An Open Framework Chalcogenide Supertetrahedral cluster as Visible

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An Open Framework Chalcogenide Supertetrahedral cluster as Visible-Light driven Photocatalysts for Selective Degradation Huan Pei, and Li Wang Cryst. Growth Des., Just Accepted Manuscript • DOI: 10.1021/acs.cgd.9b00685 • Publication Date (Web): 16 Aug 2019 Downloaded from pubs.acs.org on August 21, 2019

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Crystal Growth & Design

An Open Framework Chalcogenide Supertetrahedral cluster as Visible-Light driven Photocatalysts for Selective Degradation Huan Pei,a Li Wang,* ,a College of Chemistry & Chemical Engineering, Xinjiang Normal University, Urumqi 830054, China

ACS Paragon Plus Environment

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Crystal Growth & Design 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

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ABSTRACT: Selective photocatalytic decomposition of mixed pollutants is an effective approach to environmental remediation, yet still in its infancy. We present the syntheses, structural characterization of a crystalline open framework chalcogenide (Heta)6[In10S10Se8]•10H2O (Heta = ethanolamine-H+) (1) constructed from T3 supertetrahedral clusters. It is a 3D two-fold interpenetrated framework with protonated ethanolamine located in pores. This compound exhibits efficient and selective photocatalytic activities in the photodegradation of four kinds of organic dyes with similar backbone but different charges and sizes. Compound 1 shows excellent photodegradation of Methylene Blue upon visible-light irradiation due to the strong oxidization of superoxide radical (O2−•) generated in the photocatalytic process. The selective photocatalytic activities is related to the integration of appropriate band structures with distinct affinity and selectivity to organic dyes molecules.


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Introduction Currently, water pollution is still one of the most serious problems threatening public health, although many efforts have been made in water treatment. Semiconductor photocatalysis technology has been applied to the removal of organic pollutants in water and other media.1-3 Selective photocatalytic decomposition of mixed pollutants is effective in environmental remediation, yet much work is to be done.4 Traditionally, most visible-light-responsive photocatalysts are based on non-porous materials such as metal or nonmetal doped TiO2,5 metal doped WO3,6 Ag3PO4,7 BiVO4,8 BiOCl9 etc.. Crystalline open framework chalcogenide superlattices have attracted more and more attention because they can combine porosity with semi-conductivity. They have been a research subject in various areas ranging from fundamental optoelectronic chemistry to practical applications.10-14 Especially, driven by visible light, they have been applied to photocatalytic hydrogen production and decomposition of organic pollutants because of their large surface areas, numerous reactive sites, and the tunable band gaps.15 More importantly, possessing positive or negative charges, these chalcogenide superlattices can selectively separate organic dyes with similar molecular sizes because of the charge effect.15,16 In recent years, a few compounds in this family have been successfully applied to selective photocatalysis and separation process based on the charge and size dependent effects.16,17 Although considerable successful attempts have been performed to prepare open framework chalcogenide, those being capable of selective adsorption and separation in photocatalysis is still in its first step.17 Herein, a novel crystalline chalcogenide superlattice ([In10S10Se8]6-) constructed from T3 supertetrahedral cluster was synthesized and structurally characterized. Experimentally, driven by visible light, this compound exhibited efficient and selective photocatalytic activities in the


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photodegradation of two cationic dye molecules with different sizes, i.e., Methylene Blue (MB) and Rhodamine B (RhB) against two anionic dye molecules Methyl Orange (MO) and Kermes Red (KR). The integration of favorable band structures and distinct affinity and selectivity to different guest molecules in such supertetrahedral cluster makes it an excellent candidate for efficient and selective photocatalytic processes. Demonstrating selective photocatalytic decomposition of organic dyes, this is the first example of open framework chalcogenide constructed from T3 supertetrahedral clusters with determined a single crystalline structure. Experimental Section Synthesis. All the starting materials were analytical grade from commercial sources. S (0.0334 g, 1.04 mmol), Se (0.0335 g, 0.42 mmol), and InCl3 (0.0720 g, 0.33 mmol) in a molar ratio of 3.2:1.3:1.0 and ethanolamine (4.0 mL), H2O (2.0 mL) was mixed in a Teflon-lined stainless container (23 mL) and stirred for 1 hour at room temperature. The reaction vessel was placed in an oven and heated up to 160 °C for 96 hours. Following slow cooling of the autoclave to

