Pr. Marc Aurousseau - EPFL · PDF filePr. Marc Aurousseau ... derive these closure laws ... Intensifier le procédé par ondes ultrasonores

Actions de Recherche et de Formation dans le domaine de l’Eau à Grenoble (Grenoble INP)

Pr. Marc AurousseauInstitut Polytechnique de Grenoble

Laboratoire de Génie des Procédés Papetiers (LGP2, UMR CNRS/Grenoble INP/CTP/Pagora)

Responsable de l’équipe « Génie Papetier et de l’Environnement »

[email protected] [email protected]

France

Région Rhône-Alpes

7 Laboratoires acteurs à Grenoble : 7 UMR CNRS, Grenoble INP et UJF

[email protected]

2 domaines principaux de recherche :

1- Eaux Industrielles et de Process : Traitementet Réutilisation/Recyclage

2- Eaux Milieu Naturel : Transports et qualité

[email protected]

1- Industrial Wastewater Treatments (WWT) and Water Reuse/Recycling (WR) in Grenoble

[email protected]

WWT and WR research into Environment Rhône-Alpes Cluster

WWT and WR research supported by a Technology Plateform of Envirhonalp :

Processes, Effluents and Industries : PEI

[email protected]

4 cities: Chambéry, Grenoble , Lyon and Saint-Etienne

12 Laboratories or research groups involved

40 senior researchers

20 PhD students

Main examples realised in Grenoble

1-1 Activated Sludge Biological Treatment1-1-1 Reduction Sludge Production1-1-2 Process supervision

1-2 Biofiltration

1-3 Membrane processes: separation and valorisation

1-4 Metal removal: separation and recovery1-4-1 Electrocoagulation process1-4-2 Liquid-liquid extraction and adsorption proce sses

1-5 Ultrasound technique

1-6 Ozonation: application to deinking process1-6-1 Ozone reactive flotation 1-6-2 Deinking process modelisation and simulation

1- Industrial Wastewater Treatments (WWT) and Water Reuse/Recycling (WR) in Grenoble

Goals:

� Reducing excess sludge production

� This study focused on the oxidation of the returned activated sludge by H2O2 used alone and at room temperature in order to minimize the costs of the implementation.

Context:

� In Europe, the production of excess sludge is exceeding 10 million tons of dry solids and forecasted to increase.

� Sludge management is about half of the operating costs.

1-1 Activated Sludge Biological Treatment

1-1-1 Excess activated sludge reduction in wastewat er treatment: use of hydrogen peroxide

Partners: Arkema, CTP, Suez-Environnement,

Grenoble INP/LGP2

Key words: biological treatment, sludge reduction, sludge quality

Experimental setup: Bioreactors of 5 L



Grenoble INP/LGP2


Experimental setup: semi-industrial pilot of 70 L



Grenoble INP/LGP2


Main results:

� Same epurationefficiency with andwithout H 2O2


Total and Soluble COD in the effluent

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tota

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D (m

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CODs

H2O2 introduction


Grenoble INP/LGP2


Main results:

� No biomass growthreduction over thelong term but a significant drop justafter the introduction


TSS and VSS concentration in the aeration basin

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TSS

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70%

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100%

VS

S/T

SS

(%

)

TSS

VSS

%VSS

H2O2 introduction


Grenoble INP/LGP2


Main results:

� Improvement of settling(SVI divided by 2)


Forecasts:� understand hydrogen peroxyde action on the biomass especially for nitrogen effect (nitrification inhibition)� use for settling and dewatering improvement

Sludge Volume Index

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SV

I (m

L.g

-1)

Contact: M. Aurousseau et A. Guillet – LGP2/CNRS-Grenoble INP - [email protected]

H2O2 introduction

Goals:Context:

1-1-2 A semi-industrial pilot for wastewater biolog ical treatment:an innovative conception

Key words: biological treatment, supervision

• Design of an activated sludge pilot unit

– Semi-industrial size

– Modularity

– Flexibility

– Supervision

• Build a model to develop cooperative supervision

Drawbacks- Complex behaviour- Monitoring to prevent dysfunctions- Anticipation of upstream industrial

process accidents

On-line measurementsOff-line measurements

pHO2

ConductivityTurbidityRedox

CODBOD

TSS - VSSWaiting periodDelay of actions

Activated sludge process: the most often used process to treat biodegradable pollution

Partners: LGP2, GIPSA-Lab, Cemagref

1-1-2 A semi-industrial pilot for wastewater biolog ical treatment: an innovative conception

Experimental setup: semi-industrial pilot of 250 L

Storage (2000 L)

