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Studies in Surface Science and Catalysis 162
SCIENTIFIC BASES FOR THE PREPARATION
OF HETEROGENEOUS CATALYSTS
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Studies in Surface Science and Catalysis
Advisory Editors:B. Delmon and J.T. Yates
Series Editor: G. Centi
Vol. 162
SCIENTIFIC BASES FORTHE PREPARATION OFHETEROGENEOUS CATALYSTS
Proceedings of the 9thInternational Symposium,Louvain-la-Neuve, Belgium, September 10-14, 2006
Edited by
E.M. Gaigneaux*, M. Devillers*, D.E. De Vos**, S. Hermans*,
P.A. Jacobs**, J.A. Martens**, P. Ruiz*
* Universit Catholique de Louvain, Louvain-la-Neuve, Belgium** Katholieke Universiteit Leuven, Heverlee (Leuven), Belgium
Amsterdam Boston Heidelberg London New York Oxford Paris
San Diego San Francisco Singapore Sydney Tokyo
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ElsevierRadarweg 29, PO Box 211, 1000 AE Amsterdam, The NetherlandsThe Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, UK
First edition 2006
Copyright 2006 Elsevier B.V. All rights reserved
No part of this publication may be reproduced, stored in a retrieval systemor transmitted in any form or by any means electronic, mechanical, photocopying,recording or otherwise without the prior written permission of the publisher
Permissions may be sought directly from Elseviers Science & Technology RightsDepartment in Oxford, UK: phone (+44) (0) 1865 843830; fax (+44) (0) 1865 853333;
email: [email protected]. Alternatively you can submit your request online byvisiting the Elsevier web site at http://elsevier.com/locate/permissions, and selectingObtaining permission to use Elsevier material
NoticeNo responsibility is assumed by the publisher for any injury and/or damage to personsor property as a matter of products liability, negligence or otherwise, or from any useor operation of any methods, products, instructions or ideas contained in the materialherein. Because of rapid advances in the medical sciences, in particular, independentverification of diagnoses and drug dosages should be made
Library of Congress Cataloging-in-Publication Data
A catalog record for this book is available from the Library of Congress
British Library Cataloguing in Publication Data
A catalogue record for this book is available from the British Library
ISBN-13: 978-0-444-52827-8ISBN-10: 0-444-52827-XISSN: 0167-2991
For information on all Elsevier publicationsvisit our website at books.elsevier.com
Printed and bound in The Netherlands
06 07 08 09 10 10 9 8 7 6 5 4 3 2 1
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v
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vi Foreword
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Foreword vii
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viii Foreword
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ix
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xi
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xii Contents
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Contents xiii
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xiv Contents
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Contents xv
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xvi Contents
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Contents xvii
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xviii Contents
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Contents xix
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Contents xxi
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Scientific Bases for the Preparation of Heterogeneous Catalysts 1E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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2 U. Dingerdissen and D. Linke
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Scopes and limitations of high throughput preparation and screening tools 3
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4 U. Dingerdissen and D. Linke
PilotPlant
Plant
Classic Screening:10 /week
Main Screening: 100 /week
Evaluation Screening: >1000 /week
Exploration Screening: >1000 /day
rP
ce
onoisi
fD
aat
Num
re
b
fo
xE
p
re
mi
ne
tsF/
mro
ula
snoit
standard lab
HTSdomain
chemicalengineeringdomain
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Scopes and limitations of high throughput preparation and screening tools 5
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6 U. Dingerdissen and D. Linke
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Scopes and limitations of high throughput preparation and screening tools 7
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8 U. Dingerdissen and D. Linke
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Scopes and limitations of high throughput preparation and screening tools 9
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10 U. Dingerdissen and D. Linke
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Scopes and limitations of high throughput preparation and screening tools 11
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12 U. Dingerdissen and D. Linke
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Scientific Bases for the Preparation of Heterogeneous Catalysts 13E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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14 E. de la Rochefoucauld et al.
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Mesoporous alumina obtained by surface alumination of pure silica SBA-15 15
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16 E. de la Rochefoucauld et al.
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Mesoporous alumina obtained by surface alumination of pure silica SBA-15 17
1 2 3 4 52()
).u.a(
ytisnetnI
a)
b)
c)
d)e)
Figure 1
0
100
200
300
400
500
600
700
800
50
55
60
65
70
SBA Blank Iso1 Iso2 Iso3 Iso4
m(aeraecafruS
2
g.
1-)
)(rete
maideroP
Sample type
a)
b)
c)
Figure 2
-15
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18 E. de la Rochefoucauld et al.
-100-50050100
).u.a(ytisnetnI
(ppm)
Numberof graftings
306
54
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Mesoporous alumina obtained by surface alumination of pure silica SBA-15 19
0
0,5
1
1,5
2
2,5
0
2
4
6
8
10
% Al2O
3
01*ytivitcagnikcarcenemuC
4
h.lomm(
1-
m.
2-)
OoM
3
(yticapacnoisrepsid
m.lom
2-
)0
(SiO2)
15.1(Iso1)
24.1(Iso2)
30.0(Iso3)
35.0(Iso4)
100(Al
2O
3)
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20 E. de la Rochefoucauld et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 21E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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22 F. Klasovsky and P. Claus
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Biomimetic catalyst preparation with carbohydrates: The CHSG process 23
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24 F. Klasovsky and P. Claus
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Biomimetic catalyst preparation with carbohydrates: The CHSG process 25
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26 F. Klasovsky and P. Claus
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Biomimetic catalyst preparation with carbohydrates: The CHSG process 27
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28 F. Klasovsky and P. Claus
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Scientific Bases for the Preparation of Heterogeneous Catalysts 29E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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30 S. van Dommele et al.
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Synthesis of heterogeneous base catalysts: nitrogen containing carbon nanotubes 31
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32 S. van Dommele et al.
