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Incorporation Incorporation of of Catalytic Catalytic Compounds Compounds in in the the Porosity Porosity of of SiC SiC Wall Wall Flow Flow Filters Filters 4 4 Way Way Catalyst Catalyst and and DeNOx DeNOx Application Application examples examples DEER MEETING August 15 TH- 2007 - Detroit (MI) Jean-Pierre JOULIN CTI Bruno CARTOIXA CTI Didier TOURNIGANT CTI Arnold LAMBERT IFP Jean-Christophe RUIZ CEA Anne JULBE IEM CERAMIQUES TECHNIQUES ET INDUSTRIELLES S.A. La Resclause - Route de Saint Privat F 30340 SALINDRES - FRANCE E-mail: [email protected] Site internet: www.ctisa.fr Phone: +33 466 858 870 Fax: +33 466 857 009 1 CTI - CONFIDENTIAL

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Page 1: Incorporation of Catalytic Compounds in the … · Incorporation Incorporation of Catalytic Compounds in in the ... 4 4 Way Catalyst and DeNOx Application Application examples

IncorporationIncorporation ofof CatalyticCatalytic CompoundsCompounds inin thethePorosityPorosity ofof SiCSiC WallWall FlowFlow FiltersFilters ––

44 WayWay CatalystCatalyst andand DeNOxDeNOx ApplicationApplication examplesexamples

DEER MEETING

August 15TH-2007 - Detroit (MI)

Jean-Pierre JOULIN CTI Bruno CARTOIXA CTI Didier TOURNIGANT CTI

Arnold LAMBERT IFP Jean-Christophe RUIZ CEA Anne JULBE IEM

CERAMIQUES TECHNIQUES ET INDUSTRIELLES S.A.La Resclause - Route de Saint Privat F 30340 SALINDRES - FRANCE

E-mail: [email protected] Site internet: www.ctisa.frPhone: +33 466 858 870 Fax: +33 466 857 009

1

CTI - CONFIDENTIAL

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AGENDA

• Short CTI presentation

• Introduction – Why to concentrate in one or two components all the exhaust gas

containing HC, CO, NOx and PM

• Exploration of 3 different methods of catalyst impregnationinside the pore of a SiC DPF – Supercritical CO2 method – Sol Gel impregnation – Incorporation of catalyst with the slurry forcing method

• Zeolith impregnation of SiC DPF for DeNOx function usingSCR method

• Conclusions CTI - CONFIDENTIAL

2

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SHORT CTI PRESENTATION

CTI is specialized in perfecting the design of a wide range of technical ceramics often porous, whose applications are mainly in environment, filtration, catalysis fields and SOFC.

These include :

• Liquids filtration : membranes supports in ultra and micro filtration. • Gas and particles filtration : tubular, flat, honeycomb, foam filtration

carriers, diesel particulate filter. • Catalysts supports : pellets with high specific area, honeycombs,

smooth and grooved porous rings. • Liquid metals filtration : honeycombs and foams refractories. • Special refractories : withstanding temperatures higher than 1 600°C. • Special ceramic washcoast for COx, DeNOx, VOC treatment and

SOFC applications.

CTI - CONFIDENTIAL

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CTI - CONFIDENTIAL

Factory area : 6 000 m2

Laboratory and pilot area : 1 000 m2

Industrial and laboratory equipment :

mixers (1 to 1200Kg), extrusion press (1 to 400L), high frequency and microwave dryers, gas and electric kilns (0.4 to 10m3 until 1700°C), laboratory equipment, ...

•Scientific manager : JP. JOULIN • Adm. & Financial Manager : N. DELBIANCO •Dr in Catalysis & membranes : E. LOURADOUR

D. TOURNIGANT •4 Ceramic engineers : L. ESPIN

B. CARTOIXA F. PEY G. GAUDRY

• Quality insurance : S. ENJOLRAS •10 Technicians & laboratory people

Created : 8th of march 1990

Independent SME . French Institute Of Petrol as Share holder Capital : 220 000 €

Numbers of employees: 75

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Membrane materials and design forHigh temperature applications ( > 500°C)

Inert porous supports (mainly for filtration):Al2O3, SiO2, TiO2, SiC, ZrO2, Y2O3….