Modular tank (250 L )

From primary settler

Settler

pH, nutriments adjustment

Actuators + Sensors

Supervisor rack Electrical device Human

operator

Recycling

M O

2 O

2 O

2 O

2 O

2 O

2 O

2 O

2 O

2

Treated water

Extracted sludge

1 2

4

3

Key words: biological treatment, supervisionPartners: LGP2, GIPSA-Lab, Cemagref


Results:

Treatment efficiency on papermilleffluent:

� 70% removal for COD

� 80% removal for BOD 5

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Time (days)

CO

D-B

OD

(m

g/L)

COD input BOD5 input COD output BOD5 output

0 2 4 6 8 10 12 14 16

Partners: LGP2, GIPSA-Lab, Cemagref Key words: biological treatment, supervision


Results:

ASM1 model validation on thepilot unit:

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 55

60

65

70

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2400

2450 2500 2550

2600

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 135

140

145

150

� Excellent accuracy of the paper model

� Relevance of the moving horizon state observer

Contact: M. Aurousseau et A. Guillet – LGP2/CNRS-Grenoble INP – et C.Cadet – GIPSA-Lab/CNRS-UJF-Grenoble INP

[email protected]

Forecasts:integration of the modelinto the global model BSM1 withsettling modelisation for humanhelp tool

Partners: LEGI, LTHE, 3SR, LRP/CNRS-UJF-Grenoble INP

1-2 Coupling Hydrodynamic/Biofilm in a biofilter:Multiscale approach

Key words: bioprocesses, biofilms experiments, modelling, coupling hydrodynamic-biomass

Goals:

� To understand relations betweenhydrodynamic and biofilm:

- Initial and reversible adhesion underphysico-chemical conditions

- Cell (bacteria) growth upon surface

- Biofilm (structure, composition, activity)

- Flow-induced cell detachment

� To develop an operational model biofilter to

optimizise the design and to intensify the use

Context:

Biofiltration is a bioprocess with fixed-

biomass for wastewater treatment:

robust, compact, limited sludge

production, low functioning cost (energy),…

but with empirical design and operating

dysfunctionings mainly related to clogging

effect

limited development and use

Experimental setup and facilities:


Pilot scale biofilter (LEGI)

Flow microchamber (Rheology Lab .) for continuous observation under microscopy

� Microbiology laboratory (LTHE)- Chemical and biological analysis- Image processing…

� X-ray tomograph (3SR) : in situ measurement of biomass distribution in porous media

1-2 Coupling Hydrodynamic/Biofilm in a biofilter: Multiscale approach


� Classical Kozeny law or related models developpedfor biofilm are not able to modelized permeabilityreduction due to thebiofilter colonization:

- biofilm microstructure(EPS matrix)

- biomass distribution atthe pore scale (colonies) or in the reactor (preferentialpath)


Main Results:



� Classical Monod law is not available

� Biological kinetics are closure lawswhose structures depend on processesaveraged on the biofilm and at the reactor

scale. They integrate the biofilm response to environmental and hydrodynamical stess.

� Experiments at microscale required to derive these closure laws


y = 0,6906e0,01x

R2 = 0,9547

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time [min]

A/A

o

Tw - 1 Pa

Exponentiel(Tw - 1 Pa)

Determination of growth rate

Exponential population variation

Work in progress: to write a model at the macro-scale with the correct closure laws obtained from the experiments at the micro-scale

Contact: P. Sechet et F. Pignon – LEGI et LRP/CNRS-UJF-Grenoble INP - [email protected]

Main Results:Contexte :

� Production de biomatériaux issusentre autre de la biomasse cellulosique

� Valorisation des sous produits de fabrication de pâte à papier.

Partners: LRP/CNRS-UJF-Grenoble INP et

LGP2/CNRS-Grenoble INP

Mots clés: membrane, microfiltration, polysaccharides, amidon, cellulose

1-3 Procédés de séparation membranaire : production en continu de nanocristaux d’amidon et de polysaccharides

Objectifs :

� Produire en continu des nanocristauxd’amidon ou de cellulose

� Séparer les différents polymèrescontenus dans les liqueurs de cuissondes pâtes pour leur valorisation en biomatériaux type bioplastiques

� Caractérisation et modélisation des phénomène de colmatage

Projet : concevoir un procédé d’extraction en continu des nanocristaux d’amidon par microfiltration

Intégrer une boucle d’extraction des

nanocristaux au fur et àmesure de leur

productionNanocristaux

+ sucres

Amidon partiellement

hydrolysé + sucres

Amidon partiellement

hydrolysé +

nanocristaux +sucres

Membrane




H2SO4 3M


• Caractérisation des filtrats, rétentats et membranes :