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Synthesis of heterogeneous base catalysts: nitrogen containing carbon nanotubes 33
Amount N
(mmol/g NCNT)sampleT
(K)
N/Csource
Tube diameter rangea
(nm)XPS Titration
NPb
(%)
NQc
(%)
Co823ACN 823 ACN 5 38 (16) 7.4 0.03 50 23
Co923ACN 923 ACN 4 52 (17) 4.0 0.03 36 36Co1023ACN 1023 ACN 5 50 (18) 4.3 0.02 28 44
Co923PYR 923 PYR 5 43 (18) 7.5 0.05 50 24
Co1023PYR 1023 PYR 40 86 (62) 7.4 0.02 40 27
Co1123PYR 1123 PYR - 5.8 0.02 25 28
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34 S. van Dommele et al.
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Synthesis of heterogeneous base catalysts: nitrogen containing carbon nanotubes 35
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38 I. Melin-Cabrera et al.
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Tooling up heterogeneous catalysis through Fentons chemistry... 39
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40 I. Melin-Cabrera et al.
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Tooling up heterogeneous catalysis through Fentons chemistry... 41
0 5 10 15 20 25 30 35 40 4520
40
60
80
- 3%
+ 3%
N2
ocO
vneris
no
/%
Time on stream / h
Stability test at 700 KFe-FER (citrate, 353 K, 1 h)
0 5 10 15 20 25 30 35 40 4520
40
60
80
+ 3%
N2
ocO
vneris
no
/%
Time on stream / h
Stability test at 700 KFe-FER (citrate, 353 K, 1 h)
550 600 650 700 750 800
0
20
40
60
80
100
N2O
vnoc
resion/%
Temperature /K
(A) (B)
0 5 10 15 20 25 30 35 40 4520
40
60
80
- 3%
+ 3%
N2
ocO
vneris
no
/%
Time on stream / h
Stability test at 700 KFe-FER (citrate, 353 K, 1 h)
0 5 10 15 20 25 30 35 40 4520
40
60
80
+ 3%
N2
ocO
vneris
no
/%
Time on stream / h
Stability test at 700 KFe-FER (citrate, 353 K, 1 h)
550 600 650 700 750 800
0
20
40
60
80
100
N2O
vnoc
resion/%
Temperature /K
(A) (B)
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42 I. Melin-Cabrera et al.
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Tooling up heterogeneous catalysis through Fentons chemistry... 43
333 K / [H2O2]=10%
H2O/CO2
Fe3+
/ H2O22(Cu K) / degree
Inetnsity
/a.u.
1 m
Fe
Fe
Fe
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44 I. Melin-Cabrera et al.
4 6 8 10 12 14 16 18 20
0.00
0.02
0.04
0.06
0.08
0.10
dV/dD
/
mc
3(/g
)
pore diameter (D) /
12 6.6 x 6.7** [001] 12 5.6 x 5.6*
4 6 8 10 12 14 16 18 20
0.00
0.02
0.04
0.06
0.08
0.10
dV/dD
/
mc
3(/g
)
pore diameter (D) /
12 6.6 x 6.7** [001] 12 5.6 x 5.6*
N2Ocovn
resion
/
%
658 683 708
One-potFe-BEA
Temperature / K
0
80
40
2.0Fe-BEA TOSOH
100
733
20
602.3Fe-BEA ZEOLYST
N2Ocovn
resion
/
%
658 683 708
One-potFe-BEA
Temperature / K
0
80
40
2.0Fe-BEA TOSOH
100
733
20
602.3Fe-BEA ZEOLYST
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48 A.I. Reyes de la Torre et al.
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Molybdenum and tungsten carbides supported on mesostructured MCM-41 49
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50 A.I. Reyes de la Torre et al.
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Molybdenum and tungsten carbides supported on mesostructured MCM-41 51
a b
Amorphous
MCM41-PAN-P
DiamondGraphite
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52 A.I. Reyes de la Torre et al.
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Molybdenum and tungsten carbides supported on mesostructured MCM-41 53
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54 A.I. Reyes de la Torre et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 55E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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56 S.-C. Han et al.
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Microwave and hydrothermal synthesis 57
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58 S.-C. Han et al.
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Microwave and hydrothermal synthesis 59
(a) (b)
(c) (d)
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60 S.-C. Han et al.
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Microwave and hydrothermal synthesis 61
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62 S.-C. Han et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 63E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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64 S. Naito et al.
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Preparation of hollow silica-Rh, -Ir, and -Rh-Ir-bimetallic nanocomposites... 65
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66 S. Naito et al.
437 573 673 773 873 973 1073 11730
10
20
30
40
50 100
80
60
40
20
0
Calcination Temperature / K
mn/retemaiD
m/aeraecafr
usTEB
2g1-
hollow
SiO2
437 573 673 773 873 973 1073 11730
10
20
30
40
50 100
80
60
40
20
0437 573 673 773 873 973 1073 11730
10
20
30
40
50 100
80
60
40
20
0
Calcination Temperature / K
mn/retemaiD
m/aeraecafr
usTEB
2g1-
hollow
SiO2
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Preparation of hollow silica-Rh, -Ir, and -Rh-Ir-bimetallic nanocomposites... 67
(A)
Calcination Temperature / K
473 673 873 10730
2
4
6
8
10
12
14
473 673 873 1073
(B)
mc/no
itprosdafotnuomA
3g1-
(A)
Calcination Temperature / K
473 673 873 10730
2
4
6
8
10
12
14
473 673 873 1073
(B)
mc/no
itprosdafotnuomA
3g1-
CO
CO
H2H2
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68 S. Naito et al.
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Preparation of hollow silica-Rh, -Ir, and -Rh-Ir-bimetallic nanocomposites... 69
Reaction Time / min Reaction Time / min
%/noisrevnoC
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70 S. Naito et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 71E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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72 G.M. Veith et al.
