(560b) “H2 -Free” Hydrodeoxygenation of Guaiacol over Ni-Mo/CeO2-C Nanocatalysts

text-align:center;line-height:normal"> 14.0pt;mso-ascii-font-family:Calibri;mso-fareast-font-family:" times new roman mso-hansi-font-family:calibri en-us>H₂-free hydrodeoxygenation
of guaiacol over Ni-Mo/CeO₂-C nanocatalysts

text-align:center;line-height:normal"> 14.0pt;mso-ascii-font-family:Calibri;mso-fareast-font-family:" times new roman mso-hansi-font-family:calibri en-us>

text-align:center;line-height:normal"> " times new roman mso-fareast-language:es>W. Jin ¹, L. Pastor-Pérez ^1,2*, J.J.
Villora-Picó², S.Gu, A.
Sepúlveda-Escribano², T. R. Reina ¹*

text-align:center;line-height:normal"> mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri>

text-align:center;line-height:normal"> ^{10.0pt;mso-ascii-font-family:Calibri;mso-fareast-font-family:" times new roman mso-hansi-font-family:calibri en-gb>1} " times new roman mso-ansi-language:en-gb>Chemical and Process Engineering
Department, University of Surrey, Guildford, UK

text-align:center;line-height:normal"> ^{mso-ascii-font-family:Calibri;mso-fareast-font-family:" times new roman mso-hansi-font-family:calibri es>2} mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri>Departamento de Química
Inorgánica, Instituto Universitario de Materiales de Alicante, Alicante, Spain

text-align:center;line-height:normal"> mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri>* Calibri;mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri>Autor principal: l.pastorperez@surrey.ac.uk

normal"> " times new roman mso-fareast-language:es>

normal">1. Introduction

line-height:normal"> mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri>Catalytic
hydrodeoxygenation (HDO) is a fundamental technology Calibri;mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri> to
achieve the effective upgrading of bio-oil with low emission. Currently, the
widespread implementation of HDO is limited by the supply of high pressure H₂
(4-20 MPa). To date, several methods (e.g.
catalytic transfer hydrogenation (CTH), reforming followed by HDO, the
combination of metal oxidation with water and HDO and non-thermal plasma (NTP)
technology

Calibri;mso-fareast-font-family:"Times New Roman";mso-hansi-font-family:Calibri;
mso-bidi-font-family:Calibri;mso-ansi-language:PT;mso-fareast-language:ES'> style='mso-element:field-begin'> style='mso-spacerun:yes'> ADDIN EN.CITE
<EndNote><Cite><Author>Jin</Author><Year>2018</Year><RecNum>1021</RecNum><DisplayText><style
face="superscript">1</style></DisplayText><record><rec-number>1021</rec-number><foreign-keys><key
app="EN" db-id="ev50xfrfyztavjea2r9p0vz5tdstrx9rr2v0"
timestamp="1548931371">1021</key></foreign-keys><ref-type
name="Journal Article">17</ref-type><contributors><authors><author>Jin,
Wei</author><author>Pastor-Perez,
Laura</author><author>Shen,
DeKui</author><author>Sepúlveda-Escribano,
Antonio</author><author>Gu, Sai</author><author>Reina,
Tomas Ramirez</author></authors></contributors><titles><title>Catalytic
upgrading of biomass model compounds: Novel approaches and lessons learnt from
traditional hydrodeoxygenation‐a
review</title><secondary-title>ChemCatChem</secondary-title></titles><periodical><full-title>Chemcatchem</full-title></periodical><dates><year>2018</year></dates><isbn>1867-3880</isbn><urls></urls></record></Cite></EndNote> style='mso-element:field-separator'>¹

lang=PT style='mso-ascii-font-family:Calibri;mso-fareast-font-family:"Times New Roman";
mso-hansi-font-family:Calibri;mso-bidi-font-family:Calibri;mso-ansi-language:
PT;mso-fareast-language:ES'>) have been proposed which could achieve the
deoxygenation with in-situ hydrogen
generation. It is noteworthy that metal oxidation with H₂O (i.e. Zn) followed by subsequent HDO is
an attractive approach due to cheap water is used as the hydrogen source.
Nevertheless, the regeneration of metal requires high energy input