Geometry design Active materials (for catalysis)CeO2/ZrO2

granules, foams, tablets,

Honeycomb, flat, tubular, CeO2/Al2O3/Pt, CeO2/Gd zeolithes,

washcoat, membrane ZnO, V2O5

Perovskites (LSM), ….. 5

CTI - CONFIDENTIAL

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CTI - CONFIDENTIAL

6

HC, CO, NOx, PM

INTRODUCTION

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CTI - CONFIDENTIAL

Diesel emissions reduction legislation trends in Europe

Euro4 UFEuro4 UF DPFDPF systemsystem

VehicleVehicle’’s environmental progresss environmental progress

Fiat courtesy

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CTI - CONFIDENTIAL

CURRENTLY DPF SYSTEM + DeNOx TRAP

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CURRENTLY DPF SYSTEM + DeNOx TRAP

SYSTEMS PROCESS

Catalysed DPF Cordierite Catox + SiC DPF - Soot Oxydations with NO2 with or without catalysis

SCRT System (JM)

Cordierite Catox + SiC/cordierite DPF+SCR-NOx

-Soot Oxydations with NO2

NO2+PM CO 2+N2

-Catalytic reduction of NOX

DPNR System (Toyota)

Cordierite Catox + DPF+N0x trap 4 WAY CATALYSIS

9

CTI - CONFIDENTIAL

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4-WAY CATALYSIS : eliminate HC, CO, NOx and PM with a single treatment

Catalytic phase impregnation + NOX deeptrapping within the pores of the filtering

support

¾ Favor the NOx trapping and the oxidative catalysis in terms of volume (high SBET) together with the important function of absolute particles filtering (no thick covering of the surface that would desactivate the catalyst and blocks the NOx trapping).

¾ Favor the synergy effect between NOX trapping and particles oxidation

Interest of nanophased materials :

¾ Homogeneous materials, finely divised with

high SBET

¾ specific properties (surface activity highly increased)

device

Particles trapped and oxidized when passing through the pores

Catalyst + NOx trap deposited onto the

ceramic walls

CTI - CONFIDENTIAL

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CTI has developed a new composite SiC DPF able to be easily catalysed. The catalyst is impregnated inside the porosity of wall flow :

• Porosity of the CTI SiC DPF is around 46% and pore size around 17/19 µ.

• The great advantage of CTI’SiC composite product is to be already treated against all the oxidation attacks and so to preserve the catalyst performance during ageing. 11

CTI - CONFIDENTIAL

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CTI - CONFIDENTIAL

Since 2003 CTI has explored 3 different ways of catalysis impregnation :

• CO2 supercritical impregnation with CEA(Pierrelatte, Atomic Energy Center)

• Sol gel impregnation with IEM Montpellier (European Institute of membrane)

• Forced slurry method with IFP (French Petroleum Institute) (patented)

EXPLORATION OF 3 DIFFERENT METHODS OF CATALYST IMPREGNATION

INSIDE THE PORE OF A SiC DPF

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CTI - CONFIDENTIAL

SEM PHOTO OF A CTI’S DIESEL PARTICULATE FILTER (DPF)

Wall flow filter

Soots

Soot Deposit configuration before regeneration

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CTI - CONFIDENTIAL

SUPERCRITICAL CO2 METHOD

with collaboration of CEA Pierrelatte - 2004

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Pressure

Supercritical CO2

7,4 MPa LiquidSolid Critical

point

Triple Gaz point

Temperature 304,1 K

Phase diagram of supercritical CO2

CTI - CONFIDENTIAL

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MATERIALS

Particularity : The synthesis and macroporous support impregnation was carried out in a single step, in a 1 litre high-pressure vessel. After introducing a specific amount of selected catalyst formulation in the autoclave containing the monolith, the liquid CO2 was pumped into the vessel up to the operating pressure of 30 MPa. The reaction temperature was regulated at 573 K using an external electric heater. The contact time of the reactants in SC CO2 was 1 hour

