Abstract
Pyrolysis of cellulose powder granules impregnated with an aqueous solution of saccharose and palladium nitrate gave granular Pd/C carbons with 1–9 wt % metal. It was shown by X-ray diffraction analysis and electronic microscopy that palladium is present in the carbon matrix in the form of Pd(0) nanoparticles with sizes of 10–30 nm in the main fraction (~95%). Palladium nanoparticles are localized inside the saccharose carbonizate layer and on its surface. An IR spectral study showed that pyrolysis of the cellulose–saccharose powder composite in the presence of palladium nitrate leads to the appearance of ester groups in the carbonizate. An increase in the palladium nitrate content in the cellulose powder leads to lower yields of the carbonizate and larger metal nanoparticles in carbon. The specific catalytic activity of nanoparticles in the model decomposition reaction of hydrogen peroxide was found to be the same for all palladium-containing carbons.
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1134%2FS0040579523050305/MediaObjects/11236_2024_8701_Fig1_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1134%2FS0040579523050305/MediaObjects/11236_2024_8701_Fig2_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1134%2FS0040579523050305/MediaObjects/11236_2024_8701_Fig3_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1134%2FS0040579523050305/MediaObjects/11236_2024_8701_Fig4_HTML.png)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1134%2FS0040579523050305/MediaObjects/11236_2024_8701_Fig5_HTML.png)
REFERENCES
McAllister, M.I., Boulho, C., McMillan, L., Gilpin, L.F., Brennan, C., and Lennon, D., The hydrogenation of mandelonitrile over a Pd / C catalyst: Towards a mechanistic understanding, RSC Adv., 2019, vol. 9, no. 45, pp. 26116–26125. https://doi.org/10.1039/C9RA04618F
Belskaya, O.B., Mironenko, R.M., Talsi, V.P., Rodionov, V.A., Gulyaeva, T.I., Sysolyatin, S.V., and Likholobov, V.A., The effect of preparation conditions of Pd/C catalyst on its activity and selectivity in the aqueous-phase hydrogenation of 2,4,6-trinitrobenzoic acid, Catal. Today, 2018, vol. 301, pp. 258–265. https://doi.org/10.1016/j.cattod.2017.02.037
Cini, E., Petricci, E., and Taddei, M., Pd / C Catalysis under microwave dielectric heating, Catalysts, 2017, vol. 7, no. 3, pp. 1–27. https://doi.org/10.3390/catal7030089
Magdalinova, N.A. and Klyuev, M.V., Hydrogenation of nitro- and unsaturated organic compounds on catalysts containing palladium nanosized particles, Neftekhimiya, 2017, vol. 57, no. 6, pp. 647–652. https://doi.org/10.7868/S0028242117060065
Merkin, A.A., Komarov, A.A., Lopatkin, E.F., and Lefedova, O.V., Hydrogenation of 1,5-dinitronaphtalene on deposited catalysts in liquid phase, Izv. VUZov. Khim-. Khim. Tekhnol., 2015, vol. 58, no. 11, pp. 69–73.
Mironenko, P.N., Belskaya, O.V., and Likholobov, V.A., Synthesis of Pd/C catalysts: Approaches to regulating the structure of active sites to achieve high selectivity in hydrogenations of organic compounds, Ross. Khim. Zh., 2018, vol. 62, nos. 1–2, pp. 141–159.
Simakova, I.L., Demidova, Yu.S., Prikhod’ko, S.A., Simonov, M.N., and Shabalin, A.Yu., Liquid phase pentanol Guerbet-Markovnikov condensation over VIII group metals, Zh. Sib. Fed. Univ., Khim., 2016, vol. 9, no. 2, pp. 201–211. https://doi.org/10.17516/1998-2836-2016-9-2-201-211
Huang, X., Ouyang, X., Hendriks, B.M.S., Gonzales, O.M.M., Zhu, J., Korányi, T.I., Boot, M.D., and Hensen E.J.M., Selective production of mono-aromatics from lignocellulose over Pd / C catalyst: the influence of acid co-catalysts, Faraday Discuss., 2017, vol. 202, pp. 141–156. 10.1039/C7FD00039A
Bin, Z., Xueshan, C., Jiaojiao, X., and Cunshan, Z., Alkaline ionic liquid modified Pd/C catalyst as an efficient catalyst for oxidation of 5-hydroxymethylfurfural, J. Chem., 2018, article no. 2018743, pp. 1–9. 10.1155/2018/2018743
Carrara, N., Betti, C., Coloma-Pascual, F., Almansa, M.C., Gutierrez, L., Miranda, C., Quiroga, M.E., and Lederhos, C.R., High-active metallic-activated carbon catalysts for selective hydrogenation, Int. J. Chem. Eng., 2018, article no. 4307308. pp. 1–11. https://doi.org/10.1155/2018/4307308
Safina, A.V., Timerbaev, N.F., Ziatdinova, D.F., Safin, R.G., and Khabibullina, A.R., Heat and mass transfer simulation in the pyrolysis zone, Izv. Vyssh. Uchebn. Zaved., Lesn. Zh., 2019, no. 1, pp. 153–169. 10.17238/issn0536-1036.2019.1.153
Yur’ev, Yu.L., Gidulin, I.K., and Drozdova, N.A., Options of low-grade wood processing into carbon-base material, Izv. Vyssh. Uchebn. Zaved., Lesn. Zh., 2017, no. 5, pp. 139–149. 10.17238/issn0536-1036.2017.5.139
Eremina, A.O., Golovina, V.V., Sobolev, A.A., and Chesnokov, N.V., Sorption of palladium by carbon sorbents from aqueous solutions, Zh. Sib. Fed. Univ., Khi-m., 2015, vol. 8, no. 4, pp. 541–545. https://doi.org/10.17516/1998-2836-2015-8-4-541-549
Kuznetsov, B.N., Chesnokov, N.V., Mikhlin, Yu.L., Tsyganova, S.I., Mikova, N.M., and Garyntseva, N.V., and Ivanchenko, N.M., Studies on structure of porous carbonaceous materials obtained by pyrolysis of microcrystalline cellulose from birch wood, Khim. Interesakh Ustoich. Razvit., 2015, vol. 23, no. 5, pp. 515–521. https://doi.org/10.15372 / KhUR20150502
Lokteva, E.S., Golubina, E.V., Antonova, M.V., Klokov, S.V., Maslakov, K.I., Egorov, A.V., and Likholobov, V.A., Chlorobenzene hydrodechlorination catalyst prepared via the pyrolysis of sawdust impregnated with palladium nitrate, Kinet. Catal., 2015, vol. 56, no. 6, pp. 764–773. https://doi.org/10.1134/S0023158415060099
Tarasenko, Yu.A., Gerasimiuk, I.P., Kaleniuk, A.A., and Lapko, V.F., Palladium-carbon catalyst for processes of liquid-phase hydrogenation, Poverkhnost’, 2015, no. 7, pp. 161–172.