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The use of magnetron sputtering for the production of heterogeneous catalysts 73
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74 G.M. Veith et al.
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The use of magnetron sputtering for the production of heterogeneous catalysts 75
2 nm0
5
10
15
20
25
30
1 2 3 4 5 6 7 8 9
uoC
nt
1.37 wt% Auon -Al2O
3
Avg. Dia. = 2.29 nm
Dispersion = 49%= 0.75 nm
4 nm
nm
2 nm2 nm0
5
10
15
20
25
30
1 2 3 4 5 6 7 8 9
uoC
nt
1.37 wt% Auon -Al2O
3
Avg. Dia. = 2.29 nm
Dispersion = 49%= 0.75 nm
4 nm4 nm
nm
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76 G.M. Veith et al.
0
50
10 0
15 0
20 0
0 2 4 6 8 10 12 14 16 18 20 22
0.69 wt% Au on X40S via sputteringDispersion = 72.5%242 data points
Avg. Dia. = 1.72 nm *
*Does not include single atoms= 0.61 nm
nm
1.5 nm
0
50
10 0
15 0
20 0
0 2 4 6 8 10 12 14 16 18 20 22
0.69 wt% Au on X40S via sputteringDispersion = 72.5%242 data points
Avg. Dia. = 1.72 nm *
*Does not include single atoms= 0.61 nm
nm
1.5 nm
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The use of magnetron sputtering for the production of heterogeneous catalysts 77
0
20
40
60
80
0.5 1 1.5 2 2.5 3 3.5 4 4.5 5
11.1 wt% Pt on Vulcan XC72Avg. Pt size = 1.62 nm= 0.49 nmDispersion = 72%
nm nm
0
4
8
12
1620
24
28
0.5 1 1.5 2 2.5 3 3.5 4 4.5 5
Avg. Pt size = 2.57 nm = 0.79 nmDispersion = 53%
E-TEK 20 wt% Pt on Vulcan XC72
0
20
40
60
80
0.5 1 1.5 2 2.5 3 3.5 4 4.5 5
11.1 wt% Pt on Vulcan XC72Avg. Pt size = 1.62 nm= 0.49 nmDispersion = 72%
nm nm
0
4
8
12
1620
24
28
0.5 1 1.5 2 2.5 3 3.5 4 4.5 5
Avg. Pt size = 2.57 nm = 0.79 nmDispersion = 53%
E-TEK 20 wt% Pt on Vulcan XC72
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80 A. Deffernez et al.
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Preparation of carbon-supported Pd and Au-Pd catalysts 81
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82 A. Deffernez et al.
0
20
40
60
80
100
0 2 4 6 8 10 12 14
pH
)%(C
nodebrosdadPfotnuomA
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Preparation of carbon-supported Pd and Au-Pd catalysts 83
0
0.4
0.8
1.2
1.6
2
0 2 4 6 8 10 12 14
pH
)001*(S
PXybden
i
mretedC/uA
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84 A. Deffernez et al.
0
10
20
30
40
50
60
70
80
90
100
0 2 4 6 8 10 12 14pH
)%(no
itcarF
[Pd(H2O)4]2+
[Pd(OH)(H2O)3]+
[Pd(OH)2(H2O)2]
[Pd(OH)3(H2O)]-
[Pd(OH)4]2-
0
10
20
30
40
50
60
7080
90
100
0 2 4 6 8 10 12 14
pH
)%(noitcarF
[AuCl4]-
[AuCl3(OH)]-
[AuCl2(OH)2]-
[AuCl(OH)3]-
[Au(OH)4]-
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Preparation of carbon-supported Pd and Au-Pd catalysts 85
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86 A. Deffernez et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 87E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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88 P. Mki-Arvela et al.
H2O O
Citral Citronellal 3,7-dimethyloctanal
OH2
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Supported ionic liquid catalyst (SILCA) in the hydrogenation of citral 89
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90 P. Mki-Arvela et al.
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Supported ionic liquid catalyst (SILCA) in the hydrogenation of citral 91
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92 P. Mki-Arvela et al.
0
2
4
6
8
10
0 50 100 150 200 250 300
bulk*time(g/dm3*min)
noC
rev
%(nois
)/mgdP
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Supported ionic liquid catalyst (SILCA) in the hydrogenation of citral 93
0
10
20
30
40
50
0 50 100 150 200 250 300
bulk*time (g/dm3*min)
)%(noisrevnoC
a)
b)
0
10
20
30
40
50
0 10 20 30 40 5
Conversion (%)
eS
elctiv
yti
ot
cirtoneall
(l%)
0
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94 P. Mki-Arvela et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 95E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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96 J.R.A. Sietsma et al.
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Ordered mesoporous model supports as a tool to study catalyst preparation 97
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98 J.R.A. Sietsma et al.
(b)(a)
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Ordered mesoporous model supports as a tool to study catalyst preparation 99
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100 J.R.A. Sietsma et al.
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Ordered mesoporous model supports as a tool to study catalyst preparation 101
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102 J.R.A. Sietsma et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 103E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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104 S.L. Soled et al.
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Supported metal catalysts: some interesting new leads in an old field 105
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106 S.L. Soled et al.
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108 S.L. Soled et al.
100 150 200 250 300 350 400 450
temperature (deg C)
-20
-18
-16
-14
-12
-10
-8
-6
-4
-2
0
%wtchange
0
5E-010
1E-009
1.5E-009
2E-009
2.5E-009
MSsignal:CO2
0
2E-012
4E-012
6E-012
8E-012
1E-011
1.2E-011
1.4E-011
MS
signal:NO2,H2O
LegendTGCO2NO2H2O
TG
H2O
NO2 CO2
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Supported metal catalysts: some interesting new leads in an old field 109
0
20
40
60
80
100xH/Ru(
combined)@
40C
250 300 350reduction temperature (C)reduction temperature (C)
400150 200
aq, no TEA, dried 100C
TEA calc 275C
hr
TEA calc 400C
aq, calc300C
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110 S.L. Soled et al.
