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Publication raw data: “Zirconia functionalized monolithic cores with improved hierarchical porosity for continuous-flow microreactors in cascade reactions”

Version 1.0

Ciemięga, Agnieszka; Katarzyna Maresz; Julita Mrowiec-Białoń, 2025, "Publication raw data: “Zirconia functionalized monolithic cores with improved hierarchical porosity for continuous-flow microreactors in cascade reactions”", https://doi.org/10.18150/JCXFWD, RepOD, V1

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Description

File:ASAP

File format: *csv

Figure 1, 2, Table 1

Data from nitrogen adsorption/desorption measurements.

Isotherms and Pore Size Distribution (PSD)

ASAP2020 Micromeritics; ASAP2020 softwere

Samples degassed at 200 ◦C under vacuum for 24 h. Nitrogen adsorption at −196◦C. The specific surface area calculated using Braunauer, Emmet and Teller (BET) equation.


File:TG

File format: *csv

Data from thermogravimetric measurements of samples modified with amines: TG curves (%mass loss).

Star 850, Mettler Toledo. Temperature range of 25-800 °C, heating ramp of 10 deg/min, air flow rate: 60 ml/min


File:Flow resistance

File format: *csv

Figure 3

Data from flow resistance measurements.

Pressure controller UNIK 5000, Ex-Calibra, syringe pump.


File:RTD

File format: *csv

Figure 4, Table 2

Data from residence time distribution evaluation. Syrgine Pump, Temperature 25°C, 4 cm long microreactors with NH2-SIO2 or ZrO2-SiO2 monolithic cores. Sampling:0.5-1 min.


File:Catalytic Results

File format:*csv

Figure 5

Signals from GC chromatography

Agilent 7890A, flame ionization detector FID; capillary column HP5; 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/min


Subject
Chemistry; Engineering
Keyword

monolithic microreactor, improved porosity, zirconia-silica catalyst, cascade process

Related Publication

https://journals.pan.pl/dlibra/publication/153673/edition/134372/content doi: 10.24425/cpe.2025.153673

CC0 Creative Commons Zero 1.0 CC0 Creative Commons Zero 1.0

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ASAP.zip
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Data obtained from nitrogen absorption and desorption measurements- Isotherms and Pore Size Distribution (PSD). Sample description: ZrO2-SiO2 no treatment – silica-zirconia without modification; ZrO2-SiO2 acid – silica-zirconia after sulfuric acid treatment; ; ZrO2-SiO2 ammonia– silica-zirconia after ammonia treatment; ; ZrO2-SiO2 ammonia acid – silica-zirconia after sulfuric acid and ammonia treatment; SiO2- silica monolith; NH2-SiO2 – silica modified with amino groups RESEARCH METHOD: low temperature nitrogen adsorption FILE FORMAT: *csv (separated by commas); 2 columns: relative pressure (column 1); quantity adsorbed [cm^3/g] (Column 2). EQUIPMENT AND SOFTWARE: ASAP2020 Micromeritics; ASAP2020 software ANALYSIS 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.
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Catalytic results.zip
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Signals 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 ratio Knoevenagel condensation: benzaldehyde:ethyl cyanoacetate : 1:1 molar ratio Tandem reaction: benzaldehyde dimethyl acetal: water: ethyl cyanoacetate (1:1:1 molar ratio) FILE DESCRIPTION: File name: reaction_flow rate_sample name_sampling time Reaction: deacetalization, Knoevenagel, cascade Flow rate:0.03 ml/min, 0.08 ml/min, 0.12 ml/min Sample name: ZrO2-SiO2, NH2-SiO2, ZrO2-SiO2-NH2-SiO2 RESEARCH METHOD: Gas Chromatography FILE 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 HP5 ANALYSIS 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/min SAMPLE PREPARATION DETAILS: samples diluted in 2-propanol (5/1000 v/v).
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Flow_resistance.zip
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MD5: ea52756a0a8fa6cc41ab445b69d4246a
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Data from flow resistance measurements. Sample description: NH2-SiO2 low flow rate- silica modified with amines, flow rates from: 0.025 ml/min- 0.17 ml/min; NH2-SiO2 high flow rate- silica modified with amines, flow rates from: 0.17 ml/min- 7.14 ml/min; ZrO2-SiO2 low flow rate- zirconia-silica, flow rates from: 0.025 ml/min- 0.193 ml/min; ZrO2-SiO2 high flow rate- zirconia-silica, flow rates from: 0.051 ml/min- 0.554 ml/min. FILE FORMAT: *csv (separated by commas); 2 columns: flow rates [ml/min (column 1); pressure drop [kPa/cm] (Column 2). EQUIPMENT AND SOFTWARE: Pressure controller UNIK 5000, Ex-Calibra, syringe pump ANALYSIS METHOD DETAILS: Temperature 25°C, 4 cm long microreactors with NH2-SIO2 or ZrO2-SiO2 monolithic cores.
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RTD.zip
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Data from residence time distribution evaluation Sample description: 0.03 NH2-SiO2 Et– silica modified with amines, flow rate 0.03 ml/min, E(t) curve; 0.03 NH2-SiO2 Ft – silica modified with amines, flow rate 0.03 ml/min, F(t) curve; 0.08 NH2-SiO2 Et – silica modified with amines, flow rate 0.08 ml/min, E(t) curve; 0.08 NH2-SiO2 Ft – silica modified with amines, flow rate 0.08 ml/min, E(t) curve; 0.12 NH2-SiO2 Et – silica modified with amines, flow rate 0.12 ml/min, E(t) curve; 0.12 NH2-SiO2 Ft – silica modified with amines, flow rate 0.12 ml/min, E(t) curve; 0.03 ZrO2-SiO2 Et – zirconia-silica, flow rate 0.03 ml/min, E(t) curve; 0.03 ZrO2-SiO2 Ft – zirconia-silica, flow rate 0.03 ml/min, F(t) curve; 0.08 ZrO2-SiO2 Et – zirconia-silica, flow rate 0.08 ml/min, E(t) curve; 0.08 ZrO2-SiO2 Ft – zirconia-silica, flow rate 0.08 ml/min, F(t) curve; 0.12 ZrO2-SiO2 Et – zirconia-silica, flow rate 0.12 ml/min, E(t) curve; 0.12 ZrO2-SiO2 Ft – zirconia-silica, flow rate 0.12 ml/min, F(t) curve. FILE FORMAT: *csv (separated by commas); 2 columns: Time [min] (column 1); E(t) [-] (Column 2). EQUIPMENT AND SOFTWARE: Ex-Calibra, syringe pump ANALYSIS METHOD DETAILS: Temperature 25°C, 4 cm long microreactors with NH2-SIO2 or ZrO2-SiO2 monolithic cores. Sampling:0.5-1 min.
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TG.zip
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Data from thermogravimetric measurements of samples modified with amines: TG curves (%mass loss). Sample description: NH2-SiO2- silica modified with amine; RESEARCH METHOD: Thermogravimetry FILE FORMAT: *csv (separated by commas); 2 columns: temperature [Celsius degree (column 1); mass loss [%] (Column 2). EQUIPMENT AND SOFTWARE: Star 850, Mettler Toledo ANALYSIS METHOD DETAILS: Temperature range of 25-800 °C, heating ramp of 10 deg/min, air flow rate: 60 ml/min SAMPLE PREPARATION DETAILS: Samples dried at 110 ◦C.
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