• Développement de techniques analytiques adaptées :

SEC, chromatographie liquide ionique

• Milieux poreux (MEB), µ-analyse X, AFM, porosimétrie

au mercure

• Conception du procédé et choix des matériaux / agressivité du milieu :

• Membrane , Dispositif opératoire, Matériaux

• Optimisation des paramètres opératoires –modélisation : Pressions, débits, concentration





-Traitement de l’eau et des effluents (38%)- Biotechnologies, Pharmacie (20%)

- Agro-alimentaire (20%) - Chimie, Nucléaire, microélectronique

Caractérisation et modélisation des phénomènes

de concentration de particules au voisinage des

membranes de filtration

Pression Transmembranaire ∆∆∆∆P

Débit tangentiel Q

Flux de perméation J

Limitations lors de la filtration

La polarisation de concentration

Le colmatage

Comprendre la polarisation, le colmatage…




Comprendre les mécanismes impliqués dans la formation des

couches accumulées pour contrôler la stabilité de la filtration


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100 300 500

Distance z à la membrane (µµµµm)

Concentration en particules φφφφv (%)

z

y

xCellules de filtration adaptées à l’observation sous

diffusion de rayons x aux petits angles (SAXS) « in-situ »

ESRF

Rayons X∆∆∆∆P

Q

J

Mise en évidence de l’origine de la stabilité du procédé et de la réversibilité du colmatage

Données expérimentales essentielles pour la modélisation

��Pcroissante

Ultrafiltration de suspension de

Laponite





Intensifier le procédé par ondes ultrasonores…

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Sans Ultrasons

Avec Ultrasons

∆∆∆∆P x 105 (Pa)

Flux de perméation J (L/m²/h)

Q= 0.45 l/min

Cellule de filtration couplée avec un

système ultrasonore « in-situ »

Ondes ultrasonores

J

∆∆∆∆PQ

Rayons XRayons X

Ultrafiltration suspension d’argile

de Wyoming




Contrôle de l’organisation de la matière accumulée

Augmentation des performances


Perspectives :

� Séparation de nouveaux biomatériaux issus de la biomasse végétale

� Compréhension des phénomènes de polarisation lors de la filtration membranaire et prévention du colmatage par US

� Applications industrielles diverses :

- Amélioration des rendements de récupération de produits valorisables

- Amélioration des procédés de microfiltration comme ceux des bioréacteurs à membrane du traitement des eaux usées .





Goals:

� Development and optimization of separation processes of metals:

� decontamination of water (Mn, Cr, Zn)

� metal recovery (Li, Pt).

Context:

� Importance of metal decontamination of water and of the recovery of metals from waste or objects in end of life (batteries).

1-4 Metal removal : Separation and metal recovery

Partners: LEPMI/CNRS-UJF-Grenoble INP

Recupyl, CEA, BresilKey words: water treatment, metal recovery

Experimental setup:

1-4-1 Removal of mixture of copper, zinc and nickel from wastewater using electrocoagulation process

V A

Pump

Power supply

+ _

container

Electro -

coagulation

cell



% removal

Ni 82,3

Zn 92,6

Cu 97,9

Metal ions removal from aqueous solution during 1 hour using reactor with 4L capacity (Current density: 5mA/cm2, solution volume: 4L), iron electrodes.

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nc(

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Ni

Zn

Cu

Metal ions removal from aqueous solution during 4 hours using reactor with 20L capacity (Current density: 5mA/cm2, solution volume: 20L); Aluminum electrodes

1-4-1 Removal of mixture of copper, zinc and nickel from wastewater using electrocoagulation process



1-4-2 Liquid-liquid extraction and adsorption of li thium

Contact: PX Thivel et L. Svecova– LEPMI/CNRS-UJF-Grenoble INP - [email protected]

Extraction efficiencies versus pH (Ci= 0,01 mol Li / L, specific organic phase 1 mol, contact 3 min)

Implementation of cycle of extraction / stripping and metal concentration

Matériaux recyclés

Prétraitement(broyage)

Dissolution(mise en solution)

Séparation /purification

before stirring, after stirring, after settling

1-5 Design and scale-up of advanced oxydation process involving ultrasound technique

Forecasts: From laboratory to industrial scale: towards new combinedreactor technology

90 l/h 120 l/h 180 l/h 240 l/h

72% 65% 44% 34%

Contact: N. Gondrexon, LRP/CNRS-Grenoble INP-UJF - [email protected]

Laboratory scale pilot(UV + US 500 kHz)

Degradation yield (TCE) vs. feed flow rate

Scale up

50% removal yieldat 100l/h

Industrial scalepilot

(UV + US 500 kHz) Goals:

• To improve the ink removalselectivity

• To oxidize colloidal anddissolved contaminants in process waters

• To reduce water consumptionand effluent

Context:

• Deinking process of « old papers »generates large volumes of sludgesmainly due to the flotation stage.