CM200 FEG
20.00 nm
RuRu
Reduction at 150C, 3h, then 400C, 9h
20nm
Reduction at 150 C, 3h
20nm
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Scientific Bases for the Preparation of Heterogeneous Catalysts 111E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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112 N. Job et al.
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Metal catalysts supported on texture-tailored carbon xerogels 113
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114 N. Job et al.
0
0.5
1
1.5
2
2.5
3 4 5 6 7
pH
)g/mc(emuloveroplatoT
1
10
100
1000
)mn(eziseropnaeM
(b)(a)
pH = 6.25
pH = 5.25
10 m1 m
pH = 4.00pH = 6.00
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Metal catalysts supported on texture-tailored carbon xerogels 115
(b)
~1 nm
10 nm
(a)
20 nm
~5
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116 N. Job et al.
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Metal catalysts supported on texture-tailored carbon xerogels 117
0
0.25
0.5
0.75
1
0 300 600 900 1200
Pellet size (m)
)-(rotcafssenevitceffE
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118 N. Job et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 119E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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120 E.M. Sulman et al.
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Novel nano catalysts on the base of hypercrosslinked polystyrene.. . 121
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122 E.M. Sulman et al.
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Novel nano catalysts on the base of hypercrosslinked polystyrene.. . 123
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124 E.M. Sulman et al.
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Novel nano catalysts on the base of hypercrosslinked polystyrene.. . 125
0 50 100 150 200 2500.00
0.02
0.04
0.06
ABL
oc
ncenrt
ita
on,m
ol/l
time, min
Pd(5%)/HPS "beads"Pd(5%)/HPS d < 0,063
0 100 200-200
-100
0
10 0
m,E
V
time, min
0 50 100 150 200-300
-200
-100
0
100
Vm,E
time, min
0 50 100 150 2000.00
0.02
0.04
BL.cnoC
,A
l/lom
time, min
HPS Pd(1%) d < 0,063
HPS Pd(3%) d < 0,063HPS Pd(5%) d < 0,063
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126 E.M. Sulman et al.
0.0 0.1 0.2 0.3 0.4 0.50.0
0.2
0.4
0.6
0.8
1.0LBA
eS
tcel
tivi
y
Conversion
HPS Pd(1%) d < 0,063
HPS Pd(3%) d < 0,063
HPS Pd(5%) d < 0,063
2-keto-LBA
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128 V. Caps et al.
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Effect of the titania morphology on the preparation of Au/TiO2(/SiO2) catalysts 129
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130 V. Caps et al.
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Effect of the titania morphology on the preparation of Au/TiO2(/SiO2) catalysts 131
a b
c d
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132 V. Caps et al.
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Effect of the titania morphology on the preparation of Au/TiO2(/SiO2) catalysts 133
a
b
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134 V. Caps et al.
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136 M.V. Twigg and J.T. Richardson
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Structured ceramic foams as catalyst supports 137
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138 M.V. Twigg and J.T. Richardson
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Structured ceramic foams as catalyst supports 139
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140 M.V. Twigg and J.T. Richardson
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Structured ceramic foams as catalyst supports 141
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142 M.V. Twigg and J.T. Richardson
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Scientific Bases for the Preparation of Heterogeneous Catalysts 143E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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144 J. Tsou et al.
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Preparation of monolithic catalysts for hydrodesulfurization 145
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146 J. Tsou et al.
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Preparation of monolithic catalysts for hydrodesulfurization 147
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Preparation of monolithic catalysts for hydrodesulfurization 149
dc
ba
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150 J. Tsou et al.
0
10
20
30
40
50
60
70
80
0 10 20 30 40
Mo + Ni (wt%)
(kcm
3s//g
em
tal)
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Structured TiO2based catalysts for clean water technologies 153
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154 C.G. Silva et al.
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Structured TiO2based catalysts for clean water technologies 155
(a) (b)
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156 C.G. Silva et al.
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Structured TiO2based catalysts for clean water technologies 157
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158 C.G. Silva et al.
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160 J. Blanco et al.
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Single-step synthesis of porous supported catalysts 161
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162 J. Blanco et al.
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Single-step synthesis of porous supported catalysts 163
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164 J. Blanco et al.
(b)intensity
Mg
Si
Ti
Pt
0.0mm
1.00.5
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Single-step synthesis of porous supported catalysts 165
0
25
50
75
100
100 200 300 400 500
Temperature, C
To
%lo
m,.vnoceneul
Pt/sepiolite ICP
Pt/sep.Al2O3
Pt/sep.Al2O3 ICP
Pt/sep.TiO2
Pt/sep.TiO2 ICP 0
25
50
75
100
100 200 300 400 500
Temperature, C
,1
id2
hclorteo
ena
h
conv
m,.
o%l
(a) (b)
Extrudates
Pt/sep.TiO2ICP
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168 O. Muraza et al.
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Preparation and characterization of bimetallic catalysts... 169
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170 O. Muraza et al.
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Preparation and characterization of bimetallic catalysts... 171
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172 O. Muraza et al.
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Preparation and characterization of bimetallic catalysts... 173
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174 O. Muraza et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 175E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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176 J.A. Bergwerff et al.
Wavenumber /cm-1
Mo-OstretchNO3
-
RamanandUV-Vis measurements
impregnation
drying
calcination
cutpellet
OMo6+ CT
Co2+ d-d
transitions
Ramanshift/cm-140000 30000 20000 10000 700 800 900 1000 1100
bA
s.
0
0.5
1.0
1.5
2.0
RF-coilVolumefrom whichsignalis detected
impregnation
1Himage
-Al2O3extrudate
-Al2O3pellet
31Pimage
MagneticResonance Imaging
Wavenumber /cm-1
Mo-OstretchNO3
-
RamanandUV-Vis measurements
impregnation
drying
calcination
cutpellet
OMo6+ CT
Co2+ d-d
transitions
Ramanshift/cm-140000 30000 20000 10000 700 800 900 1000 1100
bA
s.
