PdZn/Mg(Al)(Pd)(Zn)O x for ethanol conversion:
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1 EUROPACAT 2017, FIRENZE, AUGUST PdZn/Mg(Al)(Pd)(Zn)O x for ethanol conversion: reconstruction of the active phase upon a water containing feed J. De Waele, V.V. Galvita, H. Poelman, J.W. Thybaut Laboratory for Chemical Technology
2 Acetaldehyde as platform molecule 1
3 Acetaldehyde as platform molecule 1
4 Acetaldehyde as platform molecule 1
5 Acetaldehyde as platform molecule 1
6 Acetaldehyde as platform molecule 1
7 Acetaldehyde as platform molecule and many more 1
8 Acetaldehyde as platform molecule and many more 1
9 Acetaldehyde as platform molecule and many more 1
10 Production from bio-ethanol O 2 H 2 O Metal oxide catalyst Ethanol Acetaldehyde 2
11 Production from bio-ethanol O 2 H 2 O Metal oxide catalyst Ethanol Metal catalyst Acetaldehyde H 2 2
12 Production from bio-ethanol O 2 H 2 O Metal oxide catalyst Ethanol Metal catalyst Acetaldehyde H 2 2
13 Overview 3
14 Overview 3
15 Overview 3
16 Cu catalysts give high acetaldehyde selectivity S Ac H 2 Ethanol Acetaldehyde 4
17 Cu catalysts give high acetaldehyde selectivity S Ac H 2 Ethanol Acetaldehyde but sintering is a well-known problem. 4
18 PdZn has similar electronic properties as Cu A. Pang Tsai et al., J. Phys. Soc. Jpn., 2004, 73,
19 PdZn has similar electronic properties as Cu and Zn prevents the Pd-atoms from sintering. A. Pang Tsai et al., J. Phys. Soc. Jpn., 2004, 73,
20 J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. PdZn/Mg(Al)(Pd)(Zn)O x synthesis via co-precipitation (1wt% Pd & 1.2wt% Zn, Pd/Zn=1/2 mol mol -1 ) a H 2 PdO b Pd Pd Pd Pd H 2 c H H Pd Zn Pd Pd Pd 6
21 J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. PdZn/Mg(Al)(Pd)(Zn)O x synthesis via co-precipitation (1wt% Pd & 1.2wt% Zn, Pd/Zn=1/2 mol mol -1 ) a H PdO b Pd Pd Pd Pd H 2 c H H Pd Zn Pd Pd Pd 6
22 J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. PdZn/Mg(Al)(Pd)(Zn)O x synthesis via co-precipitation (1wt% Pd & 1.2wt% Zn, Pd/Zn=1/2 mol mol -1 ) a H PdO b Pd Pd Pd Pd H c H H Pd Zn Pd Pd Pd 6
23 J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. PdZn/Mg(Al)(Pd)(Zn)O x synthesis via co-precipitation (1wt% Pd & 1.2wt% Zn, Pd/Zn=1/2 mol mol -1 ) a d PdZn Pd PdZn PdZn PdZn Pd Pd Pd Zn H PdO O 2 b Pd Pd Pd Pd H 2 e PdO PdO PdO PdO H 2 c H H Pd Zn Pd Pd Pd f PdZn PdZn PdZn PdZn PdZn PdZn 6
24 J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. PdZn/Mg(Al)(Pd)(Zn)O x synthesis via co-precipitation (1wt% Pd & 1.2wt% Zn, Pd/Zn=1/2 mol mol -1 ) a d PdZn Pd PdZn PdZn PdZn Pd Pd Pd Zn H PdO O b Pd Pd Pd Pd H 2 e PdO PdO PdO PdO H 2 c H H Pd Zn Pd Pd Pd f PdZn PdZn PdZn PdZn PdZn PdZn 6
25 J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. PdZn/Mg(Al)(Pd)(Zn)O x synthesis via co-precipitation (1wt% Pd & 1.2wt% Zn, Pd/Zn=1/2 mol mol -1 ) a d PdZn Pd PdZn PdZn PdZn Pd Pd Pd Zn H PdO O b Pd Pd Pd Pd H 2 e PdO PdO PdO PdO c H 2 H Pd Zn Pd Pd H f PdZn PdZn PdZn PdZn PdZn PdZn 6
26 STY AcH (10-4 mols -1 kg Pd -1 ) J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. S AcH (%) Coking of unwanted Pd sites improves the selectivity T: 533K, P tot : 0.5MPa, W/F EtOH :36 kg cat s mol -1 I II III Time on stream (h) I: freshly activated II: after 1st regeneration III: after 2nd regeneration
27 STY AcH (10-4 mols -1 kg Pd -1 ) J. De Waele et al., Catal. Sci. Technol., 2017, DOI: /C7CY01105A. S AcH (%) Coking of unwanted Pd sites improves the selectivity T: 533K, P tot : 0.5MPa, W/F EtOH :36 kg cat s mol -1 I II III Time on stream (h) I: freshly activated II: after 1st regeneration III: after 2nd regeneration
28 Steady-state experiments on a high-throughput set-up 2x (30min H 2 15min N 2 30min O 2 15min N 2 ) 30min H 2 8
29 Steady-state experiments on a high-throughput set-up 2x (30min H 2 15min N 2 30min O 2 15min N 2 ) 30min H 2 Temperature: 533K Total pressure: 0.5 MPa N 2 (or N 2 +H 2 O)/ethanol: 20 Space time: 36 kg cat s mol -1 8
30 Steady-state experiments on a high-throughput set-up 2x (30min H 2 15min N 2 30min O 2 15min N 2 ) 30min H 2 Temperature: 533K Total pressure: 0.5 MPa N 2 (or N 2 +H 2 O)/ethanol: 20 Space time: 36 kg cat s mol -1 Experiment 1: 100wt% ethanol Experiment 2: 30wt%H 2 O/ethanol Experiment 3: 100wt% ethanol Experiment 4: 100wt% ethanol after regeneration 8
31 S AcH (%) Conversion (%) Activity and selectivity changes Time (h) 100% ethanol gives a stable activity after 24h catalyst structure is formed and stable Time (h) 7 9
32 S AcH (%) Conversion (%) Activity and selectivity changes Time (h) 100% ethanol gives a stable activity after 24h catalyst structure is formed and stable. With 30wt%H 2 O/EtOH, the activity and acetaldehyde selectivity drops catalyst changes or different reactions occuring? Time (h) 7 9