room

temperature,

a

large

number

of

pale-yellow

octahedral

crystals

of

(Heta)6[In10S10Se8]•10H2O (Heta = ethanolamine-H+) (1) were obtained by filtration, yield 85-90 % based on In. Elemental analyses for 1 (wt %) Calc: C 5.43, H 2.56, N 3.16, S 12.06; Found: C 5.74, H 2.37, N 3.27, S 12.25. Apparatus and Characterization. Single crystal XRD was measured on a Bruker APEX-II CCD and Cu Kα radiation (λ = 1.54178 Å) at 190(2) K and integrated with the SAINT program. Direct methods were used to determine the structure and the structure was refined by full-matrix least-squares fitting on F2 with SHELXTL-97 software package18 checked with PLATON.19 Tables S1, S2, S3 and S4 show crystal data, the atomic coordinates, selected bond distances and bond angles. The powder X-ray diffraction patterns was measured on a Bruker D8 ADVANCE


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X-ray diffractometer using Cu Kα radiation (λ = 1.54178 Å) (2θ = 5−60°). IR was measured on Shimadzu IR Affinity-1 (400−4000 cm-1). Thermal analysis was measured on NETZSCH STA 449F3. UV-Vis diffuse reflectance spectroscopy was recorded on ShimadzuSolidSpec-3700DUV spectrophotometer between 350-800 nm wavelength ranges. The U-3310 UV-visible absorption spectrophotometer was used to monitor the photocatalytic process. The photocatalytic performance. A Pyrex beaker (250 mL) was used as the photoreaction vessel and a 300 W Xe lamp (cut off wavelength of filter λ ≥ 400 nm) was used as the light source. 50 mg of compound 1 was added to the 100 mL of organic dye aqueous solutions containing 1.0 × 10−5 M of MB, RhB, MO and KR. Results and Discussions Crystal Structure. Compound 1 crystallizes in tetragonal space group P43212 (No. 96) (for crystallographic data details, see Table S1). The asymmetric unit consists of ten unique In and eighteen S atoms. Among them, sixteen S positions are partially mixed with Se atoms with an occupation rate of approximately 38-62%, except for the terminal S(27) and S(28) which are all fully occupied (Table S2). Each In atoms is coordinated by four S/Se atoms, forming an In(S/Se)4 tetrahedron with In-(S/Se) distances varying from 2.455 to 2.547 Å (Table S3). In a typical T3 [In10S12Se8]10- cluster, there are 12 bicoordinated S/Se on 6 edges, 4 tricoordinated S/Se on 4 planes, and the four terminal S2- ions (Figure 1a). The terminal S2- sites are linked by other 4 clusters to form a three-dimensional open framework with two-fold interpenetration structure. One framework affords rectangular tunnel sized 16.2 × 11.2 Å2 along the [100] direction and equilateral triangular tunnel sized 21.7 Å along the [111] direction (Figure 1b and c). After the two-fold interpenetration, there are approximate 16.2 × 6.4 Å2 rectangular channels


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along the [111] direction (Figure 1d) with 53 % of void space filled by protonated ethanolamine located in channels. Single crystal diffraction, elemental analysis, IR and TG established the formula (Heta)6[In10S10Se8]•10H2O. The S:Se ratio of 5:4 was also determined by experiments of ICP-MS (Table S5). Figure S1 shows that simulated PXRD of compound 1 is in accordance with the experimental data.

Figure 1. (a) The structural diagram of a regular T3 cluster [In10S12Se8]10-. Simplified framework views along (b) the [100] direction and (c) the [111] direction. (d) A two-fold interpenetration of two sets interspersed with each other.

IR spectrum Analysis. IR spectra of ethanolamine and compound 1 were shown in Figure S2. The band around 3380 cm−1 was assigned to the stretching of hydroxyl groups. Two vibrations at 1606 and 1490 cm−1 were assigned to symmetric and asymmetric bending of -NH2. The vibrational bands of the C–O group appeared at 1060 cm−1.20 It was observed that the intensity of


