TRENDS AND NEEDS FOR ON LINE MICRO ANALYSIS FOR R&D INNOVAL and AXEL'ONE Projects from AXELERA

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1 Renewable energies Eco-friendly production Innovative transport Eco-efficient processes Sustainable resources TRENDS AND NEEDS FOR ON LINE MICRO ANALYSIS FOR R&D INNOVAL and AXEL'ONE Projects from AXELERA Dr. Franck BACO-ANTONIALI IFP Energies Nouvelles BP3, Solaize, FRANCE

2 Agenda Introduction and problematic Trends and needs for R&D on line micro analysis INNOVAL Project Technologic platform AXEL'ONE : An collaborative platform Conclusions and outlooks 2

3 L analyse des procédés: un enjeu pour l'industrie chimique Objective ANALYSIS = PROCESS CONDITIONS CONTROLS PRODUCTION Safety of employees and neighborhood R&D Process intensification Environment protection (pollution) Products Quality Reduction of costs 3

4 The future for industrial on line analysis : in situ analysis Sampling loop > Quality of the analysis Analysis in the "heart of process" > Sampling safety > Wastes management > Installation cost ($ ) >Energy consuming systems 4

5 Evolution of needs in term of analyzers in R&D Process Intensification Pilots m Pilots HTE Reducing of sample volume "Classical" analyzers m Analyzers mcaptors 5

6 Needs for R&D and Process Intensification Employ more compact analyzers to be able to analyze in the heart of process "bring the analyzer to the sample" Reduce time of experimentation - Increase the number of tests in the same time we need Smart analyzers to follow process stabilization, product quality, process control,... Excellent repeatability, accurate systems, good accordance with standard methods,... 6

7 Problematic Next generation of analyzers: - compacts (micro analyzers, micro captors) - coupling with sampling microsystems - directly integrated in the process >> Analysis at the closest of the reaction New Standard (SP76) NeSSI TM New Sampling and Sensor Initiative from CPAC PROBLEMATIC > Difficulties of direct implementation on industrial sites and R&D laboratories - Unsatisfactory accordance between analyzers and industrials and R&D needs - Some laboratories techniques are not always available for in situ application 7

8 Needs Elementary analysis Analysis in liquids Analysis in gases Properties Molecular Properties Molecular Need to employ more compact analyzers to be able to analyze "in the heart of process" 8

9 Elementary Analysis In situ analysis of elements in industrial liquids traces of S, Ni & V in petroleum products traces analysis of contaminants in ex biomass and chemical products,... traces analysis of contaminants in water following of corrosion (traces of metals)... Laser Induced Breakdown Spectroscopy 9

10 Analysis in liquids - Properties In situ analysis of elements in industrial liquids in situ density, viscosity analysis of liquids with msystems in situ refractive index analysis with msystems particles analysis in liquid (solid, catalyst, macromolecules,...) calculation of other properties using mspectrometers Adaptation in function of specific needs Specific developments 10

11 Temperature ( C) density (g/cm 3 ) Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter Repeatability Densité en ligne - Gazole P=Patm, Qv = 2 ml/min T captor ( C) direct density Corrected density at 15 C Repeatability for diesel /1/08 23:16 29/1/08 0:28 29/1/08 1:40 29/1/08 2:52 29/1/08 4:04 29/1/08 5:16 29/1/08 6:28 29/1/08 7:40 Time Products Numbers of measures MV average g/cm 3 St. Deviation g/cm 3 Reapitability g/cm 3 Gasoil 740 0,8509 1, ,

12 Temperature ( C) density (g/cm 3 ) Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter Response to a periodic feed change difference (A-B) g/cm Gasoil A Gasoil A Gasoil A T captor ( C) Raw density Corrected density Gasoil B Gasoil B /1/08 11:15 31/1/08 11:18 31/1/08 11:21 31/1/08 11:24 31/1/08 11:26 31/1/08 11:29 31/1/08 11:32 31/1/08 11:35 31/1/08 11:38 31/1/08 11:41 less than 30s Flow 2ml/min Time

13 Density (g/cm3) Temperature ( C) Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter µpilot test : gasoline + dissolved gas Corrected density at 15 C Laboratory analysis 15 C Temperature Captor ( C) Lost of gas phase Better results with on line analysis /9/08 0:00 5/9/08 0:00 7/9/08 0:00 9/9/08 0:00 11/9/08 0:00 13/9/08 0:00 15/9/08 0:00 17/9/08 0: Date & Hour 13