Vent TP

Pumps Cooler

Heater

High pressure vessel

T

PPPP

Solution of Precursors + Monolith

Liquid CO2 Tank

16

CTI - CONFIDENTIAL

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SiC grain

Catalyst layer

Catalyst layer

SiC grainSiC grain

Catalyst layer

SiC grain

Cordierite

Catalystlayer

layer

eriteCatalystlayer

17

CTI - CONFIDENTIAL

RESULTS – SEM – SiC and Cordierite analysis

SiC grain

Catalyst layer

Catalyst layer

SiC grain 550

400 - 700

150

Thickness (nm)

3.2SiC 76mm**

1.7Cordierite 15mm

1.5SiC 15mm

Mass deposited (%wt)

Samples material / length

Sol composition : Alumina – Zirconia – Ceria – Baryum oxyde

CordiCordierite

Catalyst layer Cordierite

Catalyst layer

**thickness of the active layer after 2 impregnations

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CTI - CONFIDENTIAL

SOL GEL IMPREGNATION

with collaboration of IEM Montpellier

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CERAMICS GRIT IMPREGNATED WITH NANOPHASE

CATALYST (350 nm layer) ON HONEYCOMB FILTER 1/2

19Sol gel composition Alumina, Ceria, Zirconia, Baryum oxide CTI - CONFIDENTIAL

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2 3 4

ise

de p

oids

cum

ulée

(%)

20

CTI - CONFIDENTIAL

0 1 5 0,0

0,5

1,0

1,5

2,0

2,5

3,0

3,5

4,0

4,5

5,0

Pr

Nombre d'imprégnations

CERAMICS GRIT IMPREGNATED WITH NANOPHASE

CATALYST (350 nm layer) ON HONEYCOMB FILTER 2/2

Number of coatings

Wei

ght

incr

ease

(%)

SiC3092 SiC1891

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CTI - C

21

ONFIDENTIAL

MULTI IMPREGNATION RESULTS

4M18SiC3092-3 (coupe)

4M18SiC3092-9 (cloison)

4M18SiC3092-2 (coupe-surface)

* Layer thickness is around 2µ after depositio * Cracks can appear up to 4 layers

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CTI - CONFIDENTIAL

INCORPORATION OF CATALYST

WITH THE SLURRY FORCING METHOD

with collaboration of IFP (French Petroleum Institute)

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Incorporation of a NOx-trap type catalytic formulation inside the porosity of a SiC wall flow filter

(WFF) has been performed, forcing a slurry of the catalyst

through the substrate.

CTI - CONFIDENTIAL

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SLURRY PREPARATION

NOx trap formulation :

Precious metal Pt, Pd, Rh

Catalyst oxide :BaO - CeO2 - ZrO2 - Al2O3

Adjust the viscosity and particle size distribution

• fluid enough

• Dv90/Dpores < 0.25

Dv90 : measured by laser diffraction

Dpores : mean pore size of the WFF, measured by Hg porosimetry

CTI - CONFIDENTIAL

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CTI - CONFIDENTIAL

IMPREGNATION

SiC cores characteristics:

1" diameter, 3" length, 180 cpsi,

20 µm mean pore diameter,

55% porosity

impregnation unit

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26

CTI - CONFIDENTIAL

CHARACTERISATION / TESTING

SEM pictures of a core loaded with 159 g/l catalyst

• Washcoat inside the porosity

• Whole SiC surface coated

•Thickness 1 to 8 µm

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27

CTI - CONFIDENTIAL

SCALE UP

5"66 diameter, 6" length, 180cpsi, 19 µm mean pore

diameter, 50% porosity

washcoat loading : 190 g/l

washcoat-induced pressure drop : 15 mbar (50000 h-1)

Scale up succeeded

• high loading

• low pressure drop

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CTI - CONFIDENTIAL

0

5

10

15

20

25

108 103 159 185

Washcoat loading (g/l)

