Accelerated testing with Advanced analytics

In the Flowrence platform, reactor products are kept in the gas phase as much as possible in order to be able to directly feed the complete sample stream into online GC’s. This allows for complete speciation as well as the best achievable determination of the mass balance. However, this approach calls for advanced GC methods to manage the analysis time to meet the required cycle times of the experiment.

Analysing all the components and shortening the cycle time, are two factors that need to be balanced with each application. This differs for each case, depending on whether more data points or more detailed component information is important. This choice is often a matter of which stage of R&D your application is tested for. Early stage catalyst scouting has less need for detail than the stage of process optimisation in which more complete product separation is required.

Another advantage of online analyses is to be able to analyse the non-condensable gasses when liquid samples are collected. This gives us the opportunity to achieve an even better mass balance, and to include an internal standard. The speed increase for the higher boiling components is often gained by making use of a multi-column approach, where the sample is pre-separated on the first column. Part of the sample continues onto a second column and the other part on a third column, where we can make use of the difference in the coatings/packings of the columns, to achieve the best resolution in the shortest amount of time.

 

Below there are some examples of different applications where short cycle times were established in different ways. Depending on the number of components, the number of reactors and the required cycle time, the best solution involved either multiple channels per sample line or multiple GC’s or even a combination of both.

In the Catalysis Insider issue of July 2017, the configuration and Design-of-Experiments of the IsoRON application was described. As an example of advanced analytics, we now focus on the online analytical method of RON. The RON analysis is one where you need to separate almost all paraffins, olefins, iso’s, naphthenes and aromatics from C1 to C12, to be able to calculate the Research Octane Number. The conventional way would be 2.5 hours offline analysis. This has already been improved by UOP in their ASTM method with a cycle time of 55 minutes, but we needed an even faster method and with more detail on the aromatics. Faster to be able to create a feedback loop to run reactions in an iso-RON controlled setup and more detail on the separation of xylenes was of specific interest for several customers. By optimizing the columns we ended up with a half an hour method, giving the fast feedback needed in our iso-RON control loop.

As shown below, the 1-column PONA on the left and our improved 2-column method on the right, by making use of different pre-column and analytical columns we can separate the aromatics from the rest and get a better separation between the different C8-aromatics, especially the difficult pair of meta and para-Xylene.

In conclusion, advanced GC set-up and methodology can significantly increase the speed of analysis, while providing desired separation of components. In some cases this can be crucial to enabling the application of high-throughput testing to specific catalytic processes. Please feel free to contact us to explore the possibilities to accelerate your analytics.

Single-Pellet-String-Reactors (SPSR)

No dead-zones, no bed packing & distribution effects. The catalyst packing is straightforward and does not require special procedures. A single string of catalyst particles is loaded in the reactors with an internal diameter (ID) that closely matches the particle average diameter. This applies to single catalyst systems, as well as stacked-bed systems. The use of a narrow reactor avoids any maldistribution of gas and liquid over the catalyst bed, thereby eliminating catalyst-bed channeling and incomplete wetting of the catalyst.

The most accurate and stable pressure regulator for 16-parallel reactors

The most accurate and stable pressure regulator for a multi-parallel reactors with just ±0.1bar RSD at reference conditions. The Reactor Pressure Controller (RPC) uses microfluidics technology to individually regulate the back-pressure of each reactor. By measuring the inlet pressure of each reactor, the RPC maintains a constant inlet pressure by regulating the backpressure. As a result, the distribution of the inlet flows over the 16 reactors is unaffected and a low reactor-to-reactor flow variability is achieved.

Reactor pressure control is not only important to ensure accurate pressure control, but also to help maintaining equal distribution of the inlet flow over the 16 reactors.

Automated liquid sampling system

Programmable, fully automated liquid product sampling robot for 24/7 hands-off operation. Robot equipped with a compact manifold aiming at depressurizing the effluent immediately after each reactor to atmospheric pressure. Reactor effluent is depressurized by a miniaturized (low volume) parallel dome regulator, allowing a stable control of gas or gas/liquid product streams. This eliminates the use of valves at high pressure (such as multi-position valves), which are prone to leakage.

Gas liquid separation is sone directly by collecting the liquid products in sample vials and directing the gas products to the online gas analyzer. This approach minimizes required flushing times in the downstream section of the reactor eliminating the need for high pressure gas-liquid separators, level sensors, and drain valves.

EasyLoad® reactor closing system

Unique reactor closing system, no connections required. With a rapid reactor replacement minimizing delays, improving uptime and reliability. Sealing of up to 16 reactors by simply closing the ‘top-box’ in a single action. No leak testing required!

Stable evaporation by liquid injection into reactor

The direct injection of liquid into the top of the reactor and the consecutive conditioning zone allows feeding of broad range of liquids and concentrations. Various types of liquids, both aqueous and oil phase are successfully evaporated and fed to the reactors.

Tube-in-tube reactor technology with effluent dilution

This unique tube-in-tube feature allows an easy and rapid exchange of the reactor tubes (within minutes!) with a single o-ring at the top of the reactor without the need for any connections. The use of an inert diluent gas (outside of reactor) to maintain the pressure stops undesirable reactions immediately after the catalyst bed while serving as a carrier gas to the GC, facilitating the analysis of high boiling point components, preventing dead volumes and back flow, and reducing the time required to transfer gas and liquid effluent products to the analytical instruments.

The tube-in-tube design enables the use of quartz reactors at high pressure applications.

Compact TinyPressure module glass-chip holder with integrated pressure measurement

Holds the microfluidic glass-chips for gas distribution and measures inlet (and outlet) pressure of the 16 parallel reactors at ambient temperature, allowing online measurement of catalyst bed pressure drop.

No high-temperature pressure sensors required. Pressure range of 10 – 200 bar (high pressure) or 0.5 – 10 bar (low pressure).

The modular design enables easy calibration and quick exchange of the microfluidic glass-chip, without the need for time-consuming leak testing.

Microfluidics modular gas distribution

Unrivalled accuracy in gas distribution with patented glass-chips for 4 and 16 reactors, tested with a guaranteed flow distribution of 0.5% RSD channel-to-channel variability. Quick exchange for different operating conditions, offering the unique flexibility to cover a wide range of applications using the same reactor system.

Auto-calibrating liquid feed distribution, measurement, and control

The most accurate liquid distribution for high throughput systems with real-time liquid flow measurement and control for 16-parallel reactors. Auto-calibrating function enabled by a single flow sensor guarantees that all 16 reactors are continuously operated at the desired LHSV, all the time. Innovative design based on our microfluidic glass-chips with integrated temperature-control. The system continuously regulates the liquid distribution to all 16 reactors, and together with our Reactor Pressure Control technology, eliminates the impacts of pressure variations in the flow distribution.

Proven technology with difficult feedstocks with high viscosity, such as VGO, HVGO and DAO: no blockage and or breakage observed. Different glass-chips available for different viscosities.

Liquid distribution errors below 0.2% RSD, making it the most accurate parallel liquid flow distribution device on the market.

Option to selectively isolate the liquid flow to any of the 16-parallel reactors.

 

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+31 (0)20 586 8080

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