33 S AcH (%) Conversion (%) Activity and selectivity changes Time (h) 100% ethanol gives a stable activity after 24h catalyst structure is formed and stable. With 30wt%H 2 O/EtOH, the activity and acetaldehyde selectivity drops catalyst changes or different reactions occuring? With 100%EtOH, the activity and acetaldehyde selectivity rises again, but not to the original it seems that the catalyst changes Time (h) 7 9
34 S AcH (%) Conversion (%) Activity and selectivity changes Time (h) 100% ethanol gives a stable activity after 24h catalyst structure is formed and stable. With 30wt%H 2 O/EtOH, the activity and acetaldehyde selectivity drops catalyst changes or different reactions occuring? With 100%EtOH, the activity and acetaldehyde selectivity rises again, but not to the original it seems that the catalyst changes Time (h) After regeneration, the activity and selectivity are as original, althought the catalyst deactivates more rapidly. catalyst fully restored? 7 9
35 PdZn alloy remains present in XRD, but less clear : MgO : γ-al 2 O 3 : PdZn 100wt% ethanol 30wt% H 2 O/ethanol 100wt% ethanol regeneration-100wt% ethanol θ ( ) 7 10
36 Surface area & particle size changes upon water feed BET surface area (m² g -1 ) Metal loading (%) Pd Zn 100wt% ethanol 71.4 ± wt% H 2 O/ethanol 45.9 ± wt% ethanol 44.9 ± regeneration-100wt% ethanol 90.6 ±
37 Surface area & particle size changes upon water feed BET surface area (m² g -1 ) Metal loading (%) Pd Zn 100wt% ethanol 71.4 ± wt% H 2 O/ethanol 45.9 ± wt% ethanol 44.9 ± regeneration-100wt% ethanol 90.6 ± STEM particle size (nm) 100wt% ethanol 5 ± 2 30wt% H 2 O/ethanol 2 ± 1 100wt% ethanol 2.5 ± 1.2 & 8 ± 3 regeneration-100wt% ethanol 5.5 ±
38 Hollow particles found for all samples Mg Pd Zn Al Due to the oxidizing & reducing environment hollow particles form via rapid diffusion of Pd compared to Zn 7 12
39 Zn clusters on particle upon water feed Zinc seems to be partially removed from the particle and appears as a cluster on the surface 7 13
40 Amount of cokes lower upon water feed Cokes production (mol g -1 ) 100%ethanol ± wt%H 2 O/ethanol ± %ethanol ± regeneration-100%ethanol ± The temperature at which the cokes is burned is the same same interaction between cokes and Pd-sites for all catalysts. 7 14
41 What is now happening with the catalyst? 1. More methane formation 2. Less active 3. Smaller surface area 4. Smaller particle size 5. Zn-rich spots in border particles 6. Less cokes 7 15
42 What is now happening with the catalyst? 1. More methane formation 2. Less active 3. Smaller surface area 4. Smaller particle size 5. Zn-rich spots in border particles 6. Less cokes Pd-rich alloy 7 15
43 What is now happening with the catalyst? 1. More methane formation 2. Less active 3. Smaller surface area 4. Smaller particle size 5. Zn-rich spots in border particles 6. Less cokes Pd-rich alloy Zn-rich clusters 7 15
44 What is now happening with the catalyst? 1. More methane formation 2. Less active 3. Smaller surface area 4. Smaller particle size 5. Zn-rich spots in border particles 6. Less cokes Pd-rich alloy Zn-rich clusters Changes in support 7 15
45 What is now happening with the catalyst? 1. More methane formation 2. Less active 3. Smaller surface area 4. Smaller particle size 5. Zn-rich spots in border particles 6. Less cokes Pd-rich alloy Zn-rich clusters Changes in support Desintegration of particles 7 15
46 What is now happening with the catalyst? 1. More methane formation 2. Less active 3. Smaller surface area 4. Smaller particle size 5. Zn-rich spots in border particles 6. Less cokes Pd-rich alloy Zn-rich clusters Changes in support Desintegration of particles Segregation of PdZn particles to Zn-rich clusters and an Pd-rich alloy on one particle Formation of smaller particles due to oxidizing and reducing environment in-situ 7 15
47 Conclusion Zn Zn Zn Zn Zn PdZn (highly Pd-rich alloy) Zn Zn Zn PdZn (Pd-rich alloy) Zn Zn 7 16
48 Acknowledgments This work was supported by the Interuniversity Attraction Poles Programme - Belgian State Belgian Science Policy, the European Research Council under the European Union s Seventh Framework Programme (FP7/ ) / ERC grant agreement n and the 'Long Term Structural Methusalem Funding by the Flemish Government'. Thank you for your attention! 17
49 LABORATORY FOR CHEMICAL TECHNOLOGY Technologiepark 914, 9052 Ghent, Belgium E info.lct@ugent.be T
50 Normalized Xµ(E) Extra slide Catalyst PdZn/Mg(Al)(Pd)(Zn)O x Reference Pd foil Reference PdZn Energy Energy (ev) (ev)
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