P r es

su r e

d r o

p in

d u ce

d b y

w as

h co a

tde

po s i

t io n

( m b

a r ),

at 6

3 00 0

h -1

Pressure drop as a function of washcoat loading

0

10

20

30

40

50

60

70

80

90

100

100 150 200 250 300 350 400 450 500

temperature (°C)

NO

x co

nver

sion

(%)

110 g/l

208 g/l

Synthetic gas bench testing of deNOx activity

• Low pressure drop at high loading

• DeNOx activity comparable to that of flow through monoliths

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CONCLUSIONS OF IFP/CTI METHOD

• Versatile method to deposit any type of catalytic formulation inside the porosity of wall flow filters • Method has been scaled up to real size filter • Key point resides in adapting the slurry's particle size distribution to the mean pore size of the substrate.

29

CTI - CONFIDENTIAL

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0

10

20

30

40

50

60

70

80

100 150 200 250 300 350 400 450 500

Temperature ( °C)

Con

vers

ion

NO

x(%

)

Reference ceramic contactorsol gel route 60g/LSupercritical CO 2 route 48 g/L

Reference ceramic contactorsol gel route 60g/LSupercritical CO 2 route 48 g/L

30

CTI - CONFIDENTIAL

FIRST QUALITATIVE CATALYSIS RESULT FOR NOx CONVERSION COMPARISON OF THE DIFFERENT METHODS

0

10

20

30

40

50

60

70

80

100 150 200 250 300 350 400 450 500

Temperature ( °C)

Con

vers

ion

NO

x(%

)

180 g/L sol gel route 60g/L Supercritical CO 2 route 48 g/L

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OTHERS ‘ IMPREGNATION TRIALS WITH THE SAME TECHNOLOGY

Zeolith impregnation of CTI SiC DPF for DeNOx function using SCR method.

CTI - CONFIDENTIAL

31

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IMPREGNATIONN° Filter CTI CTI 039/06 CTI 031/06 CTI 033/06

N° Filter IFP EC89 EC90

Mass before impregnation (g) 1817 1877 1811

Mass after impre + Calcination IFP (g) 2156,4 2059,5 non calcined

Impregnated

Non

Mass after impre + Calcination CTI 500°C/2h00 (g) 2048,2

Masse addes cata in g 339,4 171,2

Volume of the filter in liter 2,47 2,50 2,47

Content cata in g/liter 137,41 68,48 0

Sight face

Sight cells ∆P - mb

Stream of air co-current to the direction of impregnation

Flow 100 m3/h 7 5 3

Flow 200 m3/h 16 12 9

Flow 300 m3/h 27 21 16

Stream of air against the current of the direction

of impregnation

Flow 100 m3/h 6 5 3

Flow 200 m3/h 15 13 9

Flow 300 m3/h 26 22 16

CTI - CONFIDENTIAL

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CTI - CONFIDENTIAL

PHOTO OF THE CTI’S DPF AFTER IMPREGNATION

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IMPREGNATIONMEB PHOTO

Total zeolith deposition is inside the pore. There is no layer at the surface. Porous cavity of the support are sometimes plugged by the zeolith depending

on the concentration.

68g/l 279g/l

3420/12/2006 B. Cartoixa CTI - CONFIDENTIAL

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IMPREGNATIONMEB PHOTO

68g/l 279g/l

Excellent catalyst penetration with partial plugging of some pores, depending of the slurry concentration

20/12/2006 B. Cartoixa CTI - CONFIDENTIAL

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200

300

600

ΔP

(mm

H2O

)

Débit air à 100 m3/h

Débit air à 200 m3/h

Débit air à 300 m3/h

36

CTI - CONFIDENTIAL

IMPREGNATION BACK PRESSURE MEASUREMENT

20/12/2006 B. Cartoixa

ΔP = f (wt% cata avec flux d'air à contre-courant de l'imprégnation)

0

100

400

500

0 50 100 150 200 250 300

wt% cata (g/l)

∆P

(mb)

10

20

30

40

50

60

Air flow 100m3/h

Air flow 200 m3/h

Air flow 300m3/h

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100

200

300

400

500

600

Débit air en m3/h

ΔP

(mm

H2O

)