• Process water contamination impedethe complete closure of water circuits and zero liquid effluent emission

Partners: Grenoble INP/LGP2, CTP, ENSMSE, Kadant Lamort,

Kemira,Wedeco, Degrémont

1-6-1 Intensification of recovered cellulose fibres purification by ozone flotation

Keywords: Ozone flotation, paper deinking, water consuption

Ozonation: application to deinking process

Experimental setup and facilities:

Application and development of the processFour years project (2011-2014) for the scale up ofthe ozone flotation process

� Ozone-resistantlaboratory flotation cell

� Flotation cell instrumentationfor measurement of:

- RTD for pulp mixing regimes

- Bubble size distribution

- Gas hold-up measurement

Partners: Grenoble INP/LGP2, CTP, ENSMSE, Kadant Lamort,

Kemira,Wedeco, Degrémont

Keywords: Ozone flotation, paper deinking, water consuption


Main Results:

Forecasts:Four years project (2011-2014) for the scale up of the ozone flotation process

Same flotation rate constant with ozone with an increase of the selectivity (+ 50%)

Contact: M. Aurousseau, D. Beneventi et M. Marlin – Grenoble INP/LGP2 - [email protected]

30% COD less in flotation liquid effluents


Goals:

To develop a process simulation system for

optimising the design and control of

industrial flotation deinking lines

Context:

� Flotation deinking process is governed by

complex transport mechanisms.

� Lack of proper simulation tools for

optimising the deinking line design and

process water management

Partners: Grenoble INP/LGP2, CTP

1-6-2 Modelling and simulation of the flotation dei nking process

Keywords: Flotation deinking, simulation, process management

Experimental setup: a continuouslaboratory flotation cell

- Process simulation systemimplemented on ProSim+ software

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Rem

oval

(%

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Total ink removal

Ink removal 1st

Ink removal 2nd

Surfactant removal

Results

Application and development of the process:� Study of the impact of the fibre suspension characteristics on mixing and fibre transport in aerated slurries� Addition of ozone chemical reactions� Optimization of water reuse and quality

Contacts:D. Beneventi et P. Nortier – Grenoble INP/LGP2 - [email protected]

Ink and surfactant removal efficiency from process waters in industrial two-stagesystems vs. surfactant concentration has been succesfully simulated

1ry Froth dilution

1ry - 1 1ry - 2 1ry - 3 1ry - 4 1ry - 5 1ry - 6

2ry - 1 2ry - 2

Correlation between processperformances and chemical dosage

1-6-2 Modelling and simulation of the flotation dei nking process

2- Eaux Milieu Naturel : transports et qualité

2-1 Transfert de polluants contenus dans les sédiments

2-2 Impact des nutriments sur l’eutrophisation : Day-River project

[email protected]

Goals:

� quantification of suspended sediments and pollution fluxes

� siltation of reservoirs

� impact of hydraulic flushes vsnatural flood events

� environmental management of hydraulic flushes

Context:

� Mountainous watersheds located in the French Alps are largely impounded by reservoirs operated by EDF (French Electricity Company) for hydroelectricity production

� The understanding of solid floods and hydraulic flushes impacts is essential for a better management of alpine rivers

2-1 Study of suspended sediment and associated poll ution dynamics in mountainous rivers

Partners: LTHE-CNRS/UJF/IRD/Grenoble INP

Cemagref, EDF

Key words: suspended sediment, hydraulic flush, pollution, mountaneous watershed

Study site: Isère watershed (French Alps) i.e. 5 570 km2

Location of monitoring stations


Cemagref, EDF



Campus monitoring station

High frequency monitoring by turbidimetry

Traille + ADCP

Turbidimeter HachLange Solitax 0-50 g/L ADCP

Campus monitoring station

Automatic sampler


Cemagref, EDF



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mars-06 juin-06 sept-06 nov-06

Water flow (m3/s)

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DébitMESMES Isco

Figure : High frequencymeasurments of TSS and water flow for 2006 :

1) Natural flood

= 500 000 tons

2) Hydraulic flush

= 60 000 tons

1

2


Cemagref, EDF



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TSS (mg L-1)

PO

C%

y = 28.82x-0,7499 + 0.89

R2 = 0.79

Figure : Close relationshipbetween Particulate organicCarbon (POC) and TSS

> the high frenquencymeasurment of TSS throughturbidity measurments willhelp to better calculate POC flux and then dissolvedorganic pollution


Cemagref, EDF



Goals:

� quantification of organic and nutritive pollution fluxes

� eutrofication risk

� measurement, budget and modeling approach

Context:

� The Red River Delta is densely populated. Hanoï city releases high quantity of domestic pollution (organic matter, nutrients and bacteria) and agriculture is in expansion in the Delta.