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those signals of protonated amines located in channels was lower in comparison with the ethanolamine. Thermogravimetric Analysis. The weight loss of ∼6.95 % in the first stage was observed between room temperature and 212 °C, which was caused by the weight loss of solvent water molecules (calcd. 6.78 %). Then a weight loss of ∼13.95 % was observed between 212∼412 °C, which corresponds to the total weight of solvent ethanolamine molecules (calcd. 14.02 %) (Figure S3). The selective photocatalytic activities. Four dyes with different charges and sizes were chosen (Figure S4) to probe the correlation between the structure of organic dyes and selective photocatalytic property of compound 1. A cationic dye molecule (MB, 5.30 × 14.27 × 4.89 Å3) and an anionic dye molecule (MO, 5.10 × 15.07 × 4.10 Å3) with similar size were selected to study the charge effect. Figure 2a and Figure S5 (a) show the percentage of remaining concentration of these two organic dyes with respect to time under visible light irradiation. The residual concentration (the percentage of C/Co) of a MB aqueous solution significantly decreased to 0.08 % of the initial concentration upon elongating the irradiation time to 16 min. As for MO aqueous solution, the residual concentration remained at a high level of 90.84 % of the initial concentration upon elongating the irradiation time to 840 min (Figure S 5b). We also used a mixture of MB and MO solution with the same concentration of each dye to study charge effect. The residual concentration of MB decrease dramatically while that of MO slightly decreased, showing a selective decomposition capability of the anionic chalcogenide framework towards MB+ (Figure 3a). The above results show that the negative charge of supertetrahedral clusters [In10S12Se8]10- allows the cationic dye of MB+ to be absorbed on the surface of the catalyst.


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Figure 2. (a) UV-vis spectra of MB. (b) Degradation curve of MB. (c) UV-vis spectra of RhB. (d) Degradation curve of RhB.

Figure 3. Photocatalytic decomposition of a mixed solution (a) MB and MO and (b) MB and RhB.

We next studied the selectivity with respect to the size of the dye molecules, two cationic dye molecules with different dynamic sizes MB (5.30 × 14.27 × 4.89 Å3) and RhB (11.79 × 14.87 × 6.76 Å3) were selected. These two molecules have cationic chromophores with different sizes, making them ideal for studying the size effect. As shown in Figure 2, the residual concentration of a MB aqueous solution significantly decreased to 0.08 % of the initial concentration at 16 min while that of RhB did not change upon prolonging the irradiation time to 16 min (Figure 2a). After increasing the irradiation time to 840 min, residual concentration of RhB slowly decreased


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to 1.9 % of the initial concentration (Figure 2b). We then used the mixed dye solutions of MB and RhB to study the size-dependent effect. The residual concentration of MB lowered dramatically with time while that of RhB slightly decreased upon prolonging the irradiation time to 16 min (Figure 3b). The irradiation time needed to decompose RhB solution to the 1.9 % level was 840 min. The ln(C0/C) of MB and RhB aqueous solution is proportional to the irradiation time, which means that the photodegradation of these two dyes follows a first-order kinetic reaction rule. The apparent rate constant (k) of the photodegradation of MB is 0.309 min-1, 62 times of that of RhB (0.005 min-1) (Figure S6). As control experiments, we also monitored the concentration change of MB and RhB without catalyst or without visible light irradiation. The results indicated that the catalyst and light were essential for photocatalytic degradation. We further tested another anionic dye molecule (KR, 11.34 × 15.03× 6.27 Å3) with the same molecules size of RhB but opposite charges. The residual concentration of KR decreased to 84.61% of the initial concentration upon elongating the irradiation time to 840 min, proving that the negative charge of [In10S12Se8]10- supertetrahedral clusters rejected the adsorption of the anionic dye of KR molecules on the surface of the catalyst (Figure S 5b). The photocatalytic mechanism. UV-Vis-NIR spectroscopy shows that the absorption of compound 1 drops sharply from 375 nm (Figure 4a) and the optical band gaps were estimated to be 2.82 eV by Tauc’s equation21,22 (Figure 4b). The estimated VB and CB edge potential is 1.69 and -1.13 eV respectively using the equation EVB = X − Ee + 0.5Eg. The E ɵ (•OH/H2O) (2.27 V vs NHE) is more positive than VB potential, indicating that photogenerated-holes cannot oxidize H2O to give •OH. The CB potential is more negative than E ɵ (O2/O2−•) (-0.28 V), and thus photogenerated electrons can reduce the adsorbed O2 to produce O2−•, a strong oxidant4 (Figure S7). When we introduce


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benzoquinone (O2−• scavenger) to the photocatalysis system, only 56% of MB was degraded confirming that O2−• is an active species (Figure S8) in the process. Compound 1 shows a similar photocatalytic efficiency in three cycles of photocatalytic process (Figure 5) and PXRD patterns and IR are the same as pristine one which means that it is photo-stable (Figure S1 and Figure S2).

