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.

Flowrence® products specifications

Reactor Section

Easy and quick reactor exchange system. Possibility to use quartz reactors at high pressure.

1 block of 4 reactors

HT = High Temperature max. 800°C nominal, limited to 925°C (<0.5°C reactor to reactor deviation)

4 blocks of 4 reactors

HT  or MT = Medium Temperature max. 525°C (<0.5°C block-to-block deviation)

16 reactors with iRTC

individual Reactor Temperature Control
max. 550°C (<0.5°C reactor-to-reactor)

4 reactors with iRTC

individual Reactor Temperature Control
max. 550°C (<0.5°C reactor-to-reactor)

Temperature Ranges (°C)

100 – 800°C
up 925°C (Option)

50 – 525°C
100 – 800°C
up 925°C (Option)

50 – 550°C

50 – 550°C

Reactor Types

L= Length
OD= Outer Diameter
ID= Inner Diameter
SS= Stainless Steel (< 550⁰C)
Qz= Quartz (< 925⁰C)

L 300 mm 561 mm
OD 3 mm 6 mm
ID SS 2 / 2.6 mm 2 / 3 / 4 / 5 mm
ID Qz 2 mm 2 / 4 mm
300 mm 561 mm 561 mm
3 mm 3 mm 6 mm
2 / 2.6 mm 2 / 2.6 mm 2 / 3 / 4 / 5 mm
2 mm 2 mm 2 / 4 mm
561 mm
3 mm
2 / 2.6 mm
2 mm
561 mm
3 mm
2 / 2.6 mm
2 mm

Maximum Catalyst Bed Length

(isothermal zone tolerance ± 1°C)
Note: isothermal length is dependent on the temperature range

300 / 3 HT 561 / 6 HT
>120 mm @ 450°C >200 mm @ 500°C
>90 mm @ 800°C >150 mm @ 800°C
>140 mm @ 925°C
300 / 3 HT 561 / 3 MT 561 / 6 HT
>120 mm @ 450°C >310 mm @ 450°C >200 mm @ 500°C
>90 mm @ 800°C >150 mm @ 800°C
>140 mm @ 925°C
561 / 3 MT iRTC
250°C ±0.5°C 41cm (4reactors)
350°C±0.5°C 38cm (4reactors)
550°C±0.5°C 28cm (4reactors)
3 reactors at 550°C, 1 reactor 350°C:
550°C=27cm 350°C=41cm ±0.5°C
561 / 3 MT iRTC
250°C ±0.5°C 41cm (4reactors)
350°C±0.5°C 38cm (4reactors)
550°C±0.5°C 28cm (4reactors)
3 reactors at 550°C, 1 reactor 350°C:
550°C=27cm 350°C=41cm ±0.5°C

Catalyst Volume (mL)

(isothermal zone)

0.2 - 0.6 mL 0.4 - 2.0 mL
0.2 - 0.6 mL 0.4 - 1.0 mL 0.4 - 2.0 mL
0.4 - 1.0 mL
0.4 - 1.0 mL

Pressure Ranges (barg)

2 – 80 barg
0.5 – 180 barg (option)

2 – 100 barg
0.5 – 180 barg

2 – 80 barg
0.5 – 180 barg

2 – 20 barg
2 – 50 barg (option)

Reactor Pressure Control

Advanced control RSD ±0.1 barg at reference conditions (gas phase only and 20 barg). For trickle flow Advanced control RSD ±0.5barg.

Standard (±0.5 barg)
Advanced (±0.1 barg) (option)

Standard (±0.5 barg)
Advanced (±0.1 barg) (option)

Advanced (±0.1 barg)

Advanced (±0.1 barg)

Gas Feed Lines

(#Gas Feeds)

Up to 6 + Diluent gas

He, Ar, N2, H2, CH4, CO2, C2H4, C2H6, O2/Inert (≤5%), CO, Other gases

Up to 7 + Diluent gas

He, Ar, N2, H2, CH4, CO2, C2H4, C2H6, O2/Inert (≤5%), CO, Other gases

Up to 7 + Diluent gas

He, Ar, N2, H2, CH4, CO2, C2H4, C2H6, O2/Inert (≤5%), CO, Other gases

Up to 6 + Diluent gas

He, Ar, N2, H2, CH4, CO2, C2H4, C2H6, O2/Inert (≤5%), CO, Other gases

Online Analysis

Full integration GC, MS , GC/MS with data visualisation (option)

Full integration GC, MS , GC/MS with data visualisation

Full integration GC, MS , GC/MS with data visualisation

Full integration GC, MS , GC/MS with data visualisation

Liquid Feed

 Split feeding 8 + 8 reators (option)

