Trends and Needs for on Line Micro Analysis for R&D ...depts.washington.edu/cpac/NeSSI/42_IFPAC_2011/presentations/FB… · L’analyse des procédés: un enjeu pour l'industrie chimique

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

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FBA – IFP Energies nouvelles – IFPAC 2011 – Baltimore – MD - USA

Trends and Needs for on Line Micro Analysis for R&D

INnovAL: Innovative Project for Micro Process

Analytical Technology

Dr. Franck BACO-ANTONIALI IFP Energies nouvelles BP3, 69360 Solaize, FRANCE [email protected]

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FBA – IFP Energies nouvelles – IFPAC 2011 – Baltimore – MD - USA 2

Agenda

Introduction

Trends and needs for R&D on line micro analysis

INNOVAL Project

Technologic platform AXEL'ONE : An collaborative platform

Conclusions and outlooks

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L’analyse des procédés: un enjeu pour l'industrie chimique

PRODUCTION

Products Quality

Safety of employees

and neighborhood

Environment protection (pollution)

R&D

Reduction of costs

Process intensification

ANALYSIS = PROCESS CONDITIONS CONTROLS

Objective

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Evolution of needs in term of analyzers in R&D

µ Pilots HTE Pilots Process Intensification

Reducing of sample volume

"Classical" analyzers

µ Analyzers

µCaptors

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• 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, ...

Needs for R&D and Process Intensification

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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

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Needs

Need to employ more compact analyzers to be able to

analyze "in the heart of process"

Properties Molecular Properties Molecular

Analysis in liquids Analysis in gases Elementary analysis

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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

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Analysis in liquids - Properties

In situ analysis of elements in industrial liquids

in situ density, viscosity analysis of liquids with µsystems in situ refractive index analysis with µsystems particles analysis in liquid (solid, catalyst, macromolecules, ...) calculation of other properties using µspectrometers

Adaptation in function of specific needs Specific developments

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Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter Repeatability

Densité en ligne - Gazole

P=Patm, Qv = 2 ml/min

22

22.5

23

23.5

24

24.5

25

28/1/08 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

Tem

pera

ture

(°C)

0.8435

0.8445

0.8455

0.8465

0.8475

0.8485

0.8495

0.8505

0.8515

dens

ity

(g/c

m3 )

T captor (°C)direct densityCorrected density at 15°C

Products

Numbers of measures

MV average g/cm3

St. Deviation g/cm3

Reapitability g/cm3

Gasoil

740

0,8509

1,96.10-5

5,49 10-5

Repeatability for diesel

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Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter Response to a periodic feed change

less than 30s – Flow 2ml/min

23

23.5

24

24.5

25

25.5

26

26.5

27

31/1/08 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

Time

Tem

pera

ture

(°C)

0.8405

0.8415

0.8425

0.8435

0.8445

0.8455

0.8465

0.8475

0.8485

0.8495

0.8505

dens

ity

(g/c

m3 )

T captor (°C)

Raw density

Corrected density

Gasoil A Gasoil A Gasoil A

Gasoil B Gasoil B

difference (A-B) 0.0006 g/cm3

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Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter µpilot test : gasoline + dissolved gas

0.7105

0.7155

0.7205

0.7255

0.7305

0.7355

0.7405

0.7455

0.7505

3/9/08 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 0:00

Date & Hour

Den

sity

(g/

cm3)

15.00

25.00

35.00

45.00

55.00

65.00

75.00

Tem

pera

ture

(°C

)

Corrected density at 15°CLaboratory analysis 15°CTemperature Captor (°C)

Better results with on line analysis

Lost of gas phase

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In situ analysis in different industrial liquids

in situ analysis with µspectrometric methods (miniaturized systems), using in situ probes Development and performance optimization

in situ analysis of dissolved gases (traces) in hydrocarbons (H2, O2, ...)

optimization of liquid injection systems for on line GC analysis

in situ analysis of liquid by µGC (at the moment only used

for gas analysis) ...

