Synthesis and Characterization of Composite H6P2Mo18O62/Zn(BDC)(Bipy)0.5 and Its Adsorption Activity for Methylene Blue†

doi:10.7503/cjcu20160253

Abstract

Abstract:

By employing the H₆P₂Mo₁₈O₆₂, terephthalic acid(H₂BDC), 4,4'-bipyridine(Bipy) to assemble with Zn²⁺ ion, a three-dimensional(3D) metal organic framework composite, named H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5, was synthesized. The composition, structure, morphology, stability and toleration of H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5 were characterized by X-ray powder diffraction pattern(XRD), Fourier transform infrared(FTIR) spectrum, scanning electron microscopy(SEM), thermogravimetric(TG) analysis and N₂ adsorption-desorption analysis. The adsorption of methylene blue(MB) onto H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5 in aqueous solution was studied. The effects of the experimental parameters including the temperature, the initial pH value and initial concentration of methylene blue solution were discussed. The experimental data could be well described by the Langmuir equations and pseudo-second-order kinetic model. The adsorption process of methylene blue on the composite was spontaneous and exothermic. Furthermore, we also explored the adsorption properties of H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5 to methyl violet, malachite green, rhodamine B, and methyl orange. The results indicated that this new absorbent showed better adsorption performance towards cationic dyes.

Key words: Three-dimensional(3D) metal organic framework, H6P2Mo18O62, Adsorption, Separation, Dye

CLC Number:

O614.6

TrendMD:

GONG Wenpeng, TIAN Chaoqiang, DU Xiaogang, YANG Shuijin. Synthesis and Characterization of Composite H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5 and Its Adsorption Activity for Methylene Blue^†[J]. Chem. J. Chinese Universities, 2016, 37(9): 1596.

Figures/Tables 17

Fig.1 FTIR spectra of H6P2Mo18O62(a), Zn(BDC)(Bipy)0.5(b) and H6P2Mo18O62/Zn(BDC)(Bipy)0.5(c)

Fig.2 XRD patterns of H6P2Mo18O62(a), Zn(BDC)(Bipy)0.5(b) and H6P2Mo18O62/Zn(BDC)(Bipy)0.5(c)

Table 1 Elemental analysis of Zn(BDC)(Bipy)0.5 and H6P2Mo18O62/Zn(BDC)(Bipy)0.5

Sample	Element	w(%)	n(Mo):n(P)
H₆P₂Mo₁₈O₆₂	P	2.13	9.1
	Mo	60.02
	Zn	0
H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5	P	1.74	9.0
	Mo	48.59
	Zn	20.61

Fig.3 TG curves of Zn(BDC)(Bipy)0.5(a) and H6P2Mo18O62/Zn(BDC)(Bipy)0.5(b)

Fig.4 Nitrogen adsorption isotherms of Zn(BDC)(Bipy)0.5 and H6P2Mo18O62/Zn(BDC)(Bipy)0.5

Table 2 Structural properties of Zn(BDC)(Bipy)0.5 and H6P2Mo18O62/Zn(BDC)(Bipy)0.5

Sample	S_BET/(m²·g^-1)	V_total/(cm³·g^-1)	D/nm
Zn(BDC)(Bipy)_0.5	710.6	0.32	1.79
H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5	249.9	0.12	1.92

Fig.5 SEM images of H6P2Mo18O62(A), Zn(BDC)(Bipy)0.5(B) and H6P2Mo18O62/Zn(BDC)(Bipy)0.5(C)

Fig.6 Effect of pH values on adsorption capacities for MB

Fig.7 Effect of initial mass concentration on adsorption capacities for MB Initial mass concentration of MB/(mg·mL-1): a. 40;b. 60; c. 80; d. 100; e. 120; f. 140.

Fig.8 Effect of temperature on adsorption capacity for MB

Fig.9 Comparison of adsorption activity of H6P2Mo18O62(a), Zn(BDC)(Bipy)0.5(b) and H6P2Mo18O62/Zn(BDC)(Bipy)0.5(c)

Fig.10 Adsorption amounts of different dyes on H6P2Mo18O62/Zn(BDC)(Bipy)0.5

Fig.11 Selective adsorption capability of H6P2Mo18O62/Zn(BDC)(Bipy)0.5 to the mixed dyes solution

Table 3 Parameters of pseudo-first-order and pseudo-second-order adsorption kinetics model in different initial concentrations

Kinetics model	Initial concentration of MB/ (mg·L^-1)	Q_e,exp/ (mg·g^-1)	Q_e,cal/ (mg·g^-1)	K₁/min^-1 or K₂/ (g·mg^-1·min^-1)	R²
Pseudo-first-order model	90	179.43	1.1693	0.09343	0.9661
	100	198.64	1.7124	0.10918	0.9669
Pseudo-second-order model	90	179.43	179.53	0.000021	1
	100	198.64	198.81	0.0000157	1

Fig.12 Langmuir isotherm of methylene blue adsorption onto H6P2Mo18O62/Zn(BDC)(Bipy)0.5

Table 4 Isotherm parameters of the adsorption of methylene blue by H6P2Mo18O62/Zn(BDC)(Bipy)0.5 at different temperature

Temperature/K	Langmuir				Freundlich
Temperature/K	Q_m/(mg·g^-1)	K_L/(L·mg^-1)	R_L	R²	K_F/(mg·g^-1)	n	R²
293	277.78	0.00319	0.7337	0.9986	244.84	13.18	0.9606
303	275.48	1.9621	0.00459	0.9893	194.54	7.76	0.9137
313	273.22	0.7205	0.01242	0.9695	157.66	5.76	0.7916

Table 5 Thermodynamic parameters of adsorption methylene blue onto H6P2Mo18O62/Zn(BDC)(Bipy)0.5

ΔG^o/(kJ·mol^-1)			ΔH^o/(kJ·mol^-1)	ΔS^o/(J·mol^-1·K^-1)
293 K	303 K	313 K	ΔH^o/(kJ·mol^-1)	ΔS^o/(J·mol^-1·K^-1)
-14.87	-11.33	-9.5	-93.81	-270.31

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Synthesis and Characterization of Composite H₆P₂Mo₁₈O₆₂/Zn(BDC)(Bipy)_0.5 and Its Adsorption Activity for Methylene Blue^†

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