors can be easily verified in scale up laboratory (technology hall) where pilot plant Normag reactors [33] and rectification unit are placed.
The laboratory offers analytical services in the scope of FT-IR and UV-Vis spectroscopy and particle size analysis. FT-IR spectrometer (Nicolet iS 50) equipped with built-in diamond ATR module, DRIFT module, automated beamsplitter exchanger with two beamsplitters and DLaTGS detector enable measurements of solid and liquid samples in the range of 12 000 – 350 cm-1 with a 0.09 cm-1 resolution. The analysis is supported by advanced software options and the library containing over 10000 spectra. The laboratory has a portable in-situ FT-IR spectrometer (Mettler Toledo ReactIR 15) of spectral range 4000 – 650 cm-1 equipped with 1.5 m DiComp ATR fibre probe and MCT detector for in-situ measurements.
For samples analysis in a UV-Vis range (190-1100 nm) a Nicolet Evolution 220 PC can be used. Thiscompact, simple in use, double-beam geometry with 1 nm spectral bandwidth, spectrophotometer offers a possibility of precise measurements in 4 basic modes: spectral analysis, fixed wavelength analysis and quantum or kinetic analysis supported by advanced INSIGHT software options.
Dispersive properties of the materials can be characterised by laser diffraction technique with Mastersizer 3000 (Malvern Instruments Ltd.). The laser diffraction method is based on two physical phenomena: diffraction and interference of light waves. The results are obtained as a relation between the volume (in %) and the diameter of particles, in fact of a fraction of particles. The instrument measures particles of the sizes from 0.2 to 2000 μm. Particle diameters in the range of 0.6 – 10000 nm can be analyzed employing the method of dynamic light scattering (DLS) with NanoPlus-3 (Micromeritics Instruments Co.). Dynamic light scattering is a non-invasive, well-established technique for measuring the size and size distribution of molecules and particles, with the latest technology even those of sizes lower than 1 nm. Typical applications of DLS are the characterisation of particles dispersed or dissolved in a liquid. It is also possible to measure electrophoretic mobility (zeta potential) in the range from –200 to 200 mV.