Klokov, S.V., Based on palladium, cobalt, and carbon mono- and bimetallic composite catalysts for hydrodechlorination of chlorobenzenes, Cand. (Chem.) Dissertation, Moscow, Mosk. Gos. Univ., 2021.
Shishmakov, A.B., Mikushina, Yu.V., and Koryakova, O.V., Catalyst “palladium on carbon” prepared by pyrolysis of the powder cellulose granules impregnated with palladium nitrate, Khim. Rastit. Syr’ya, 2021, no. 2, pp. 333–342. https://doi.org/10.14258/jcprm.2021028813
Harris, P.J.F., Burian, A., and Duber, S., High-resolution electron microscopy of a microporous carbon, Philos. Mag. Lett., 2000, vol. 80, no. 6, pp. 381–386. https://doi.org/10.1080/095008300403512
Fey, G.T.-K. and Kao, Y.-C. Synthesis and characterization of pyrolyzed sugar carbons under nitrogen or argon atmospheres as anode materials for lithium-ion batteries, Mater. Chem. Phys., 2002, vol. 73, no. 1, pp. 37–46. https://doi.org/10.1016/S0254-0584(01)00348-0
Myronyuk, I.F., Mandzyuk, V.I., Sachko, V.M., and Gun’ko, V.M. Structural features of carbons produced using glucose, lactose, and saccharose, Nanoscale Res. Lett., 2016, vol. 11, pp. 1–9. https://doi.org/10.1186/s11671-016-1723-z
Cai, J., Yang. M., **ng, Y., and Zhao, X. Large surface area sucrose-based carbons via template-assisted routes: Preparation, microstructure, and hydrogen adsorption properties, Colloids Surf., A, 2014, vol. 444, pp. 240–245. https://doi.org/10.1016/j.colsurfa2013.12.063
Wang, N., Hong, Y., Liu, T.Z., Wang, Q., and Huang, J., Sucrose derived microporous–mesoporous carbon for advanced lithium–sulfur batteries, Ceram. Int., 2021, vol. 47, no. 1, pp. 899–906. https://doi.org/10.1016/j.ceramint.2020.08.202
Onishchenko, D.V., Technology of preparation of anodic materials for lithium-ionic (polymeric) accumulators from renewable vegetable raw materials and agricultural crop waste, Extended abstract of Cand. (Eng.) Dissertation, Vladivostok: DVPI, 2008.
Xue, J., Chen, S.C., Tang, H.K., **ang, H.K., Wang, X.H., and Cao, H. Structure and magnetic properties of carbon encapsulated Co nanoparticles prepared by the pyrolysis of mixture of sucrose and cobalt nitrate, Adv. Mater. Res., 2010, vols. 97–101, pp. 2201–2204. https://doi.org/10.4028/www.scientific.net/AMR.97-101.2201
Khalilov, I.F., Il’yasov, I.P., Gerasimova, A.V., Lamberov, A.A., Bikmurzin, A.Sh., and Shatilov, V.M., Influence of promoting with cobalt and zinc on hydrogenating and oligomerazing activity of Pd/Al2O3 catalyst at hydrogenating BTK-fraction, Katal. Prom-sti., 2013, no. 5, pp. 29–38. https://doi.org/10.1134/S2070050413040053
Chen, Y., Hu, Y., Shao, J., Shen, Z., Chen, R., Zhang, X., He, X, Song, Y., and **ng, X., Pyrolytic carbon-coated silicon/carbon nanofiber composite anodes for high-performance lithium-ion batteries, J. Power Sources, 2015, vol. 298, pp. 130–137. https://doi.org/10.1016/J.JPOWSOUR2015.08.058
Funding
This study was financially supported by the Ural Branch, Russian Academy of Sciences (Competition program, project no. AAAA-A19-119011790132-7).
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
The authors of this work declare that they have no conflicts of interest.
Additional information
Translated by L. Smolina
Publisher’s Note.
Pleiades Publishing remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Rights and permissions
About this article
Cite this article
Shishmakov, A.B., Mikushina, Y.V. & Koryakova, O.V. Synthesis of Pd(0)/C by Pyrolysis of the Cellulose–Saccharose–Palladium Nitrate Powder Composite. Theor Found Chem Eng 57, 985–990 (2023). https://doi.org/10.1134/S0040579523050305
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0040579523050305