13X@SiO2: Synthesis and Toluene Adsorption

doi:10.15541/jim20220449

Abstract

Abstract:

In practice, adsorbents such as 13X have strong hydrophilicity due to their low Si/Al ratio, whose competitive adsorption between vapour and volatile organic compounds (VOCs) often impairs the actual removal effect of VOCs on the adsorbents. Here, 13X was modified using CTABr as a templating agent and tetraethoxysilane (TEOS) as a silica source.Based on this modified 13X, a core-shell composites with 13X core and a mesoporous silica shell, named as 13X@SiO₂, was therefore synthesized. Its adsorption performance was tested by using toluene as a probe molecule under different humidity conditions on a penetration experimental device, compared with that of the pristine 13X. The results show that the adsorption capacity of sample 13X@SiO₂-2.6 (2.6 mL TEOS added in the preparation) was about 18% higher than that of 13X original sample under dry conditions. At 30% and 50% relative humidity, the optimum adsorption capacity of 13X@SiO₂ was increased by about 53% and 90%, respectively. In order to test the stability and reusability of the adsorbents, twice regeneration of sample 13X@SiO₂-2.6, treated for 2 h in situ desorption at 350 ℃, were performed, and the result showed that the regenerated sample 13X@SiO₂-2.6 still retained 90% of the original toluene adsorption capacity.

Key words: core-shell structure, composite material, hydrophobic modification, volatile organic compounds, adsorption

CLC Number:

TQ174

MA Xiaosen, ZHANG Lichen, LIU Yanchao, WANG Quanhua, ZHENG Jiajun, LI Ruifeng. 13X@SiO₂: Synthesis and Toluene Adsorption[J]. Journal of Inorganic Materials, 2023, 38(5): 537-543.

Figures/Tables 14

Fig. S1 Diagram of the penetration experimental apparatus

Fig. 1 XRD patterns of the samples of (a) 13X, (b, e) 13X@SiO2-2.2,(c, f) 13X@SiO2-2.6, and (d, g) 13X@SiO2-3.5 (A) Large angle XRD patterns; (B) Small angle XRD patterns

Fig. 2 SEM images of the samples (A) 13X; (B, E, F) 13X@SiO2-2.2; (C) 13X@SiO2-2.6; (D) 13X@SiO2-3.5

Fig. S2 SEM images and the corresponding EDS results of samples (A) 13X; (B) 13X@SiO2-2.2; (C) 13X@SiO2-2.6; (D) 13X@SiO2-3.5

Fig. 3 TEM images of the samples (A, B, E) 13X@SiO2-2.2; (C, D) 13X@SiO2-2.6

Fig. S3 (A) Nitrogen adsorption-desorption isothermal curves and (B) the corresponding pore size distributions decided by a DFT model of samples

Table 1 Textural properties of the samples

Sample	S_BET/(m²·g^-1)	S_ext/(m²·g^-1)	S_mic/(m²·g^-1)	V_mic/(cm³·g^-1)	V_mes/(cm³·g^-1)
13X	314	14	299	0.11	0.02
13X@SiO₂-2.2	324	95	229	0.09	0.07
13X@SiO₂-2.6	337	130	207	0.08	0.09
13X@SiO₂-3.5	444	259	184	0.07	0.18

Fig. S4 FT-IR spectra of the sample (a) 13X; (b) 13X@SiO2-2.2; (C) 13X@SiO2-2.6; (D) 13X@SiO2-3.5

Fig. S5 Images of water droplets on the surfaces of different samples

Fig. 4 Adsorption of toluene on the different adsorbents under dry condition (A) Adsorption breakthrough curves; (B) Saturated adsorption capacity; (C) Comparison of the breakthrough times; (D) Cumulative adsorption capacity of different adsorbents

Fig. S6 (A) Toluene adsorption breakthrough curves and (B) cumulative toluene adsorption capacity of SiO2 under dry condition

Fig. 5 Adsorption of toluene on the different adsorbents under 30% relative humid conditions (A) Adsorption breakthrough curves; (B) Saturated adsorption capacity; (C) Comparison of the breakthrough time; (D) Cumulative adsorption capacities of different adsorbents of toluene

Fig. 6 Adsorption of toluene on the different adsorbents under 50% relative humid conditions (A) Adsorption breakthrough curves; (B) Saturated adsorption capacity; (C) Comparison of the breakthrough time; (D) Cumulative adsorption capacity of different adsorbents of toluene

Fig. S7 (A) Adsorption of toluene on different adsorbents with triple adsorption-desorption cycle. Adsorption penetration curve and (B) saturated adsorption capacity under 50% relative humid conditions

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13X@SiO₂: Synthesis and Toluene Adsorption

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