0
0.5
1.0
1.5
2.0
RF-coilVolumefrom whichsignalis detected
impregnation
1Himage
-Al2O3extrudate
-Al2O3pellet
31Pimage
MagneticResonance Imaging
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Monitoring the preparation of (Co)Mo/Al2O3extrudates. .. 177
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178 J.A. Bergwerff et al.
30 min
c
a
c
b
Raman shift (cm-1)
ON
3-
09
1
49
4 168
a
bb
c
b
a
c
ON
3-
Raman shift (cm-1)
109
49
4168
a
b
c
b
a
c
ON
3-
Raman shift (cm-1)
109
49
4168
aa
bb
I ( MoO2t)I (NO3-)
12
6
4
2
0
10
8I ( MoO2t)
I (NO3-)
12
6
4
2
0
10
8180 min
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Monitoring the preparation of (Co)Mo/Al2O3extrudates. .. 179
c
a
b
c
b
a
Raman shift (cm-1)
099
518
482
266 73
2
33337
3
a
b
c
Raman shift (cm-1)
765
153
998
749
69
8
049O
N
3-
After impregnation After calcinationI (816 cm-1)
6000
3000
20001000
0
5000
4000
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180 J.A. Bergwerff et al.
flexiblelatex seal
Movable platform(computer -controlled)
latex seal
ovable platform(computer -controlled)
optical fiber
sample holder
sample holder
environmental cell
pellet
environmental cell UV -Vis probe
pellet
pellet
flexiblelatex seal
ovable platform(computer -controlled)
latex seal
ovable platform(computer -controlled)
optical fiber
sample holder
sample holder
environmental cell
pellet
environmental cell UV -Vis probe
pellet
pellet
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Monitoring the preparation of (Co)Mo/Al2O3extrudates. .. 181
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182 J.A. Bergwerff et al.
15 min 180 min
19300
Wavenumber (cm-1)Wavenumber (cm-1)
17600
40000 30000 20000 10000 40000 30000 20000 10000
1.0 1.0
0.6
0.4
0.2
0
0.8 0.8
0.6
0.4
0.2
0
sbA
.bA
.s
Wavenumber (cm-1)Wavenumber (cm-1)
240 min15 min
17600
40000 30000 20000 10000
00
0.40.4
0.80.8
1.2 1.2
sbA
.bA
.s
40000 30000 20000 10000
CoMoP(0.1) CoMoP(0.3)CA(0.2)
1.4 mm
0.7 mm
0 mm
15 min 180 min
19300
Wavenumber (cm-1)Wavenumber (cm-1)
17600
40000 30000 20000 10000 40000 30000 20000 10000
1.0 1.0
0.6
0.4
0.2
0
0.8 0.8
0.6
0.4
0.2
0
sbA
.bA
.s
Wavenumber (cm-1)Wavenumber (cm-1)
240 min15 min
17600
40000 30000 20000 10000
00
0.40.4
0.80.8
1.2 1.2
sbA
.bA
.s
40000 30000 20000 10000
CoMoP(0.1) CoMoP(0.3)CA(0.2)15 min 180 min
19300
Wavenumber (cm-1)Wavenumber (cm-1)
17600
40000 30000 20000 10000 40000 30000 20000 10000
1.0 1.0
0.6
0.4
0.2
0
0.8 0.8
0.6
0.4
0.2
0
sbA
.bA
.s
Wavenumber (cm-1)Wavenumber (cm-1)
240 min15 min
17600
40000 30000 20000 10000
00
0.40.4
0.80.8
1.2 1.2
sbA
.bA
.s
40000 30000 20000 10000
CoMoP(0.1) CoMoP(0.3)CA(0.2)
1.4 mm
0.7 mm
0 mm
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184 J.A. Bergwerff et al.
a. d.c.b.
h. i.g. k.j.
f.e.
l.
a. d.c.b.
h. i.g. k.j.
f.e.
l.
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Monitoring the preparation of (Co)Mo/Al2O3extrudates. .. 185
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186 J.A. Bergwerff et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 187E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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188 R. Prada Silvy et al.
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Parameters controlling the scaling-up of a V-Al oxynitride catalyst 189
020406080
NOPrZ
lAV
NO
lA
NOPaG l
A
NOPrC
lA
NOP
NOPrZaG
NOiT
C3 conversion ACN selectivity ACN yield
)%(
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Parameters controlling the scaling-up of a V-Al oxynitride catalyst 191
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192 R. Prada Silvy et al.
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194 R. Prada Silvy et al.
0
1020
30
40
50
60
70
50 g 100 g 1 kg
C3 conversion ACN selectivity COx selectivity
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Scientific Bases for the Preparation of Heterogeneous Catalysts 195E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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196 T. Cukic et al.
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Approaching the preparation of Pd-Al2O3catalyst systematically 197
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198 T. Cukic et al.
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Approaching the preparation of Pd-Al2O3catalyst systematically 199
n pH ti Vi/Vp sd Td td sc Tc tc0
Calcination
Exp errorestimate
Impregnation Drying
n pH ti Vi/Vp sd Td td sc Tc
eva
rage
nahc
eg
of
i
datub
eneconv
sre
ion,[-]
Calcination
0.05
0.10
0.15
0.20
0.25
n pH ti Vi/Vp sd Td td sc Tc tc0
Calcination
Exp errorestimate
Impregnation Drying
n pH ti Vi/Vp sd Td td sc Tc
eva
rage
nahc
eg
of
i
datub
eneconv
sre
ion,[-]
Calcination
0.05
0.10
0.15
0.20
0.25
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200 T. Cukic et al.
