Application of NESSI to Modeling and Product /Process Development

Transcription

1 Application of NESSI to Modeling and Product /Process Development Michelle J. Cohn uop LLC 2004 UOP LLC. All Rights Reserved.

2 UOP LLC Who We Are Global company with 11 manufacturing sites and offices in 25 countries More than 3,600 highly trained employees 90 years of innovative solutions for the hydrocarbon processing industry UOP s customers are located in more than 200 countries. World s largest supplier of molecular sieve adsorbents

3 What We Do Develop technology that provides solutions to problems License, design, engineer, and service process technology Develop and manufacture catalysts, molecular sieves, adsorbents, and specialized equipment Transfer technology to customers who achieve high yield of high quality products

4 UOP Research & Development Resources More than 185 pilot plants (> 60 operating each day) More than 20,000 pilot plant-days per year Combinatorial chemistry capabilities 300 million data points generated per day 350,000 laboratory analyses performed per year Modeling capabilities include: physical, computational fluid dynamics, kinetic, and process simulation (dynamic and steady-state) state) Average annual R&D spending: 8-10% 8 of sales

5 Process Analytical Technology (PAT) PAT in Heterogeneous Catalysis Product and Process Controll Continuous composition diversity Diversity in phase, microstructure, particle characteristics Diversity in process conditions for all unit operations Applied to synthesis, preparation, testing and characterization Requires detailed material characterization design, monitoring, control and modeling of materials and process conditions

6 Desired Outcomes from PAT Increased manufacturing and production efficiency Increased product quality Reduced product variability Increased innovation Real time lot certification

7 Enablers for PAT Model Building T Time Reactor Sensor Data Analysis Feedback Control Online Process Analytics Sampling NIR FTIR DLS RAMAN Ultrasound LAMIMS Micro-calorimetry calorimetry FTIR V P A NESSI T NESSI P.S.

8 High Throughput Characterization Tools HT XRF Element Analysis HT Raman Active Site, Phase ID HT XRD Structural, Phase ID HT SEM Morphology, Particle Size Goals Full spectrum of tools Ultra-fast collection times 100 s s to 1000 s s samples /day Characterization is Key to Success From Data Structure/Function Models = Knowledge IR Thermography TPD, Adsorption HT Adsorption Surface Area, Pore Size Distribution LAMIMS Reactivity

9 High Throughput Screening LAMIMS Laser Activated Membrane Introduction Mass Spectrometry Micro reactivity test Closed environment (realistic catalyst exposure) Very broad temperature application Full QMS product analysis Real world catalysts

10 The LAMIMS Screening System System Components LAMIMS reactant delivery system A 25 watt CO 2 barcode writing laser LAMIMS reactor Quadrupole mass spectrometer (QMS)

11 LAMIMS System Measure of metal sites CH 3 CH 3 Metal + MCH Toluene Fenix Laser Marker Laser Beam Gas out To QMS 3 H 2 Reactant Gas Inlet Porous inlet barrier Laser heats samples Large array of samples in reactor Mass spec monitors product stream Dehydrogenation test for metal activity Goal: 1000 samples tested per day

12 Reactor Sample Inlet Heat Cartridge Well Catalyst Spot Al toothed flow distributor ZnSe window Silicone Rubber Membrane Tripod Base To QMA

13 Data from Reactor System 45 samples

14 Applying NeSSI Technology Honeywell sensors Parker Hannifin Intraflow substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration, control, data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic, control, and data collection capabilities Remote monitoring and control via standard internet tools Fast and easy configuration using LabView

15 Overview of System Safety Enclosure Nitrogen MFC Laser Vent Cell Argon MFC Hydrogen MFC Neslab

16 NC LAMIMS FlowSystem HT-603 vent vent cell PSI PSI MFC-20010( ccm) vent vent PSI Laser MS NC KV PI-2008 PCV- PSV KV-4005 KV-4001 VP-4007 CK-4006 PSV-4011 LA-4015 PCV PSI PI-1008 vent Set at 250 PSI 0-250PSI MFC ( ccm) NC 5011 HT-4014 CON Set at 250 PSI PI CK-1013 KV-1014 CK-4018 Set at 7 PSIG Set at 250 PSI PI CK-4017 Vent Vent Argon gas cylinder House Nitrogen gas PUR PSI PI-7010 House Hydrogen gas PSI vent PSI MFC ( ccm) HV-3005 NC KV PI PI CK-3013 V-5002 PSV CON- PSV- PCV- AL- HV PCV- PSV- PCV- ISC- TE HV PSI PSI PI-2003 CON- CON- PCV- HV PSI PI PSI To TSR system Set at 250 PSI PSV PSI 1002 PI-1003 PUR-2004 Set at 250 PSI refil vessell To TSR system Optional Neslab Safety enclosure KV-4008 NC NC KV-2014 KV-3014 PI-2011 CK PCV- HV-1005 KV-1006 HV-1001 PCV- Corridor area

17 Automated System Components # Description Device Net Flow controllers Back Pressure Regulators 4 port two position valves 3 port two position valve 24VDC bellows sealed valves Pressure Indicators Pressure reducing regulators

18 LABVIEW SCREEN

19 LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI Mass Spectrometer installed Laser installed NESSI gas manifold installed Lab View Automation software completed Safety review completed Resources Elapsed time Personnel time Manifold cost W/NeSSI 4months 2months +10% Typical 6 months 4months baseline

20 Installation Went Very Well List of Minor Issues The check valves were ordered with a 1psi cracking pressure. However, the check valves were delivered with a much higher cracking pressure. This was corrected the following day by ordering new springs for the check valves. All the block valves and the mass flow controller for the nitrogen line were specified to be normally opened. They all were delivered normally closed. A simple nitrogen line (needle valve and block valve) added to correct this safety issue All the connections to the Neslab four-way valve (KV-4001) and to the vent four-way valve (KV-4005) were incorrectly installed. We had to take apart most of the NeSSI system to correct this. Original design to put all electronics modules (labview( field point modules, power supply, etc.) inside an enclosure. The NeSSI system arrived without such an enclosure, and all the electronics parts were exposed to the outside, including the 110V cables. The Brooks mass flow controllers failed to communicate (DeviceNet communication) correctly with the automation software. Falaah resolved this issue with Brooks. Overall the NeSSI system performs well

21 Desired Outcomes from PAT and NESSI Increased manufacturing and process efficiency Increased quality Reduced variability Increased innovation Real time certification

22 PAT Summary Technology and industry needs are converging for PAT and NESSI In-situ measurements Sensor integration Computational capacity and methods Demonstrated success in refining and petrochemicals Opportunities for cross-industry fertilization

23 Summary Innovation and growth driven by enabler toolbox Opportunities PAT and NESSI Seek enhanced understanding of process variables and relationship to performance Enabling technologies cut across industries PAT NESSI Advanced Characterization Informatics Enabling Step Changes In Technology

24 Acknowledgments Eugene Smotkin, IIT, UPR-RP RP Renxuan Liu, NuVant Systems Inc., currently GTI Yongtae Kim, IIT Doug Galloway, UOP Richard R. Willis, UOP Falaah Falih, UOP Robert J. Allen, UOP Michael J. McCall, UOP Jose A. Rodriguez, UPR-RP RP Amit Nayar,, IIT John Mosher, Honeywell Robert Nickels, Honeywell Steve Doe, Parker Hannifin A portion of this work was performed under the support of the U.S. Department of Commerce, National Institute of Standards and Technology, Advanced Technology Program, Cooperative Agreement 70NANB9H3035.