37

CTI - CONFIDENTIAL

IMPREGNATION CHARACTERISATION DP

20/12/2006 B. Cartoixa

ΔP = f (débit d'air à contre-courant de l'imprégnation)

0 0 50 100 150 200 250 300 350

EC 88 257g/l

EC 89 137g/l

EC 90 68g/l

ref 0g/l

20

10

30

40

50

60

∆P

(mb)

Air flow in m3/h

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38

CTI - CONFIDENTIAL

190-230° C 250 - 300° C

• MOTOR BENCH TEST FOR ZEOLITH DeNOx DPF Content 137 g/l

Exhaust sytem schema

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temps

NOx EMISSION

BEFORE AND AFTER DPF

sans injection

injection d'air injection air + injection d'Urée

sans in jection d'air

injection d'air

1000

900

800

700

600

500

400

300

200

0 0 600 1200 1800 2400 3000 3600 4200 4800 5400 6000 6600 7200

émissions amont FAP

dilution

émissions aval FAP

rétention rétention

di+

lution

Time (s)

NO

x (p

pm)

CTI - CONFIDENTIAL

39

100

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EFFICACITE FAP ((NOx amont - NOx aval)/NOx amont)

temps

Effic

acité

FA

P (%

)

efficaciefficact

40

CTI - CONFIDENTIAL

0

10

20

30

40

50

60

70

80

90

100

0 600 1200 1800 2400 3000 3600 4200 4800 5400 6000 6600 7200

té réelle é relative

efficacité due à la dilution efficacité due à

la rétention

REAL AND RELATIVE EFFICIENCY

DPF NOx efficiency ((NOx amont – NOx aval))/NOx amont)

Efficien

cy F

AP

(%)

Real efficiency

Relative efficiency

Time (s)

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EVOLUTION DE LA PERTE DE CHARGE DU FAP

temps

41

CTI - CONFIDENTIAL

DELTA P EVOLUTION OF THE DPF

0

20

40

60

80

100

120

140

160

180

200

0 600 1200 1800 2400 3000 3600 4200 4800 5400 6000

(mba

r)

VVH 30000 VVH 66000

retour

∆P

Time (s)

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CTI rev3.0 CTI rev3.242

CTI - CONFIDENTIAL

PM / MVEG Cycle

0

0,001

0,002

0,003

0,004

0,005

0,006

CTI rev3.1

PM g/K

m PM EFFICIENCY OF THE PARTICULATE FILTER

(test made by IFP)

The CTI product when it is virgin (worst condition) is 3 to 4 time below the upper limit requested for Euro V in 2009 (SMPS test done by IFP).

EURO 5

CTI 20µ CTI 15µ CTI asymetric shape

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CONCLUSIONS

• The 3 different impregnation methods shows a real industrial potential for 4 way catalysistechnology or separatively CatOx + DPF DeNOxfunction.

• Today the most easy and cheapest method seems to be the slurry forcing technology (Patent IFP – CTI)

• CTI’s composite SiC product could be easilyimpregnated with catalyst with very low increaseof back pressure.

CTI - CONFIDENTIAL

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This work has been done with the financial support of the : French Research Ministry Predit VP008

convention 04K133 From june 2004 until june 2007 (Cti - Peugeot -Irma –Faurecia- Le moteur moderne Eft )

FSH (Fonds de soutien hydrocarbure) from 2001 until 2004 (A50004/01 – A59009/01)

(IFP –CTI)

CTI - CONFIDENTIAL

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CERAMIQUES TECHNIQUES ET INDUSTRIELLES S.A.

THANK YOU FOR YOUR ATTENTION

CERAMICS MANUFACTURER AS ENVIRONMENTALLY FRIENDLY

MATERIALS

C.T.I. S.A.La Resclause - Route de Saint Privat F 30340 SALINDRES - FRANCE E-mail: [email protected] Site internet: www.ctisa.fr

�: +33 (0) 4 66 85 88 70 Fax: +33 (0) 4 66 85 70 09 45

CTI - CONFIDENTIAL