0 10 20 30 40 50 600.0
0.2
0.4
0.6
0.8
1.0
tuB
aid
ne
vnoce
re
oisn
[-]
Vi/Vp
0 10 20 30 40 50 600.0
0.2
0.4
0.6
0.8
1.0
tuB
aid
ocene
oisrevn
]-[,n
Vi/Vp
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Approaching the preparation of Pd-Al2O3catalyst systematically 201
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202 T. Cukic et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 203E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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204 F. Patcas and W. Krysmann
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Design and preparation of controlled porous oxidic structures on metallic substrates 205
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206 F. Patcas and W. Krysmann
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Design and preparation of controlled porous oxidic structures on metallic substrates 207
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208 F. Patcas and W. Krysmann
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Design and preparation of controlled porous oxidic structures on metallic substrates 209
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210 F. Patcas and W. Krysmann
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212 L. Jiao et al.
0
0.2
0.4
0.6
0.8
1
0 2 4 6 8 10 12 14pH Final
(de
bros
da
tP
m/lom
2) L90
M7D
EH5
VN3S
FK300
Model
OH2+
O-
pHPZC
OHPZC
K1
K2
[PtCl6]-2
[(NH3)4Pt]+2
[H]+
(pH shifts)
Kads
Kads
OH2+
O-
pHPZC
OHOHPZC
K1
K2
[PtCl6]-2
[(NH3)4Pt]+2
[H]+
(pH shifts)
Kads
Kads
0
2
4
6
8
10
12
14
0 2 4 6 8 10 12 14
pH Initial
laniFHp
L90
M-7D
EH-5
VN-3S
FK300Model
H2
d. Reduce to retain
high dispersion
b. PZC determination
20 nm
c. Uptake pH survey
a. Mechanism
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Simple, scientific syntheses with common catalyst precursors 213
0
0.2
0.4
0.6
0.8
1
1.2
1.4
0 2 4 6 8 10 12 14
pH final
)2
^m/lomu(ekatpulateM
Tetraammine Pd
0
0.5
1
1.5
2
2.5
3
0 2 4 6 8 10 12 14
pH final
)2
^m/lomu(ekatpulateM
Self-preparedtetraammine Cu
Purchased
tetraammine Cu
SEA at pH 11: SEA at pH 11:DI: DI:
a) b)
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214 L. Jiao et al.
0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
1.8
2
0 2 4 6 8 10 12 14
pH
(ammaG
m/lom
2)
SX4 SXU SX2 VXC
E250 E350
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0 2 4 6 8 10 12 14
pH finals
tisneDe
cafruS
y(m
m/lo
2)
S51 KB Asbury Timrex
SEA at pH 2.9:DI: DI:
a) b)
SEA at pH 12:
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Simple, scientific syntheses with common catalyst precursors 215
-300
-200
-100
0
100
200
300
0 2 4 6 8 10 12 14pH final
(Vm
)
H H H H H H
+ +
--
PZ
cobalt oxide or
alumina
oxidized carbon
or niobia
-
O-
O-
O-
O-
OH2+ OH2
+ OH2+OH2
+
[PtCl6]-2
[(NH3)4Pt]+2
O-
O-
O-
O-
OH2+ OH2
+ OH2+OH2
+
[PtCl6]-2
[(NH3)4Pt]+2
+
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216 L. Jiao et al.
area Al,
wt%Nb,
wt%Pt,
wt%4-1 0.1 58.9 41
4-2 99.6 0.4 0
4-3 16.5 76.2 7.3
4-4 97.8 1.3 0.9
4-5 0.6 70.6 28.8
4-6 0 58.6 41.4
b)
c)
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
1.1
1.2
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
pH final
,
m/lom
2
.
PTA on Niobia
PTA on Alumina
PTA on Niobia+Alumina
model-PTAonNb
model-PTAonAl
model-PTA on mixture
model-PTA on Nb in mixture
model-PTA on Al in mixture
a)
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Simple, scientific syntheses with common catalyst precursors 217
0.02
0.04
0.06
0 1 2 3 4 5
R []
Pt foil (Pt-Pt)NPt-Pt= 12,R = 2.77
Pt-CoNPt-Co= 7.8,
R = 2.55
0
2
4
6
8
10
12
0 100 200 300 400 500 600 700
Temp (deg C)
%2H CPA/(Co3O4/SiO2)
CPA/Co3O4
CPA/SiO2 x 10
Co3O4
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Scientific Bases for the Preparation of Heterogeneous Catalysts 219E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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220 Z.-R. Tang et al.
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Preparation of TiO2using supercritical CO2antisolvent precipitation (SAS) 221
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224 Z.-R. Tang et al.
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Preparation of TiO2using supercritical CO2antisolvent precipitation (SAS) 225
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226 Z.-R. Tang et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 227E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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Clean transesterification of -ketoesters catalyzed by hybrid silica sol-gel 229
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230 G. Sathicq et al.
a)
b)
c) d)
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Clean transesterification of -ketoesters catalyzed by hybrid silica sol-gel 231
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Clean transesterification of -ketoesters catalyzed by hybrid silica sol-gel 233
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Scientific Bases for the Preparation of Heterogeneous Catalysts 235E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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Development of tools and methods for high-throughput preparation... 237
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238 R.W. Mayer et al.
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Development of tools and methods for high-throughput preparation... 239
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240 R.W. Mayer et al.
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Development of tools and methods for high-throughput preparation... 241
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242 R.W. Mayer et al.
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Scientific Bases for the Preparation of Heterogeneous Catalysts 243E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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244 F. Cambier
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Production of catalysts with an inductive atmospheric plasma torch 245
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246 F. Cambier
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Production of catalysts with an inductive atmospheric plasma torch 247
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248 F. Cambier
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Production of catalysts with an inductive atmospheric plasma torch 249
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250 F. Cambier
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Scientific Bases for the Preparation of Heterogeneous Catalysts 251E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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252 K. Bourikas et al.
