New SILP materials based on TiO2-SiO2 and TiO2-SiO2/lignin supports as effective catalysts for hydrosilylation reaction.

Published: 7 December 2021| Version 1 | DOI: 10.17632/m3rbdpvb34.1
Olga Bartlewicz


This dataset contains results of conducted physicochemical analysis and catalytic tests on new Supported Ionic Liquid Phase materials with rhodium and platinum based on TiO2-SiO2 and TiO2-SiO2/lignin supports. The aim of this research was to obtain new SILP materials with rhodium and platinum, based on the oxide systems TiO2-SiO2 and TiO2-SiO2/lignin supports. As part of this research, the synthesis of oxide systems was carried out and obtained supports were applied in new SILP materials. Catalytic activity of the obtained SILP materials was tested in the hydrosilylation of 1-octene with 1,1,1,3,5,5,5-heptamethyltrisiloxane. The supports and catalytic materials were subjected to thorough characterization by elemental analysis, XRD, SEM-EDX, IR, and TGA, and their particle size distribution and porous properties were assessed. The conducted research proved the possibility of easy isolation and re-use in subsequent catalytic cycles of new SILP materials with rhodium and platinum. It is worth noting that the oxide systems TiO2-SiO2 and TiO2-SiO2 /lignin have not been used in this type of catalytic materials so far. Samples description was included in the README file.


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Materials: Reagents used in catalytic tests, such as 1-octene, 1,1,1,3,5,5,5-heptamethyltrisiloxane (HMTS) and n-decan were supplied by Sigma Aldrich and used as received. Ionic liquids: 1-butyl-3-methylimidazolium chloride, 1-butyl-4-methylpyridinium chloride, tributhyltetradecylphosphonium chloride, triethylsulfonium bis(trifluoromethanesulfonyl)amide, trimethylsulfonium methylsulfate and lithium bis(trifluoromethanesulfonyl)amide, dimethyl sulfate and lithium bis(trifluoromethylsulfonyl)- imide were purchased from Iolitec. The reagents used to obtain the supports and their modification, i.e. methanol, ammonia solution (25%), titanium (IV) isopropoxide (TIPP), Kraft lignin, 1,4-dioxane, sodium(meta)periodate, 3-(trimethoxysilyl)propyl isocyanate were purchased from Sigma Aldrich and did not require additional purification. The solvents used to prepare the SILP, such as: acetonitrile and dichloromethane were purchased from Fisher Chemicals. Techniques: The reaction yield was determined by using Clarus 680 gas chromatograph (Perkin Elmer) equipped with a 30 m capillary column Agilent VF-5ms and TCD detector. The measurement were carried out by using temperature program: 60 ℃ (3 min.), 10℃ min-1, 290℃ (5min.). Obtained hydrosilylation reaction product and synthesized ionic liquids were subjected to NMR analysis. NMR spectra were made with Brucker BioSpin (400Hz) spectrometer using acetonitrile-d3 and chloroform-d as solvents. FT-IR in situ tests were implemented by using Mettler Toledo ReactIR 15 instrument. The IR spectra were recorded in the Bruker Tensor 27 apparatus in the range 500–4000 cm−1 of wave number. XRD analysis of inorganic supports was performed by using X-ray diffractometer Bruker D8 Advance and standard measuring cuvette. The measurement was carried out for 1 hour, at an 2theta angle length 0 – 75. Thermogravimetric analysis was performer by TA Instruments analyser, model TG Q50at a linear heating rate 10℃/min. under nitrogen (50ml/min.). The adsorption characteristic was performed by using Micromeritics ASAP 2010 sorptometer. The analysed samples were first degassed at 393K for 20h. The BET (Brunauer-Emmet-Teller) surface area of supports and SILP materials were determined by N2 adsorption at 77K. Indication of the percentage of N, C, H, S in the samples was performed by elemental analysis. For this purpose Elementar Analyser Vario EL III was used. The samples were burned at a temperature of 1200℃, and then the generated gases were separated on adsorption columns and detected by the difference in thermal conductivity. SEM-EDX analysis was performed by using scanning electron microscope (SEM) Hitachi S-3500 N equipped with an energy-dispersive X-ray (EDX) detector Ultra Dry Silicon Drift X-ray Detector made by Thermo Scientific was used. The particle size measurement analysis was performed using the Zetasizer Nano ZS analyser by Malvern Instruments Ltd.


Uniwersytet im Adama Mickiewicza w Poznaniu Wydzial Chemii


Chemistry, Catalysis, Ionic Liquid, Heterogeneous Catalyst