14 PIC4 PIC1 PIC2 PIC3 Analysis in liquids- Molecular Analysis In situ analysis in different industrial liquids in situ analysis with mspectrometric methods (miniaturized systems), using in situ probes Development and performance optimization in situ analysis of dissolved gases (traces) in hydrocarbons (H 2, O 2,...) optimization of liquid injection systems for on line GC analysis pa FID1 A, (D:\DOCUMENTS AND SETTINGS\JACQUINE\BUREAU\ETUDE HPLIS\DATA\P20BARS\001F0101.D) in situ analysis of liquid by mgc (at the moment only used for gas analysis) min

15 Analysis in gases - Properties and Molecular Analysis In situ analysis in different industrial gases in situ analysis with mspectrometric methods using in situ probes Development en optimization of performances Optimization of Tunable Diode Laser for specific applications TDL Optimization of sensors Density, moisture, H 2,... Analysis in corrosive environments (HF, HCl,...) 15

16 Density (g/m3) Analysis in gases - Properties Example of in situ density in gas phase in µpilot: total gas flow 1l/h CPG analysis for calculate gas density density No flow - Pilot's problem Put to atmospheric presure of gas/liquid pot during liquid sampling GC analysis Density (g/m3) at 15 C 200 Start Pilot /04 23/04 23/04 24/04 24/04 24/04 24/04 24/04 25/04 25/04 25/04 25/04 25/04 26/04 26/04 26/04 26/04 26/04 27/04 27/04 27/04 27/04 27/04 28/04 28/04 28/04 28/04 28/04 29/04 29/04 29/04 29/04 29/04 30/04 30/04 30/04 30/04 13:12 18:00 22:48 03:36 08:24 13:12 18:00 22:48 03:36 08:24 13:12 18:00 22:48 03:36 08:24 13:12 18:00 22:48 03:36 08:24 13:12 18:00 22:48 03:36 08:24 13:12 18:00 22:48 03:36 08:24 13:12 18:00 22:48 03:36 08:24 13:12 18:00 Date & Hour We are able to follow the "real life" of process Better knowledge for R&D development

17 How to answer to the needs for Micro Analysis? Micro Analysis Needs Collaborative project USERS Request - Validation LABORATORIES Research INSTRUMENTALISTS Development & Industrialization INNovAL Project 17

18 INNovAL Project (AXELERA) "L'Analyse en Ligne au cœur du procédé" Targets: -Development of new in situ on line analyzers in accordance with industrial and R&D needs > On the cutting edge of technology -Optimization available technologies presents on the market -Development of new and innovating solutions 18

19 INNovAL Main Actors USERS Request - Validation LABORATORIES Research INSTRUMENTALISTS Development & Industrialization 19

20 INNovAL A structuring project First innovative collaborative technological platform in Lyon Axel ONE (2013) Axel'ONE USERS Request - Validation INNovAL LABORATORIES Research INSTRUMENTALISTS Development & Industrialization 20

21 AXEL ONE An innovative collaborative platform Clean processes UPSTREAM Factory of the futur PROCESS ECO- DESIGN & ECO- EFFICIENCY Technological development, steering, diversification of raw materials, demonstrations, training MODELING Simulation, process control TEST BENCHES Pilots, On line analysis, technological development INNovAL 21

22 AXEL ONE Mode of management and functioning of the platform R&D spaces including: Technological halls Laboratories Shared facilities (Lab benches, extractors, fluids transportation services...) Equipped spaces for service sector (offices, meeting rooms... ) Integrated management facilities (Reception, maintenance, security, logistical support...) Axel One offers: kits dedicated to innovative collaborative project management Axel One Payment model: Rent + charges of kit spaces rent by the partners who have 22 implemented projects

23 Conclusion & outlooks In R&D we need manalyzers to intensify and optimize research productivity and results quality Increase the links between industrials, academic laboratories and instrumentalists to employ new analytical solutions in accordance with real industrial needs INNOVAL project Need to employ an innovative collaborative platform in order to evaluate analytical instruments : pre industrialization before implementation on site Platform AXEL'ONE 23

24 Lyon : Center of Excellence for "Industrial Analysis" in AXELERA Academics laboratories in UCBL Laboratories in CNRS/SCA Ecole des Mînes de St. Etienne in all laboratories : evaluation benches analyzers,... In Axel'One platform 2 laboratories for industrial experimentations, Industrial users (Industrial partners : INnovAL, others) Project of training in UCBL (Master II) specialized in "Industrial Analysis" 24

25 Lyon : Center of Excellence for "Industrial Analysis" in AXELERA Reseach laboratories Industrial laboratories - Training 25

26 Thank you Dr. Franck BACO-ANTONIALI IFP Energies Nouvelles BP3, Solaize, FRANCE 26

27 Renewable energies Eco-friendly production Innovative transport Eco-efficient processes Sustainable resources

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