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Investigation of the mode of interfacial deposition. .. 253
1 20 Diffuselayer
Specifically adsorbed anions(disubstituted and monosubstituted
inner-sphere complexes)
Electrolyte hydrated cations
Electrolyte counter ions(solvated anions)
Secondarywater layer
Primarywater layerSurface
oxygens
Metal ions
Metal oxide surface(positively charged)
1 20 Diffuselayer
Specifically adsorbed anions(disubstituted and monosubstituted
inner-sphere complexes)
Electrolyte hydrated cations
Electrolyte counter ions(solvated anions)
Secondarywater layer
Primarywater layerSurface
oxygens
Metal ions
Metal oxide surface(positively charged)
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254 K. Bourikas et al.
10-6M Mo
10-5M Mo
10-4M Mo
-3,5
-2,5
-1,5
-0,5
0,5
4 5 6 7 8 9 10 11pH
go
l
mlom/
2-
pzcTiO2= 6.5
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Investigation of the mode of interfacial deposition. .. 255
4
4.5
5
5.5
6
0 0.004 0.008 0.012 0.016CMo, total/ mol l
-1
Hp
pHinitial
pHfinal
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256 K. Bourikas et al.
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Investigation of the mode of interfacial deposition. .. 257
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Scientific Bases for the Preparation of Heterogeneous Catalysts 259E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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260 B.C. Gagea et al.
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Synthesis and characterization of nanocrystal zeolite/mesoporous matrix... 261
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262 B.C. Gagea et al.
4 h
8h 4 h
7h
A B
DC
E F
HG
I 4 h4 h
8hh 4 h4 h
7hh
A B
DC
E F
HG
I
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Synthesis and characterization of nanocrystal zeolite/mesoporous matrix... 263
300500700900110013001500
wavelenght(cm-1)
SG (24h)
nanoZSM-5
0 10 20 30 40 50
2theta
nanoZSM-5
SG (24h)
XRD FT-IR
300500700900110013001500
wavelenght(cm-1)
SG (24h)
nanoZSM-5
0 10 20 30 40 50
2theta
nanoZSM-5
SG (24h)
300500700900110013001500
wavelenght(cm-1)
SG (24h)
nanoZSM-5
SG (24h)
nanoZSM-5
0 10 20 30 40 50
2theta
nanoZSM-5
SG (24h)
0 10 20 30 40 50
2theta
nanoZSM-5
SG (24h)
XRD FT-IR
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264 B.C. Gagea et al.
0
200
400
600
800
1000
0 0.2 0.4 0.6 0.8 1
Relative Pressure (P/Po)
Qu
n
a
ittyAdsorbde
c(mg/STP)
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0 5 10 15 20 25 30
Pore Width (nm)
PoerVoulme(cmg/nm)
SG (24h)
nanoZSM-5
SG (24h)
0
200
400
600
800
1000
0 0.2 0.4 0.6 0.8 1
Relative Pressure (P/Po)
Qu
n
a
ittyAdsorbde
c(mg/STP)
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0 5 10 15 20 25 30
Pore Width (nm)
PoerVoulme(cmg/nm)
SG (24h)
nanoZSM-5
0
200
400
600
800
1000
0 0.2 0.4 0.6 0.8 1
Relative Pressure (P/Po)
Qu
n
a
ittyAdsorbde
c(mg/STP)
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0 5 10 15 20 25 30
Pore Width (nm)
PoerVoulme(cmg/nm)
0
200
400
600
800
1000
0 0.2 0.4 0.6 0.8 1
Relative Pressure (P/Po)
Qu
n
a
ittyAdsorbde
c(mg/STP)
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0 5 10 15 20 25 30
Pore Width (nm)
PoerVoulme(cmg/nm)
SG (24h)
nanoZSM-5
SG (24h)
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Synthesis and characterization of nanocrystal zeolite/mesoporous matrix... 265
0
20
40
60
80
100
170 190 210 230 250
Temperature (C)
Covnersio
(
n
)
SG (0h)
SG (7h)
SG (8h)
SG (10h)
SG (14h)
SG (24h)
SG (48h)
nanoZSM-50
20
40
60
80
100
0 10 20 30 40 50 60
Heating Time(h)
Conv
sre
ion
(
)
0
20
40
60
80
100
170 190 210 230 250
Temperature (C)
%
SG (0h)
SG (7h)
SG (8h)
SG (10h)
SG (14h)
SG (24h)
SG (48h)
nanoZSM-50
20
40
60
80
100
0 10 20 30 40 50 60
Heating Time(h)
%
0
10
20
30
40
50
60
70
80
90
100
0 20 40 60 80 100
Conversion ( )
i
Yeld()
total isomersdibranched isomers
cracked products
0
10
20
30
40
50
60
0 20 40 60 80
Conversion ( )
i
Yeld()
100
5+4 methyl-nonane
2 methyl-nonane
3 methyl nonane
0
10
20
30
40
50
60
0 2 4 6 8 10
Carbon number
mol.arc
ckdeprdouct/100mols
cracek
nd-decaen
A B
C
0
10
20
30
40
50
60
70
80
90
100
0 20 40 60 80 100
Conversion ( )
i
Yeld
total isomersdibranched isomers
cracked products
0
10
20
30
40
50
60
0 20 40 60 80
Conversion ( )
i
Yeld
100
5+4 methyl-nonane
2 methyl-nonane
3 methyl nonane
0
10
20
30
40
50
60
0 2 4 6 8 10
Carbon number
mol.arc
ckdeprdouct/100mols
cracek
nd-decaen
0
10
20
30
40
50
60
70
80
90
100
0 20 40 60 80 100
Conversion%
i
Yeld%
total isomersdibranched isomers
cracked products
0
10
20
30
40
50
60
0 20 40 60 80
Conversion%
i
Yeld%
100
5+4 methyl-nonane
2 methyl-nonane
3 methyl nonane
0
10
20
30
40
50
60
0 2 4 6 8 10
Carbon number
mol.arc
ckdeprdouct/100mols
cracek
nd-decaen
A B
C
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268 J.C. Groen et al.
