DOI: 10.18150/iclhsu
title: Publication raw data: Bifunctionalized acid-base hierarchically structured monolithic microreactor for continuous-flow tandem catalytic processes of cyanocinnamte synthesis

description: Data collected for the publication entitled: “Bifunctionalized acid-base hierarchically structured monolithic microreactor for continuous-flow tandem catalytic processes of cyanocinnamte synthesis” File: AcidicyData obtained from IR absorption measurements on amine/zirconia/silica sample exposed to pyridine vapors.RESEARCH METHOD: Fourier transform infrared spectroscopyFILE FORMAT: *csv (separated by commas); 2 columns: wavelength [cm^1] (column 1); Absorbance (Column 2)EQUIPMENT AND SOFTWARE: FTIR spectrometer Invenio, Bruker, MCT detector; Opus Touch software;ANALYSIS METHOD DETAILS: Spectra range 4000–600 cm^−1; 100 scans; resolution 2 cm^−1; SAMPLE PREPARATION DETAILS: Samples were pressed into pellets at p = 3 bar. Activation of the sample: drying 200◦C; Adsorption of pyridine vapors: 150◦C; Desorption: 150◦C File: ASAPData obtained from nitrogen absorption and desorption measurements- Isotherms and Cumulative Pore Size Distribution (CPSD).Sample description: Zr-M – silica modified with zirconia; NH2-Zr-M- silica modified with amine and zirconia; M- pure silicaRESEARCH METHOD: low temperature nitrogen adsorptionFILE FORMAT: *csv (separated by commas); 2 columns: relative pressure (column 1); quantity adsorbed [cm^3/g] (Column 2).EQUIPMENT AND SOFTWARE: ASAP2020 Micromeritics; ASAP2020 softwareANALYSIS METHOD DETAILS: Nitrogen adsorption at −196◦C. The specific surface area calculated using Braunauer, Emmet and Teller (BET) equation.SAMPLE PREPARATION DETAILS: Samples degassed at 200 ◦C under vacuum for 24 h. File: TGData from thermogravimetric measurements of samples modified with amines using two different experimental methods: TG curves (%mass loss) and DTG curve.Sample description: NH2-Zr-M- silica modified with amine and zirconia; TG curves (slice 1-4) (A)-flow method and (B)-soaking method.RESEARCH METHOD: ThermogravimetryFILE FORMAT: *csv (separated by commas); 2 columns: temperature [Celsius degree (column 1); mass loss [%] (Column 2).EQUIPMENT AND SOFTWARE: Star 850, Mettler ToledoANALYSIS METHOD DETAILS: Temperature range of 25-800 °C, heating ramp of 10 deg/min, air flow rate: 60 ml/minSAMPLE PREPARATION DETAILS: Samples dried at 110 ◦C. File: Catalytic resultsSignals from GC chromatography. Experimental data after reaction obtained for samples taken at the outlet of the microreactor.Reaction details:Deacetalization: benzaldehyde dimethyl acetal: water :1:1 molar ratioKnoevenagel condensation: benzaldehyde:ethyl cyanoacetate : 1:1 molar ratioTandem reaction: benzaldehyde dimethyl acetal: water: ethyl cyanoacetate (1:1:1 molar ratio)FILE DESCRIPTION:File name: Figure/Table Number_entry number/sample name_timeTable1/entry 1: chromatogram of the sample after deacetalization reaction in microreactor NH2-Zr-M- (silica modified with amine and zirconia)Table1/entry 2: : chromatogram of the sample after condensation reaction in microreactor NH2-Zr-M- (silica modified with amine and zirconia)Table1/entry 4: chromatogram of the sample after tandem reaction in microreactor NH2-Zr-M- (silica modified with amine and zirconia)Table1/entry 5: chromatogram of the sample after deacetalization reaction in microreactor Zr-M- (silica modified with zirconia)Table1/entry 6: chromatogram of the sample after condensation reaction in microreactor Zr-M- (silica modified with zirconia)Table1/entry 7: chromatogram of the sample after tandem reaction in microreactor Zr-M- (silica modified with zirconia)Table1/entry 8: chromatogram of the sample after deacetalization reaction in microreactor NH2-M (silica modified with amine)Table1/entry 10: chromatogram of the sample after tandem reaction in microreactor NH2-M (silica modified with amine)Fig2: chromatogram of the sample after deacetalization reaction in 1-cm-long microreactor Zr-M (silica modified with zirconia)Fig S3_ACN: chromatogram of the sample after condensation reaction in microreactor NH2-M (silica modified with amines, Acetonitrile as solvent)Fig S3_Toluene: chromatogram of the sample after condensation reaction in microreactor NH2-M (silica modified with amines, Toluene as solvent)Fig 6_Toluene_ACN chromatogram of the sample after tandem reaction in microreactor NH2-M (silica modified with amines, Toluene and acetonitrile solvent)Fig 6_Toluene_H2O chromatogram of the sample after tandem reaction in microreactor NH2-M (silica modified with amines, Toluene and water solvent)FigS5 chromatogram of the samples after tandem reaction in microreactor NH2-M (silica modified with amines, Toluene and water solvent at 80 degree temperature)FigS5_BATCH chromatogram of the sample after tandem reaction in batch reactor; catalysts NH2-Zr-M (silica modified with zirconia and amine)Fig7_KASKADE chromatogram of the sample after tandem reaction in cascade reactor; catalysts NH2-Zr-M (silica modified with zirconia and amine)RESEARCH METHOD: Gas ChromatographyFILE FORMAT: *csv (separated by commas); 2 columns: time [min](column 1); signal value (Column 2).EQUIPMENT AND SOFTWARE: Agilent 7890A, flame ionization detector FID; capillary column HP5ANALYSIS METHOD DETAILS: Inlet temperature: 250◦C ; sample volume: 1um, split ratio: 5:1; oven temp: 40◦C-200o◦C He flow 6.5 ml/min; detector: temperature 300◦C; H2 flow:30 ml/min, Air flow:400ml/minSAMPLE PREPARATION DETAILS: samples diluted in 2-propanol (5/1000 v/v) File: XRFData obtained from Wavelength-dispersive X-ray fluorescenceSample description: sample 1 – Zr conc. in 1 part; sample 2 – Zr conc. in 2 part; sample 3 – Zr conc. in 3 part; sample 4 – Zr conc. in 4 partRESEARCH METHOD: WD-XRFFILE FORMAT: *csv (separated by commas); 2 columns: element; element concentration [%]EQUIPMENT AND SOFTWARE: Spectrometer Axios mAX; Rh lamp, Malvern Panalytical’s SuperQManager softwareSAMPLE PREPARATION DETAILS: Sample preparation: Cereox binder (C38H76N2O2). Sample : binder ratio = 1 : 3. Homogenisation time approx. 1 min. File: FTIRData obtained from Diffuse reflectance infrared Fourier transform spectroscopySample description: NH2/Zr-M- sample after modification with amines naz zirconia; Zr-M- sample modified with zirconia, SiO2- silicaRESEARCH METHOD: FTIR DRIFTFILE FORMAT: *csv (separated by commas); 2 columns: wavenumber [cm-1]; transmitance [a.u]EQUIPMENT AND SOFTWARE: Nicolet 6700 (Thermo Scientific) device; DRIFT cell, OMNIC softwareANALYSIS METHOD DETAILS : spectras in the range of 4000-2500 cm-1; resolution of 4 cm−1;SAMPLE PREPARATION DETAILS: Sample preparation: samples diluted in KBr; 5%Sample in KBr Homogenisation time approx. 10 min.