Figure 4. (a) UV-vis absorption spectrum and (b) (F(R)hν)1/2 as a function of hν of compound 1.

Figure 5. The residual concentration of MB in the presence of 1 over 3 cycles.

We compared the photocatalytic decomposition of MB with narrow band gap semiconductor CdS (81.2 m2g−1, 0.38 cm3g−1) and zeolite with pore distribution of 10-20 Å under the same condition. The residual concentration of a MB decreased to 41.4 % and 93.6%, respectively, after 16 min with CdS and zeolite as catalysts under visible light irradiation (Figure S9). We also compared the photocatalytic performance of 1 with a commercial TiO2 powder (P25). The


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apparent rate constants of MB with 1 was 9.09 times of that of TiO2 (Figure S10). This result may be due to the fact that anionic open framework helps increasing the number of active reaction sites and improving charge adsorption of the dyes on the catalyst surface. We compared further the photocatalytic performance of 1 and SOF-211, and found the apparent photodegradation rate constants of MB to be 6.18 times of that of SOF-2. Conclusions In conclusion, an open framework chalcogenide (Heta)6[In10S10Se8]•10H2O based on supertetrahedra T3 cluster was used as efficient and selective photocatalyst. The open framework chalcogenide exhibited both size and charge selectivity in photocatalytic decomposition of organic dyes. We anticipate that the demonstrated performance of the open frameworks chalcogenide promise a new opportunity of selective photocatalysts for applications such as decomposition organic mixed pollutants. ASSOCIATED CONTENT Supporting Information CIF file, final coordinates, selected bond distances, bond angles, XRD patterns, IR, TG. These materials are available free of charge via the Internet at http://pubs.acs.org. CCDC number of (Heta)6[In10S10Se8]•10H2O is 1898079. AUTHOR INFORMATION Corresponding Authors * E-mail: [email protected] (L. Wang) Author Contributions a

These authors contributed equally to this work.


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Notes The authors declare no competing financial interests. ACKNOWLEDGMENT This work is supported by the National Natural Science Foundation of China (NSFC, Grant No. 51762039), Tianshan Xue Song Program “Xinjiang Youth Top Talent Backup Project” (Grant No. 2017XS03) REFERENCES (1) Elimelech, M.; Phillip, W. A. The future of seawater desalination: energy, technology, and the environment. Science 2011, 333, 712-717. (2) Shannon, M. A.; Bohn, P. W.; Elimelech, M.; Georgiadis, J. G.; Marinas, B. J.; Mayes, A. M. Science and technology for water purification in the coming decades. Nature 2008, 452, 301−310. (3) Qin, Q.; Hao, J.; Zheng, W. J. Ni/Ni3C core/shell hierarchical nanospheres with enhanced electrocatalytic activity for water oxidation. ACS Appl. Mater. Interfaces 2018, 10, 17827-17834. (4) Kou, J.; Lu, C.; Wang, J.; Chen, Y.; Xu, Z.; Varma, R. S. Selectivity enhancement in heterogeneous photocatalytic transformations. Chem. Rev. 2017, 117, 1445-1514. (5) Pelaez, M.; Nolan, N. T.; Pillai, S. C.; Seery, M. K.; Falaras, P.; Kontos, A. G.; Dunlop, P. S. M.; Hamilton, J. W. J.; Byrne, J. A.; O’Shea, K.; Entezari, M. H.; Dionysiou, D. D. A review on the visible light active titanium dioxide photocatalysts for environmental applications. Appl. Catal. B: Environ. 2012, 125, 331−349. (6) Kim, J.; Lee, C. W.; Choi, W. Platinized WO3 as an environmental photocatalyst that generates OH radicals under visible light. Environ. Sci. Technol. 2010, 44, 6849−6854. (7) Huang, G.; Ma, Z.; Huang, W.; Tian, Y.; Jiao, C.; Yang, Z.; Wan, Z.; Pan, A. Ag3PO4


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For Table of Contents Use Only

An Open Framework Chalcogenide Supertetrahedral cluster as Visible-Light driven Photocatalysts for Selective Degradation Huan Pei,a Li Wang,* ,a College of Chemistry & Chemical Engineering, Xinjiang Normal University, Urumqi 830054, China

Table of Contents Graphic and Synopsis

Novel open framework chalcogenide (Heta)6[In10S10Se8]•10H2O based on T3 supertetrahedral clusters demonstrated efficient and selective photocatalytic decomposition of organic pollutants.


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An Open Framework Chalcogenide Supertetrahedral cluster as Visible

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