Metrics
1 Download
Share Dataset

Share this dataset on your favorite social media networks.

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

Version 2.0

Ciemięga, Agnieszka, 2024, "Publication raw data: Bifunctionalized acid-base hierarchically structured monolithic microreactor for continuous-flow tandem catalytic processes of cyanocinnamte synthesis", https://doi.org/10.18150/ICLHSU, RepOD, V2

Learn about Data Citation Standards.

Description

Data collected for the publication entitled: “Bifunctionalized acid-base hierarchically structured monolithic microreactor for continuous-flow tandem catalytic processes of cyanocinnamte synthesis”

 

File: Acidicy

Data obtained from IR absorption measurements on amine/zirconia/silica sample exposed to pyridine vapors.

RESEARCH METHOD: Fourier transform infrared spectroscopy

FILE 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: ASAP

Data 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 silica

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.

 

File: TG

Data 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: 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.

 

File: Catalytic results

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: Figure/Table Number_entry number/sample name_time

Table1/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 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) 


File: XRF

Data obtained from Wavelength-dispersive X-ray fluorescence

Sample 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 part

RESEARCH METHOD: WD-XRF

FILE FORMAT: *csv (separated by commas); 2 columns: element; element concentration [%]

EQUIPMENT AND SOFTWARE: Spectrometer Axios mAX; Rh lamp, Malvern Panalytical’s SuperQManager software

SAMPLE PREPARATION DETAILS: Sample preparation: Cereox binder (C38H76N2O2). Sample : binder ratio = 1 : 3. Homogenisation time approx. 1 min.

 

File: FTIR

Data obtained from Diffuse reflectance infrared Fourier transform spectroscopy

Sample description: NH2/Zr-M- sample after modification with amines naz zirconia; Zr-M- sample modified with zirconia, SiO2- silica

RESEARCH METHOD: FTIR DRIFT

FILE FORMAT: *csv (separated by commas); 2 columns: wavenumber [cm-1]; transmitance [a.u]

EQUIPMENT AND SOFTWARE: Nicolet 6700 (Thermo Scientific) device; DRIFT cell, OMNIC software

ANALYSIS 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.

Subject
Chemistry; Engineering
Keyword

microreactors, bifunctional catalysts, tandem reactions

Related Publication

Ciemięga, A., Maresz, K. & Mrowiec-Białoń, J. Bifunctionalised acid-base hierarchically structured monolithic microreactor for continuous-flow tandem catalytic process of cyanocinnamate synthesis. Sci Rep 14, 25332 (2024). https://doi.org/10.1038/s41598-024-77146-7 https://doi.org/10.1038/s41598-024-77146-7 doi: 10.1038/s41598-024-77146-7

CC BY - Creative Commons Attribution 4.0 CC BY - Creative Commons Attribution 4.0