Analysis in liquids- Molecular Analysis

min0 20 40 60 80 100

pA

10

15

20

25

30

35

40

45

FID1 A, (D:\DOCUMENTS AND SETTINGS\JACQUINE\BUREAU\ETUDE HPLIS\DATA\P20BARS\001F0101.D)

PIC

1

PIC

2

PIC

3

PIC

4

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In situ analysis in different industrial gases

in situ analysis with µspectrometric methods using in situ probes Development en optimization of performances

Optimization of Tunable Diode Laser for specific applications Optimization of sensors

Density, moisture, H2, ... Analysis in corrosive environments (HF, HCl, ...)

Analysis in gases - Properties and Molecular Analysis

TDL

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Analysis in gases - Properties Example of in situ density in gas phase in µPilot: total gas flow 1l/h

density 1200

0

200

400

600

800

1000

1200

1400

23/0413:12

23/0418:00

23/0422:48

24/0403:36

24/0408:24

24/0413:12

24/0418:00

24/0422:48

25/0403:36

25/0408:24

25/0413:12

25/0418:00

25/0422:48

26/0403:36

26/0408:24

26/0413:12

26/0418:00

26/0422:48

27/0403:36

27/0408:24

27/0413:12

27/0418:00

27/0422:48

28/0403:36

28/0408:24

28/0413:12

28/0418:00

28/0422:48

29/0403:36

29/0408:24

29/0413:12

29/0418:00

29/0422:48

30/0403:36

30/0408:24

30/0413:12

30/0418:00

Date & Hour

Den

sity

(g/m

3)

GC analysisDensity (g/m3) at 15°C

CPG analysis for calculate gas density

Put to atmospheric presure of gas/liquid pot duringliquid sampling

No flow - Pilot's problem

Start Pilot

We are able to follow the "real life" of process Better knowledge for R&D development

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How to answer to the needs for Micro Analysis?

Micro Analysis Needs Collaborative project

USERS Request - Validation

LABORATORIES Research

INSTRUMENTALISTS Development & Industrialization

INNovAL Project

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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

INNovAL Project (AXELERA) "L'Analyse en Ligne au cœur du procédé"

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5 Skids on NeSSI platforms (Astute, Intraflow) for development of on-line applications – Evaluation in real conditions (P, T, ...)

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INNovAL – Main Actors




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First innovative collaborative technological platforms in Lyon

INDEED (2013)

INNovAL – A structuring project




INNovAL INDEED

Specific platform for industrial analysis in INDEED

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INDEED 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

TEST BENCHES Pilots, On line analysis, technological development

MODELING Simulation,

process control

INNovAL

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Conclusion & outlooks In R&D we need µanalyzers to intensify and optimize research

productivity and results quality Increase the links between industrials, academic laboratories and

instrumentalists to develop new analytical solutions in accordance with real industrial needs

INNOVAL project

Need to employ an innovative collaborative platform in order to develop & evaluate analytical instruments : pre industrialization before implementation on site

Platform Industrial Analysis in INDEED

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Lyon : Center of Excellence for "Industrial Analysis" in INDEED

Academics laboratories in UCBL Laboratories in CNRS/SCA Ecole des Mînes de St. Etienne

in all laboratories : teams, evaluation benches analyzers, ....

In INDEED platform laboratories for industrial experimentations, pilots, ...

Industrial users (Industrial partners : INnovAL, others)

Project of training in UCBL (Master) specialized in "Industrial

Analysis"

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Lyon : Center of Excellence for "Industrial Analysis" in INDEED Reseach laboratories – Industrial laboratories - Training

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Thank you

Dr. Franck BACO-ANTONIALI IFP Energies nouvelles BP3, 69360 Solaize, FRANCE [email protected]

Documents

Trends and Needs for on Line Micro Analysis for R&D ...depts.washington.edu/cpac/NeSSI/42_IFPAC_2011/presentations/FB… · L’analyse des procédés: un enjeu pour l'industrie chimique