lang=PT style='mso-ascii-font-family:Calibri;mso-fareast-font-family:"Times New Roman";
mso-hansi-font-family:Calibri;mso-bidi-font-family:Calibri;mso-ansi-language:
PT;mso-fareast-language:ES'> style='mso-spacerun:yes'> ADDIN EN.CITE
<EndNote><Cite><Author>Cheng</Author><Year>2017</Year><RecNum>807</RecNum><DisplayText><style
face="superscript">2-3</style></DisplayText><record><rec-number>807</rec-number><foreign-keys><key
app="EN" db-id="ev50xfrfyztavjea2r9p0vz5tdstrx9rr2v0"
timestamp="1516717974">807</key></foreign-keys><ref-type
name="Journal Article">17</ref-type><contributors><authors><author>Cheng,
Shouyun</author><author>Wei,
Lin</author><author>Alsowij, Mustafa
Radhi</author><author>Corbin, Fletcher</author><author>Julson,
James</author><author>Boakye,
Eric</author><author>Raynie, Douglas</author></authors></contributors><titles><title>In
situ hydrodeoxygenation upgrading of pine sawdust bio-oil to hydrocarbon
biofuel using Pd/C catalyst</title><secondary-title>Journal of the
Energy Institute</secondary-title></titles><periodical><full-title>Journal
of the Energy
Institute</full-title></periodical><dates><year>2017</year></dates><urls></urls></record></Cite><Cite><Author>Cheng</Author><Year>2017</Year><RecNum>818</RecNum><record><rec-number>818</rec-number><foreign-keys><key
app="EN" db-id="ev50xfrfyztavjea2r9p0vz5tdstrx9rr2v0"
timestamp="1516810530">818</key></foreign-keys><ref-type
name="Journal
Article">17</ref-type><contributors><authors><author>Cheng,
Shouyun</author><author>Wei,
Lin</author><author>Julson,
James</author><author>Muthukumarappan,
Kasiviswanathan</author><author>Kharel, Parashu
Ram</author><author>Cao, Yuhe</author><author>Boakye,
Eric</author><author>Raynie,
Douglas</author><author>Gu, Zhengrong</author></authors></contributors><titles><title>Hydrodeoxygenation
upgrading of pine sawdust bio-oil using zinc metal with zero
valency</title><secondary-title>Journal of the Taiwan Institute of
Chemical
Engineers</secondary-title></titles><periodical><full-title>Journal
of the Taiwan Institute of Chemical Engineers</full-title></periodical><dates><year>2017</year></dates><urls></urls></record></Cite></EndNote> style='mso-element:field-separator'>^2-3

lang=PT style='mso-ascii-font-family:Calibri;mso-fareast-font-family:"Times New Roman";
mso-hansi-font-family:Calibri;mso-bidi-font-family:Calibri;mso-ansi-language:
PT;mso-fareast-language:ES'> limiting its industrial application. Undoubtedly,
it is ideal to use water as the hydrogen source during HDO process considering
readily available and cheap advantages of water over other candidates.
Accordingly, we propose a novel HDO method to realize the normal">in-situ HDO suppressing the supply of external H₂. It is
envisioned that water would undergo splitting on the catalytic surface to
produce hydrogen. Hydrogen can further participate in the HDO of bio-oil to
faciliate the oxygen removal purpose. " times new roman> EN-GB">Ni-based catalysts are promising candidates for normal">in-situ HDO process by tuning the support composition and/or
including promoters to adjust their catalytic functions. In this work, Ni-based
CeO₂ and/or activated Calibri;mso-fareast-font-family:" times new roman mso-bidi-font-family:calibri>carbon
supported catalysts were synthesized, characterized and tested in guaiacol HDO
water-only reaction system. This novel method brings a new perspetive in the
development of econimically viable bio-oil upgrading technologies. mso-bidi-font-family:" times new roman> mso-bidi-font-family:" times new roman>

normal">

normal">2. Experimental

justify;text-justify:inter-ideograph;line-height:normal">CeO₂-C (10wt.%
CeO₂) was prepared in advance before the synthesis of Ni-based
catalysts. Five catalysts namely, Ni/CeO₂, NiMo/CeO₂,
Ni/C, Ni/CeO₂-C and NiMo/CeO₂-C
(with 15 wt.% Ni and 2 wt.% Mo) were synthesized by wet impregnation method and
characterized by H₂-TPR, XRD, N₂-adsorption, TEM, XPS and
Raman analysis. Prior to the activity tests, catalysts were activated at 400 ^oC for 1h under H₂ atmosphere. The
catalytic performances of catalysts for guaiacol HDO
process were tested in a high pressure batch reactor (Parr Series 5500 HPCL
Reactor) by feeding 50 mL of a 0.01 mg/mL guaiacol
solution and 200 mg of catalyst at 250 ^oC
for 4h. After the reaction, the catalyst was collected by filtration. Products
were separated from water by using ethyl acetate and then analyzed by GC/FID
and GC/MS.

