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Link to original content: https://pubmed.ncbi.nlm.nih.gov/32092961
Sorption of CO2 and CH4 on Raw and Calcined Halloysite-Structural and Pore Characterization Study - PubMed Skip to main page content
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. 2020 Feb 19;13(4):917.
doi: 10.3390/ma13040917.

Sorption of CO2 and CH4 on Raw and Calcined Halloysite-Structural and Pore Characterization Study

Anna Pajdak  1 , Norbert Skoczylas  1 , Arkadiusz Szymanek  2 , Marcin Lutyński  3 , Piotr Sakiewicz  4
Affiliations

Sorption of CO2 and CH4 on Raw and Calcined Halloysite-Structural and Pore Characterization Study

Anna Pajdak et al. Materials (Basel). .

Abstract

The article presents comparative characteristics of the pore structure and sorption properties of raw halloysite (R-HAL) and after calcination (C-HAL) at the temperature of 873 K. Structural parameters were determined by optical scanning and transmission electron microscopy methods as well as by mercury porosimetry (MIP, Hg) and low-pressure nitrogen adsorption (LPNA, N2, 77 K). The surface area parameter (LPNA) of halloysite mesopores before calcination was 54-61 m2/g. Calcining caused the pore surface to develop to 70-73 m2/g. The porosity (MIP) of halloysite after calcination increased from 29% to 46%, while the surface area within macropores increased from 43 m2/g to 54 m2/g. The total pore volume within mesopores and macropores increased almost twice after calcination. The course of CH4 and CO2 sorption on the halloysite was examined and sorption isotherms (0-1.5 MPa, 313 K) were determined by gravimetric method. The values of equilibrium sorption capacities increased at higher pressures. The sorption capacity of CH4 in R-HAL was 0.18 mmol/g, while in C-HAL 0.21 mmol/g. CO2 sorption capacities were 0.54 mmol/g and 0.63 mmol/g, respectively. Halloysite had a very high rate of sorption equilibrium. The values of the effective diffusion coefficient for methane on the tested halloysite were higher than De > 4.2 × 10-7 cm2/s while for carbon dioxide De > 3.1 × 10-7 cm2/s.

Keywords: effective diffusion coefficient; halloysite; kinetics of diffusion; pore structure; sorption capacity of CH4 and CO2.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
IGA 001 gravimetric gas sorption analyser.
Figure 2
Figure 2
SEM image of the microstructure of the surface of raw halloysite R-HAL and chemical composition determined by an X-ray dispersion energy spectrometer (EDS).
Figure 3
Figure 3
SEM image of the microstructure of the surface of calcined halloysite C-HAL and chemical composition determined by an X-ray dispersion energy spectrometer (EDS).
Figure 4
Figure 4
TEM images of raw halloysite samples showing halloysite nanoplates and nanotubes: (a) bright field (BF); (b) dark field (DF).
Figure 5
Figure 5
N2 sorption isotherms of halloysites R-HAL and C-HAL, 77K (LPNA method).
Figure 6
Figure 6
Distribution of pore volume as a function of their diameter in halloysites (LPNA method, BJH model).
Figure 7
Figure 7
Pore size distribution in halloysites (LPNA method, NLDFT model).
Figure 8
Figure 8
Distribution of pore volume as a function of their diameter in halloysite (MIP method) drawn.
Figure 9
Figure 9
Sorption isotherms of raw halloysite: (a) CH4 sorption isotherm; (b) CO2 sorption isotherm.
Figure 10
Figure 10
Sorption isotherms of calcined halloysite: (a) CH4 sorption isotherm; (b) CO2 sorption isotherm.
Figure 11
Figure 11
Diffusion kinetics of raw halloysite: (a) diffusion kinetic of CH4; (b) diffusion kinetic of CO2.
Figure 12
Figure 12
Diffusion kinetics of C-HAL calcined halloysite: (a) diffusion kinetic of CH4; (b) diffusion kinetic of CO2.
See this image and copyright information in PMC

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