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. 2025 Feb 26;30(5):1073.
doi: 10.3390/molecules30051073.

Influence of Aluminum Incorporation on the Adsorptive Performance of Silica-Based Supported Sulfonic Acid for the Chemical Recovery of Gaseous O-Xylene

Yaxu Wang  1 , Jiaxuan Chai  1 , Yining Li  1 , Zichuan Ma  1
Affiliations

Influence of Aluminum Incorporation on the Adsorptive Performance of Silica-Based Supported Sulfonic Acid for the Chemical Recovery of Gaseous O-Xylene

Yaxu Wang et al. Molecules. .

Abstract

A group of silica-based supports with varying Al/Si ratios (S-x) was synthesized using the sol-gel method, followed by a chlorosulfonic acid modification to produce supported sulfonic acids (SA-x). The S-x and SA-x materials, along with their adsorption products, were characterized via techniques such as FTIR, BET, and HPLC-MS. The analysis revealed that the sulfonic acid groups in the SA-x materials existed in two anchoring states: the covalently bonded (CB) state [SiOx-O]ɗ--SO3Hɗ+ and the ion-paired (IP) state AlOy+:OSO3H-. The sulfonation reactivity of the CB-state sulfonic acid was enhanced, whereas that of the IP-state counterpart was diminished. The incorporation of a minor quantity of aluminum ions (x = 0.1) markedly enhanced the adsorption efficiency of SAs for o-xylene, extending the reaction temperature range to 110-190 °C and increasing the breakthrough adsorption capacity (QB) to 946.1 mg g-1. However, excessive aluminum ion incorporation was detrimental to the adsorption performance of SAs for o-xylene. SA-0.1 showed superior adsorptive capabilities and excellent recyclability, maintaining its performance over four consecutive adsorption/regeneration cycles with only a minor decrease of 4.5%. These findings suggest that SAs prepared with a minor amount of aluminum ions have significant potential for application as adsorbents for the removal of benzene series pollutants.

Keywords: Al/Si ratios; CB-state; IP-state; adsorption; o-xylene.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Scheme 1
Scheme 1
Preparation process for the SA−x series.
Figure 1
Figure 1
(a) Relationship between o-xylene Xo–x and T for the SA−x series. Adsorption breakthrough curves for o-xylene in (b) SA−0, (c) SA−0.1, (d) SA−0.2, and (e) SA−0.3 at different temperatures.
Figure 2
Figure 2
SEM images and corresponding EDS spectra of S−0 (a), SA−0 (b), S−0.1 (c), SA−0.1 (d), S−0.2 (e), SA−0.2 (f), S−0.3 (g), SA−0.3 (h), S−0.5 (i), and SA−0.5 (j).
Figure 3
Figure 3
XRD patterns (a), N2 adsorption/desorption isotherms (c), and pore size distribution profiles (d) of the S-x supports; XRD patterns (b), N2 adsorption/desorption isotherms (e), and pore size distribution profiles (f) of the SA-x adsorbents.
Figure 4
Figure 4
(a) FTIR spectra of the supports; (b) FTIR spectra of the samples.
Figure 5
Figure 5
(a) Two anchoring states of the sulfonic acid and adsorption reaction equation of CB-state sulfonic acid with o-xylene; (b) NH3-TPD curves of SA−x materials.
Figure 6
Figure 6
(a) ESI-MS spectrum of adsorption product; (b) FTIR spectrum of adsorption product; and (c) reusability of SA−0.1 in repeated adsorption/desorption cycles.
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