Find
1 to 6 of 6 Files
TG.zip
ZIP Archive - 10.7 KB - Jun 3, 2024 - 0 Downloads
MD5: 9ff91953e774d34de0a7080d82983023
License: CC BY - Creative Commons Attribution 4.0
Data 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: 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.
Download
Acidicy.zip
ZIP Archive - 5.8 KB - Jun 3, 2024 - 1 Download
MD5: 036c51efbb9c902d6278bb6915792c96
License: CC BY - Creative Commons Attribution 4.0
Data obtained from IR absorption measurements on amine/zirconia/silica sample exposed to pyridine vapors. RESEARCH METHOD: Fourier transform infrared spectroscopy FILE 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
Download
ASAP.zip
ZIP Archive - 6.9 KB - Jun 3, 2024 - 0 Downloads
MD5: 229e9fb995794fd83eaacb95dce2e16c
License: CC BY - Creative Commons Attribution 4.0
Data 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 silica 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.
Download
Catalytic_results.zip
ZIP Archive - 13.9 MB - Jun 3, 2024 - 0 Downloads
MD5: 23e23cfb23cbba888a187cf0d95b5004
License: CC BY - Creative Commons Attribution 4.0
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: Figure/Table Number_entry number/sample name_time Table1/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 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)
Download
FTIR.zip
ZIP Archive - 63.6 KB - Feb 3, 2025 - 0 Downloads
MD5: e91dcb13efe5d8de6186364f59d8737b
License: CC BY - Creative Commons Attribution 4.0
Data obtained from Diffuse reflectance infrared Fourier transform spectroscopy Sample description: NH2/Zr-M- sample after modification with amines naz zirconia; Zr-M- sample modified with zirconia, SiO2- silica RESEARCH METHOD: FTIR DRIFT FILE FORMAT: *csv (separated by commas); 2 columns: wavenumber [cm-1]; transmitance [a.u] EQUIPMENT AND SOFTWARE: Nicolet 6700 (Thermo Scientific) device; DRIFT cell, OMNIC software ANALYSIS 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.
Download
XRF.zip
ZIP Archive - 937 B - Feb 3, 2025 - 0 Downloads
MD5: 87fcee979d947c634692242699a31697
License: CC BY - Creative Commons Attribution 4.0
Data obtained from Wavelength-dispersive X-ray fluorescence Sample 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 part RESEARCH METHOD: WD-XRF FILE FORMAT: *csv (separated by commas); 2 columns: element; element concentration [%] EQUIPMENT AND SOFTWARE: Spectrometer Axios mAX; Rh lamp, Malvern Panalytical’s SuperQManager software SAMPLE PREPARATION DETAILS: Sample preparation: Cereox binder (C38H76N2O2). Sample : binder ratio = 1 : 3. Homogenisation time approx. 1 min.
Download
Select File(s)

Please select a file or files to be deleted.

Delete Files

The file(s) will be deleted after you click on the Delete button.

Files will not be removed from previously published versions of the dataset.

Select File(s)

Please select a file or files to be edited.

Select File(s)

Please select a file or files to be edited.

Select File(s)

Please select a file or files to be edited.

Edit license

For selected file(s) set a license to

Select File(s)

Please select a file or files to be downloaded.

Select File(s)

Please select a file or files for access request.

Select File(s)

Please select restricted file(s) to be unrestricted.

Request Access

  You need to Log In/Sign Up to request access to this file.

Continue
Dataset Terms

Please confirm and/or complete the information needed below in order to continue.

Asterisks indicate required fields

Request Access

Access to file(s) subject to additional consent under following conditions:

Accept
Package File Download
Restricted Files Selected

The restricted file(s) selected may not be downloaded because you have not been granted access.

Restricted Files Selected

The restricted file(s) selected may not be downloaded because you have not been granted access.

Click Continue to download the files you have access to download.

Delete Dataset

Are you sure you want to delete this dataset and all of its files? You cannot undelete this dataset.

Embargo

Embargo

Are you sure you want to lift the embargo?

Once you lift the embargo, you will not be able to set it again.

Delete Draft Version

Are you sure you want to delete this draft version? Files will be reverted to the most recently published version. You cannot undelete this draft.

Dataset Private URL

Use a Private URL to allow those without Dataverse accounts to access your dataset. For more information about the Private URL feature, please refer to the User Guide.

Private URL has not been created.

Dataset Private URL

Are you sure you want to disable the Private URL? If you have shared the Private URL with others they will no longer be able to use it to access your dataset.

Submit for Review

You will not be able to make changes to this dataset while it is in review.

Submit
Publish Dataset

This dataset cannot be published until Institute of Chemical Engineering PAS is published. Would you like to publish both right now?

Once you publish this dataset it must remain published.

Publish Dataset

Are you sure you want to republish this dataset?

Select if this is a minor or major version update.

Publish Dataset

This dataset cannot be published until Institute of Chemical Engineering PAS is published by its administrator.

Publish Dataset

This dataset cannot be published until Institute of Chemical Engineering PAS and RepOD are published.

Return for modification


Send a copy of this message to the return e-mail address.
OK
Deaccession Dataset

Are you sure you want to deaccession? The selected version(s) will no longer be viewable by the public.