normal">

normal">3. Results and discussion

justify;text-justify:inter-ideograph;line-height:normal">The XRD patterns of
Ni-based catalysts after activation were shown in Figure 1.It is clear that
ceria and Ni dispersion are much better when activated carbon are used as
primary support. The Ni and ceria particle sizes are smaller in the carbon
supported materials. The textural properties summarised in Table 1 also
indicate the suitability of activated carbon to achieve large surface areas mso-bidi-font-family:" times new roman>. The catalytic
performance of all studied catalysts is presented in Figure 2. C-containing
catalysts exhibited higher activity compared to CeO₂ supported
catalysts. For instance, Calibri;mso-hansi-font-family:Calibri;mso-bidi-font-family:" times new roman mso-ansi-language:en-gb>22 % mso-bidi-font-family:" times new roman>conversion of guaiacol is obtained in HDO over Ni/CeO₂-C
catalyst,

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mso-hansi-font-family:Calibri;mso-bidi-font-family:" times new roman mso-ansi-language:en-gb>which is a significant

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Figure 1 XRD patterns of reduced catalysts
Table 1 Textural properties of catalysts SBET (m2/g) Vmicro (cc/g)a Vtotal (cc/g)
Ni/CeO2 78 0.029 0.064
NiMo/CeO2 46 0.017 0.069
Ni/C 1062 0.378 0.85
Ni/CeO2-C 1027 0.368 0.79
NiMo/CeO2-C 1017 0.364 0.79
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UEsBAi0AFAAGAAgAAAAhADj9If/WAAAAlAEAAAsAAAAAAAAAAAAAAAAALwEAAF9yZWxzLy5yZWxz
UEsBAi0AFAAGAAgAAAAhAB1pnUUjAgAAIwQAAA4AAAAAAAAAAAAAAAAALgIAAGRycy9lMm9Eb2Mu
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cmV2LnhtbFBLBQYAAAAABAAEAPMAAACJBQAAAAA=
" stroked="f">

Figure 2. Activity of catalysts during in-situ HDO process
Figure 3. Selected TEM images of Ni/CeO2-C
" v:shapes="_x0000_s1026" class="documentimage"> Calibri;mso-hansi-font-family:Calibri;mso-bidi-font-family:" times new roman mso-ansi-language:en-gb>case of water-only HDO reaction system. Regarding the
characterization of spent samples, no metal sintering and minor
concentration of carbon deposition were observed in the TEM images (Figure 3)
and also by XRD and Raman.

normal"> " times new roman mso-ansi-language:en-gb>

normal">4. Conclusions

mso-bidi-font-family:" times new roman>A novel
approach consisting on the combination of water splitting and subsequent hydrodeoxygenation (HDO) is proposed in this work with the
aim to suppress the supply of H₂ to the HDO reactor. CeO₂-C
supported catalysts performed high HDO ability compared to CeO₂-supported
catalysts in guaiacol normal">in-situ HDO process. The high HDO activity of CeO₂-C
supported catalysts is likely attributed to the high dispersion and small
particle size of active phase along with the high surface area of catalysts.
The proposed novel method by using available and cheap water as hydrogen source
in HDO reaction is an interesting alternative which opens new research
possibilities to achieve low-cost bio-oil upgrading process.

normal">

normal">References

lang=EN-US style='mso-fareast-language:ES'> style='mso-ansi-language:ES;mso-fareast-language:ES'> style='mso-spacerun:yes'> ADDIN EN.REFLIST

lang=EN-US style='mso-fareast-language:ES'>1. Jin, W.; Pastor-Perez, L.; Shen, D.;
Sepúlveda-Escribano, A.; Gu, S.; Reina, T. R., normal">ChemCatChem 2019, 11,
924-960.

2. Cheng, S.; Wei, L.; Alsowij, M. R.; Corbin, F.; Julson, J.;
Boakye, E.; Raynie, D., Journal of the
Energy Institute 2018, 91,
163-171.

3. Cheng, S.; Wei, L.; Julson,
J.; Muthukumarappan, K.; Kharel, P. R.; Cao, Y.; Boakye, E.; Raynie, D.; Gu,
Z., Journal of the Taiwan Institute of
Chemical Engineers 2017, 74,
146-153. mso-fareast-font-family:" times new roman mso-ansi-language:en-gb>