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On the role of iron in preparation of mesoporous Fe-MFI zeolites via desilication 269
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270 J.C. Groen et al.
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On the role of iron in preparation of mesoporous Fe-MFI zeolites via desilication 271
1 10
Pore diameter / nm
dVd/logd
mc/
3g
1-
1.0
Z25-at
Z35-at
Z200-at
FeS-at
20 40 60 80 200 400 600 800 10000
50
100
150
200
S
em
os
m/
2
g1-
Molar Si/M3+ ratio / -
(Si/Al)optimal
FeS-at
(a) (b)
100
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On the role of iron in preparation of mesoporous Fe-MFI zeolites via desilication 273
0
50
100
150
200
0 0.30 0.50 1.10
Fe loading / wt.%
S
emso
m/
2g1-
0
1000
2000
3000
4000
iS[
]ftlirate
gm/
l1-
Z25
Fems-Z25
Fes-Z25
Fem-Z25
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276 N. Nishiyama et al.
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Selective formation of p-xylene over single crystal-like zeolite composite 277
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278 N. Nishiyama et al.
0
20
40
60
80
100
0.0 2.0 4.0 6.0
Conversion [%]
ap
ras-
le
itce
viyt
%[
]
:uncoated
coated
: x= 0.0
: x= 0.12
: x= 0.24
0
20
40
60
80
100
0.0 2.0 4.0 6.0
Conversion [%]
ap
ras-
le
itce
viyt
%[
]
:uncoated
coated
: x= 0.0
: x= 0.12
: x= 0.24
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Selective formation of p-xylene over single crystal-like zeolite composite 279
0
20
40
60
80
100
0 60 120 180 240
Time-on-stream [min]
Co
vn
oisre
n
]%[
0
20
40
60
80
100
ap
ar-s
ele
cvit
iyt
]%[
0
20
40
60
80
100
0 60 120 180 240
Time-on-stream [min]
Co
vn
oisre
n
]%[
0
20
40
60
80
100
ap
ar-s
ele
cvit
iyt
]%[
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280 N. Nishiyama et al.
Time-on-stream [min]
C
o
vn
oisre
[n
%]
ap
ar-s
leec
tiv
iyt
%[
]
0
20
40
60
80
100
0 120 240 360 480
0
20
40
60
80
100
Time-on-stream [min]
C
o
vn
oisre
[n
%]
ap
ar-s
leec
tiv
iyt
%[
]
0
20
40
60
80
100
0 120 240 360 480
0
20
40
60
80
100
W/F [kg-catalyst/(mol/h)]
Co
vn
re
ison[%]
ap
ar
-sle
ce
itvity[%]
0
20
40
60
80
100
0 0.1 0.2 0.3
0
20
40
60
80
100
W/F [kg-catalyst/(mol/h)]
Co
vn
re
ison[%]
ap
ar
-sle
ce
itvity[%]
0
20
40
60
80
100
0 0.1 0.2 0.3
0
20
40
60
80
100
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0
20
40
60
80
100
0 120 240 360 480
Time-on-stream [min]
Co
vn
re
ois
n[%
]
0
20
40
60
80
100
ap
ar
s-electiviyt
]%[
0
20
40
60
80
100
0 120 240 360 480
Time-on-stream [min]
Co
vn
re
ois
n[%
]
0
20
40
60
80
100
ap
ar
s-electiviyt
]%[
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Control of the basic sites strength by adjusting the active species dispersion 285
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0,0 0,5 1,0 1,5 2,0 2,5
0
20
40
60
80
100
120
140
160
Jk(Q
/mol)
CO2adsorbed (mol/m2)
KF/-aluminaKF/-aluminaMgLa mixed oxide
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20 40 60 80
La(OH)3
In
net
syti
(a.
).u
Mg(OH)2
La2(CO
3)
2(OH)
2
Two Theta (degree)
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0
5
35
30
1) without SO2 2) with SO23) without SO2
25
20
15
10mgNOg/
cat
KNO3 + 2%
Cu/ZrS
KNO3 + 5%
Cu/ZrS
Pt-Ba-
Al2O3
0 10 20 30 40 500
20
40
60
80
100
120
2% Cu / ZrSPt / -Al
2O
3
5% Cu / ZrS
Qidffk(J/m
o)l
CO2adsorbed (mol/g)
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Scientific Bases for the Preparation of Heterogeneous Catalysts 291E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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292 B. Fremon et al.
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294 B. Fremon et al.
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A new approach of hydrotreating catalysts preparation... 295
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296 B. Fremon et al.
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A new approach of hydrotreating catalysts preparation... 297
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Scientific Bases for the Preparation of Heterogeneous Catalysts 299E.M. Gaigneaux et al. (Editors) 2006 Elsevier B.V. All rights reserved.
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300 M. Cozzolino et al.
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Preparation, characterization and catalytic performances... 301
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100 200 300 400 500
20TS-D
7.30TS-I
7.62TS-D
17.8TS-Tol
3.09T/S-D
S
i
ang
l
yrarti
bra(
)sti
nu
Temperature(C)
0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.14 0.160.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
2.2
Ii
T
I/i
S
nTi/n
Si
ITi/I
Siexp Dioxane
ITi/I
Siexp Toluene
ITi/I
Siexp Isopropanol
ITi/I
Sicalculated byKerkhof and Moulijn model
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Preparation, characterization and catalytic performances... 303
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0 5 10 15 200
10
20
30
40
50
60
70
80
90
100
TiO2/SiO
2in Dioxane
TiO2/SiO
2in Isopropanol
TiO2/SiO
2in Toluene
YAF
ME
%,
%wt TiO2
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306 M. Cozzolino et al.