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Nouryon is exploringreactive distillationUlf Schröder, Stijn Oudenhoven, Gerrald Bargeman, Antoon ten KateNouryon – ECCD
EFCE WP Fluid SeparationsGöteborg SE, 19 June 2019
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EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation
Simultaneous removal of vapor products from a boiling, reacting mixture
Reactive Distillationtechnology in short
Traditional process
Reaction A + B ↔ C + D
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Reactive DistillationD
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Source:Bob Huss, Reactive Distillation:What, why, and how?East Tennessee AICHE Seminar Program (17 November 2015)
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EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation
Simultaneous removal of vapor products from a boiling, reacting mixture
Technological benefits:• Beat low equilibrium constants• Enhance overall rates• Improve selectivity & reduce byproducts• Avoid/eliminate difficult separations• React away impurities• Reduce/eliminate solvents• Energy reduction potential
Reactive Distillationtechnology in short + benefits
Reaction A + B ↔ C + D
Reactive DistillationD
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EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation
Reactive Distillationmethylacetate production
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Sources:Bob Huss, Reactive Distillation:What, why, and how?East Tennessee AICHE Seminar Program (17 November 2015)James Bielenberg, Michelle Bryner, Realize the Potential of Process Intensification,CEP (March, 2018)
(Quote: prof. Krishna,University of Amsterdam)
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
route scouting process development engineering CCSconstruction, commissioning, start-up
EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation 5
Structured approach for reactive distillation
Validation
conceptual designmodel & parameters
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experiment
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Complexity in reactive distillationAn artist impression
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Literature & patent reviewBibliography (1970 - Mid 2018)
Sources:Sascha Kersten, University of Twente, Private Communications, 2018
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• RD methods typically developed from SepTech perspective:à Strong need for ReactorTech perspective.
• Process design software appears (far) less developed for RD than it is for distillation,which quite easily can lead to annoying & significant errors (a number of examples in lit.!)à Need for more advanced tools for RD in simulation software
• Most (engineering) literature is based on simulations only (>95%)à Need for experimental validation
• Focus (mainly) on RD column as such (or aspects thereof); less on integral processà Need focus on (integral) process or at least RD section (RD unit ± 1 unit operation)
• No clear design procedureà Need for clear design procedure & guideline, especially for relatively slow reactions.
Literature & patent reviewObservations
Cooperation with• Universities (UCL, prof E. Sorensen; Univ Twente, prof S. Kersten)• Software vendors (AspenTech)• Hardware suppliers (Montz)
Design Guidelines
EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation 9
Collaboration on Reactive Distillationpurpose
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
SepTechperspective
ReactorTechperspective
MitigationstrategiesRD test unitsShort-cut
methods
Cooperation with• Universities (UCL, prof E. Sorensen; Univ Twente, prof S. Kersten)• Software vendors (AspenTech)• Hardware suppliers (Montz)
Design Guidelines
EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation 10
Collaboration on Reactive Distillationpurpose
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
SepTechperspective
ReactorTechperspective
MitigationstrategiesRD test unitsShort-cut
methods
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90%95%99%99.9%
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Mapping of applicability window
Study*) initiated on applicability window ofreactive distillation. Results showed:• there is a window of feasible RD
configurations that provide in-specproduct streams
• the feasibility window is characterized byminimum reflux ratio (RRmin) as well asminimum number of stages (Nmin),(similar to that of distillation)
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Keq=0.01Keq=0.1Keq=0.2Keq=1Keq=10
*) Novel method for mapping the applicability of reactive distillationRahma Muthia et alChemical Engineering and Processing - Process IntensificationVolume 128, June 2018, Pages 263-275
Cooperation with• Universities (UCL, prof E. Sorensen; Univ Twente, prof S. Kersten)• Software vendors (AspenTech)• Hardware suppliers (Montz)
Design Guidelines
EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation 12
Collaboration on Reactive Distillationpurpose
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
SepTechperspective
ReactorTechperspective
MitigationstrategiesRD test unitsShort-cut
methods
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Some ReactorTech PerspectivesThe reactor engineering point of view
