Degradation of Methylene Blue and Rhodamine B Using a New Visible Light-Responsive Photocatalyst, KSb2PO8-x N y

doi:10.1007/s40195-016-0401-6

Abstract

Abstract:

Potassium phosphatoantimonates, KSb₂PO₈ (KSbPO) and KSb₂PO_8-_x N _y (KSbPON), are prepared by solid-state method. Urea is employed as a source of nitrogen for N-doping. Structural, morphological and optical properties of both KSbPO and KSbPON are characterized by powder X-ray diffraction (PXRD), scanning electron microscopy, energy-dispersive spectroscopy, Fourier transform infrared spectroscopy and UV-visible diffuse reflectance spectroscopy. Both samples are found to crystallize in a monoclinic lattice with Cc space group. The d-lines of KSbPO and KSbPON are refined by least square fitting the PXRD data, using POWD software to obtain their unit cell parameters. The bandgap energy (E _g) of both pristine and N-doped KSbPO is found from their Kubelka-Munk plot. The KSbPON/visible photocatalytic degradation of methylene blue and rhodamine B has been investigated in aqueous heterogeneous suspension. The generation of ·OH in the presence of KSbPON during the photoreaction is verified by a fluorescence technique using terephthalic acid (TA) as a probe.

Key words: Potassium, phosphatoantimonates, Characterization, Organic, dyes, Photodegradation

G. Ravi, CH. Sudhakar Reddy, K. Sreenu, Ravinder Guje, Radha Velchuri, M. Vithal. Degradation of Methylene Blue and Rhodamine B Using a New Visible Light-Responsive Photocatalyst, KSb₂PO_8-_x N _y[J]. Acta Metallurgica Sinica (English Letters), 2016, 29(4): 335-343.

Figures/Tables 13

Fig. 1 Schematic structure of KSb2PO8

Fig. 2 XRD patterns of a KSbPO and KSbPON, b expanded XRD patterns of KSbPO and KSbPON. Insets show the colour of the samples

Table 1 Observed and calculated d-values along with their hkl values for the KSbPO and KSbPON

h k l	KSbPO		KSbPON
h k l	d _obs	d _cal	d _obs	d _cal
0 0 2	7.4637	7.4634	7.4715	7.4737
1 1 0	6.1258	6.1257	6.1319	6.1334
2 0 0	6.1258	6.1151	6.1319	6.1259
-1 1 1	5.7711	5.7712	5.7752	5.7775
1 1 1	5.5684	5.5685	5.5705	5.5764
-2 0 2	4.9851	4.9849	4.9906	4.9906
1 1 2	4.6211	4.6212	4.6223	4.6281
2 0 2	4.5117	4.5109	4.5117	4.5198
-1 1 3	3.9621	3.9620	3.9645	3.9664
1 1 3	3.7698	3.7694	3.7738	3.7752
0 2 0	3.5387	3.5388	3.5444	3.5425
-2 0 4	3.3400	3.3399	3.3426	3.3434
-1 1 4	3.2616	3.2615	3.2716	3.2712
1 1 4	3.1172	3.1173	3.1251	3.1220
3 1 2	3.0895	3.0896	3.0937	3.0952
2 0 4	3.0576	3.0575	3.0583	3.0562
-2 2 1	3.0309	3.0309	3.0351	3.0344
2 2 1	2.9706	2.9707	2.9902	2.9895

Table 2 Unit cell parameters and volumes of KSbPO and KSbPON

Samples	a(Å) ± (0.005)	B(Å) ± (0.005)	c (Å) ± (0.005)	β (°)	Vol (Å)³
KSbPO	12.29	7.078	15.00	95.83	1298.78
KSbPON	12.31	7.08	15.02	95.78	1304.15

Fig. 3 FTIR spectra of KSbPO and KSbPON in the regions a 400-1200 cm-1, b 1200-1600 cm-1

Table 3 Vibration bands observed for KSbPO and KSbPON (cm-1)

KSbPO	KSbPON
487	473
517	503
567	551
628	617
677	665
744	734
799	787
821	814
1021	1009
1051	1038
1106	1098
1134	1123
1221	1207
-	1260
-	1330
-	1425
-	1490

Fig. 4 Thermogravimetric profile of KSbPON

Fig. 5 SEM-EDS of a1-a4 KSbPO and b1-b4 KSbPON

Fig. 6 UV-Vis a absorption and b EDS profiles of KSbPO and KSbPON

Fig. 7 UV-Vis absorption spectra of MB and RhB dye at 0 and 180 min under visible light irradiation in the presence of KSbPO

Fig. 8 a Variation in concentration and b first-order kinetics plots of MB and RhB with irradiation time against KSbPON

Table 4 Kinetic parameters, rate constant (k) and half-life time (t 1/2) of KSbPON in the first-order photocatalytic reaction

Photocatalyst (dye)	First-order rate constant,k ( min^-1)	Square of correlation coefficient R ²	t _1/2(min^-1)
KSbPON (MB)	0.0102 ± 0.0009	0.962	68
KSbPON (RhB)	0.0051 ± 0.0005	0.952	136

Fig. 9 Fluorescence spectra of visible light-irradiated KSbPON suspensions in 3 mmol L-1 terephthalic acid (λexcitation = 320 nm)

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Degradation of Methylene Blue and Rhodamine B Using a New Visible Light-Responsive Photocatalyst, KSb₂PO_8-_x N _y

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