Pump-Coriolis dosing system
(ambient, cooled)

Pump-Coriolis dosing system
(ambient, cooled, heated 80°C)

Pump-Coriolis dosing system
(ambient, cooled, heated 80°C)

Pump-Coriolis dosing system
(ambient, cooled, heated 80°C)

Liquid Distribution

Microfluidic Distribution
(4-channel glass-chip)

Microfluidics Distribution
(4x4-channel glass-chip)
(16-channel glass-chip)
Active Liquid Distribution (option)
(with automatic isolation valves)

Active Liquid Distribution
(with automatic isolation valves)

Microfluidic Distribution
(4-channel glass-chip)

Liquid Sampling

(G/L Separation)

Parallel liquid sampling (4 x 20ml vials) with sequential on-line gas phase sampling (option)

Automated liquid sampling (4 rows x 16 vials x 8ml) with sequential on-line gas phase sampling (option)

Automated liquid sampling (4 rows x 16 vials x 8ml) with sequential on-line gas phase sampling (option)

Parallel liquid sampling (4 x 20ml vials) with sequential on-line gas phase sampling (option)

Reactors Effluent Handling

(Off-line Analysis Connection)

Full heated circuit up to 180°C with sequential on-line full gas phase sampling (option)

Full heated circuit up to 200°C with sequential on-line full gas phase sampling

Full heated circuit up to 200°C with sequential on-line full gas phase sampling

Full heated circuit up to 200°C with sequential on-line full gas phase sampling

Offline Analysis

Integrated Workflow: SimDist, total S/N, liquid density, balance, label printer, barcode (option)

Integrated Workflow: SimDist, total S/N, liquid density, balance, label printer, barcode

Integrated Workflow: SimDist, total S/N, liquid density, balance, label printer, barcode

Integrated Workflow: SimDist, total S/N, liquid density, balance, label printer, barcode

Waste Handling

Ambient temperature
Heated wax trapping (option)

Ambient temperature / Cooled containers / Heated compartment (wax trapping, heavies)

Ambient temperature / Cooled containers / Heated compartment (wax trapping, heavies)

Ambient temperature / Cooled containers / Heated compartment (wax trapping, heavies)

Safety

Gas sensors and control box (CO, LEL, VOC)

Gas sensors and control box (CO, LEL, VOC)

Gas sensors and control box (CO, LEL, VOC)

Gas sensors and control box (CO, LEL, VOC)

Flowrence® Software

Flowrence® recipe builder, control & database builder

Flowrence® recipe builder, control & database builder

Flowrence® recipe builder, control & database builder

Flowrence® recipe builder, control & database builder

Microfluidics modular gas distribution

Unrivalled accuracy in gas distribution with patented glass-chips for 4 and 16 reactors, with a guaranteed flow distribution of 0.5% RSD. Quick exchange of glass-chips for different operating conditions. Flexibility to cover a wide range of applications.

TinyPressure glass-chip holder with integrated pressure measurement

Compact modular design for gas and liquid distribution. No high-temperature pressure sensors required. Quick exchange of the microfluidic glass-chips, without the need for time-consuming leak testing.

Tube-in-tube reactor technology with effluent dilution

Unique tube-in-tube design with easy and rapid exchange of the reactor tubes (within minutes!). No need for any connections. Use of inert diluent gas (outside of reactor) to maintain the pressure prevents dead volumes and back flow. Possibility to use quartz reactors at high pressure applications.

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. Eliminates the use of high pressure valves.

Reactor Pressure Control (RPC)

The most accurate and stable pressure regulator for a 16-parallel reactors with just ±0.1bar RSD. The RPC uses microfluidics technology to regulate the pressure of each reactor, maintaining equal distribution of the inlet flow over the 16 reactors.

Auto-calibrating liquid feed distribution, measurement, and control

Distribution of difficult feedstocks e.g., VGO, HVGO, DAO. Liquid distribution 0.2% RSD, making it the most accurate liquid distribution device on the market. Option to selectively isolate each reactor.

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 avoiding maldistribution, eliminating channeling and incomplete wetting.

EasyLoad®

Unique reactor closing system with no connections. Rapid reactor replacement minimizing delays, improving uptime and reliability. Stable evaporation by liquid injection into reactor.

Contact us

We are here to help you

 

 

 

 

 

 

 

 

Avantium Headquarters

+31 (0)20 586 8080

Zekeringstraat 29
1014 BV Amsterdam
The Netherlands

Contact us