�The delta is essential for living resources (fishing, aquaculture) and water resources

2-2 Day-River project (2005-2008) : Impact of nutrients inputs on the Red River Delta: eutrofication risk

Partners: Univ. Paris 6 (Sisyphe), Université Toulouse (GET),

VAST-Hanoï, Institut of technology and environment-Hanoï

Key words: Red river Delta, nutrients and organicpollution, eutrofication risk assessment

Figure 1: Population density in the Red River delta Figure 2 : Land use in the Red River delta

From Luu et al, Biogeochemistry 2010

Partners: Univ. Paris 6 (Sisyphe), Université Toulouse (GET),

VAST-Hanoï, Institut of technology and environment-Hanoï

Key words: Red river Delta, nutrients and organicpollution, eutrofication risk assessment

2-2 Day-River project : Impact of nutrients inputs on the Red River Delta: eutrofication risk

Nitrogen massbalance in theRed River Delta : domestic andagricultural sources andexportation to thecoastal zone.

From Luu et al, Biogeochemistry 2010

Contact: J. Némery – LTHE-CNRS/UJF/IRD/Grenoble INP - [email protected]

2-2 Day-River project : Impact of nutrients inputs on the Red River Delta: eutrofication risk

Better knowledgefor actions plan

and control

Des cours ou cursus dans le domaine de l’environnement et/ou de l’eau dans :

� les filières des écoles de Grenoble INP :

ENSE3, Phelma, Pagora

� Programme PIME inter-écoles (1 semestre) :

Procédés Industriels et Management Environnemental

[email protected]

Formation dans le groupe Grenoble INP

Contact: A. Guillet – Grenoble INP-Pagora – [email protected]

Engineering training: Industrial Processes and Environmental Management - PIME

• Goals of the training→ give a double-competence in environmental issues to future

engineers: technical and managerial aptitudes to face environmental problems

• Organisation→ 25 students

→ the last semester of the engineer training – 6 months from September to January

→ Location: Grenoble

→ 30 ECTS credits given in French language

Engineering training : Industrial Processes and Environmental Management - PIME

• Main courses→ Wastewater physico-chemical and biological treatments: waste

waters, gas and solids

→ Process control

→ Ecosystem functioning: pollutant dispersion and impact

→ Environmental management – quality and security

→ Life cycle assessment

→ Renewable energies

→ Industrial project

→ Experimental works on semi-industrial pilot equipment

Engineering training: Industrial Processes and Environmental Management - PIME

Experimental setup and facilities: several pilots and analytical laboratories

Membran processes

Coagulation-Floculation-Sletting

Activated Sludge Process

Resin bed filtration

En conclusion, dans le domaine de l’eau :

[email protected]

Grenoble INP et ses laboratoires associés réalisent une Recherche sur :

� des procédés de traitement des effluents et des eaux d e process :

� Traitemenents biologiques à biomasse libre ou fixée, Procédés

membranaires et Procédés par oxydation avancée (US, Ozone,…)

pour la pollution organique

� Electogoagulation, Extraction et Cémentation électochimique pour

les métaux en solution

� l’étude du milieux naturel et des phénomènes de transpor t :

� Interractions/transferts eaux usées/sédiments

� Interractions/transferts sédiments/eau du milieu naturel

[email protected]

Grenoble INP et ses écoles d’ingénieurs réalisent une Formation sur :

� les procédés de traitement des effluents et des eaux d e process :

� l’étude du milieux naturel

� les ouvrages et réseaux hydrauliques

� le management environnemental

� Etc…

Merci pour votre écoute… des questions ?

Donc de nombreuses possibilités d’échanges tant en Connaissances Scientifiques qu’en Etudiants

ou Enseignants-chercheurs

En conclusion, dans le domaine de l’eau :

Documents

Pr. Marc Aurousseau - EPFL · PDF filePr. Marc Aurousseau ... derive these closure laws ... Intensifier le procédé par ondes ultrasonores