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Reactive distillation is not limited to stoichiometric feed and distillation
Some Integral Process Perspectives
Conventional distillation
Input:• Flow• XA XB
• Pà temp
Spec:• Flow• XA XB Input:
• Flow• XA
Spec:• Flow• XC
Input:• Flow• XB
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Input:• Flow• XA
Spec:• Flow• XC
Input:• Flow• XB
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Spec:• Flow• XD
Reactive distillation Excess reactant operationà increased reaction rateà Suppression of undesired side reactionsà enhanced operability & controllability
Cooperation with• Universities (UCL, prof E. Sorensen; Univ Twente, prof S. Kersten)• Software vendors (AspenTech)• Hardware suppliers (Montz)
Design Guidelines
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Collaboration on Reactive Distillationpurpose
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
SepTechperspective
ReactorTechperspective
MitigationstrategiesRD test unitsShort-cut
methods
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Purpose:• validate RD designApplications:• Various chemistries (alkaline, acid)• Slow, fast & instantaneous reactionsFeatures:• Minimum residence time in reboiler• Dedicated column wall temperature control to
compensate for heat losses• Flexible feed points• Multiple sampling and temperature points• Vacuum, atmospheric to 6-10 bara• MoC: glass, glass-lined and SS316• Atex
RD test unitsimpression
Cooperation with• Universities (UCL, prof E. Sorensen; Univ Twente, prof S. Kersten)• Software vendors (AspenTech)• Hardware suppliers (Montz)
Design Guidelines
EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation 17
Collaboration on Reactive Distillationpurpose
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
SepTechperspective
ReactorTechperspective
MitigationstrategiesRD test unitsShort-cut
methods
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Considerations• Experiments have errors in process parameters and analysis.• Models are simplified representation of reality.• Strict design of RD column (Overdesign can lead to higher OPEX)• Pilot testing expensive and time consuming
Need for guidelines to mitigate uncertainties, thereby increasing plant acceptance andspeeding up design and implementation process.
Mitigation and process control
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Design mitigation required when solely control cannot mitigate process deviation.
Mitigation and process controlInterconnection between both topics
Cooperation with• Universities (UCL, prof E. Sorensen; Univ Twente, prof S. Kersten)• Software vendors (AspenTech)• Hardware suppliers (Montz)
Design Guidelines
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Collaboration on Reactive Distillationpurpose
route scouting engineering CCSprocess developmentconstruction, commissioning, start-up
SepTechperspective
ReactorTechperspective
MitigationstrategiesRD test unitsShort-cut
methods
EFCE WP FluidSep 190619 | Nouryon is exploring reactive distillation 21
• Delivering world-class support indevelopment of reactive distillation process:o Structured process development approach§ for fast and slow reactions§ from ideation until pilot scale§ kinetics, VLE, conceptual design, validation§ experimental + modeling, incl physprops
o RD columns for validation§ for acid, neutral and alkaline systems (glass-lined; SS316)§ capacity: ~ 0.5 - 5 kg/h throughput
o Close connection with key suppliers§ RD column suppliers§ Simulation software
Visit us in Deventer or our website
ECCD Process Technologyreactive distillation
Nouryon ECCD Deventer 22
Who? Over 80 skilled, highly educated and experienced scientistsWhat? Process & product technology, analytical scienceWhere? Deventer, NLWith? State of the art laboratories and equipment, including ATEXWhat else?
• Broad knowledge of chemical products and processes• Fast response• Collaboration with universities, knowledge institutes and Nouryon RD&I groups• REACH notification, GLP accreditation
Expert Capability Center Deventer
Your challenges:• Developing new and improved products• Developing and implementing new and optimized technologies
and processes
Our supporting role:• Multi-disciplinary approach in industrial R&D perspective• Using in/online analytical techniques to control processes• Developing models for improved process control• Performing dedicated trials at lab, pilot or plant scale• Analyzing in complex matrices• Failure analysis
Expert Capability Center DeventerSolving your challenges using our expertise
Nouryon ECCD Deventer 23
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University Twente, NL:Prof S. Kersten;V. Kroeze, PhD student; L. Noll, PhD student;F. Kooijman, MSc student; K. Zijp, MSc student
University College London, UK:Prof E. Sorensen; A. Tsatse, PhD student
University Manchester, UK:Prof T. Kiss, R. Muthia, PhD student
AspenTech, USA: Dr D. TremblayMontz, DE: Dr R. Schulz; Dr M. Krapoth
Acknowledgement
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ECCD PT Lead scientist Antoon ten Kateantoon.tenkate@nouryon.com+31 (0)6 2933 6596
ECCD PT Leader Gerrald Bargemangerrald.bargeman@nouryon.com+31 (0)6 2306 4091
Visiting address Zutphenseweg 107418 AJ DeventerThe Netherlands
Website https://www.nouryon.com/company/innovation/eccd
ECCD Process Technologycontact information