Evaluation of magnetic poly(methyl methacrylate) microspheres as catalysts in heterogeneous Fenton processes

This work reports the preparation of magnetic polymeric microspheres based on poly(methyl methacrylate) and the investigation of these materials as catalysts in heterogeneous Fenton processes for the decolorization of methyl orange (MO). The microspheres were prepared by polymerization of the magnetic material together with the monomers by aqueous suspension polymerization. The microspheres had specific surface area of 48.2 m² g^-1. Mossbauer data indicated that the magnetic material was a mixture of magnetite (31%), maghemite (21%), and goethite (48%). Fenton reactions were performed by varying the concentration of H₂O₂, pH, composite mass, and contact time. The highest color removal rates (around 80%) were reached at pH 3.0, 20% w/v of composite, 20 minutes contact time, and 10 ppm of H₂O₂. The composite could be reused during four cycles with removal efficiency above 50%. The results indicated that the adsorption and oxidation mechanisms act together determining the variation of the MO dye removal.

Keywords:
heterogeneous Fenton reactions; magnetic materials; methyl orange; poly(methyl methacrylate) microspheres

Authorship

Alan Kardec da Silva

Departamento de Farmácia, Faculdade de Ciências Biológicas e da Saúde, Campus Zona Oeste, Universidade do Estado do Rio de Janeiro – UERJ, Rio de Janeiro, RJ, BrasilUniversidade do Estado do Rio de JaneiroBrasilRio de Janeiro, RJ, BrasilDepartamento de Farmácia, Faculdade de Ciências Biológicas e da Saúde, Campus Zona Oeste, Universidade do Estado do Rio de Janeiro – UERJ, Rio de Janeiro, RJ, Brasil

http://orcid.org/0000-0003-2498-7957

Ezaine Cristina Corrêa Torquato

http://orcid.org/0000-0002-9828-9353

Jacira Aparecida Castanharo

Departamento de Processos Químicos, Instituto de Química, Universidade do Estado do Rio de Janeiro – UERJ, Rio de Janeiro, RJ, BrasilUniversidade do Estado do Rio de JaneiroBrasilRio de Janeiro, RJ, BrasilDepartamento de Processos Químicos, Instituto de Química, Universidade do Estado do Rio de Janeiro – UERJ, Rio de Janeiro, RJ, Brasil

http://orcid.org/0000-0001-6553-1417

Marcos Antonio da Silva Costa

http://orcid.org/0000-0002-1435-8818

Mônica Regina da Costa Marques

Departamento de Química Orgânica, Instituto de Química, Universidade do Estado do Rio de Janeiro – UERJ, Rio de Janeiro, RJ, BrasilUniversidade do Estado do Rio de JaneiroBrasilRio de Janeiro, RJ, BrasilDepartamento de Química Orgânica, Instituto de Química, Universidade do Estado do Rio de Janeiro – UERJ, Rio de Janeiro, RJ, Brasil

http://orcid.org/0000-0001-6906-8327

Luciana da Cunha Costa ^* * luciana.cunha.costa@gmail.com

http://orcid.org/0000-0002-2374-5043

* luciana.cunha.costa@gmail.com

• Conceptualization – Luciana da Cunha Costa; Mônica Regina da Costa Marques.

• Data curation – NA.

• Formal analysis – NA.

• Funding acquisition – Luciana da Cunha Costa; Mônica Regina da Costa Marques.

• Investigation – Alan Kardec Silva; Jacira Aparecida Castanharo.

• Methodology – Alan Kardec Silva; Jacira Aparecida Castanharo.

• Project administration – NA.

• Resources – NA.

• Software – NA.

• Supervision – Luciana da Cunha Costa; Mônica Regina da Costa Marques.

• Validation – NA.

• Visualization – NA.

• Writing – original draft – Alan Kardec Silva; Ezaine Cristina Corrêa Torquato.

• Writing – review & editing – Luciana da Cunha Costa; Jacira Aparecida Castanharo; Marcos Antonio da Silva Costa; Mônica Regina da Costa Marques.

SCIMAGO INSTITUTIONS RANKINGS

Figures | Tables | Formulas

Figures (6)
Tables (1)
Formulas (1)

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Figure 1
(a) EDS spectrum and iron distribution map of the magnetic material, SEM image of magnetic microsphere; (b) FT-IR spectrum of the magnetic microspheres; (c) XRD spectra of the magnetic material and magnetic microspheres; (d) Transmission Mossbauer spectra of the magnetic microspheres.

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Figure 2
Principal reactions involving ferrous ions in magnetite, maghemite and goethite domains. Based on the works of Panda et al.^[¹⁴14 Panda, N., Sahoo, H., & Mohapatra, S. (2011). Decolorization of methyl orange using Fenton-like mesoporous Fe2O3–SiO2 composite. Journal of Hazardous Materials, 185(1), 359-365. http://dx.doi.org/10.1016/j.jhazmat.2010.09.042. PMid:20934248.
http://dx.doi.org/10.1016/j.jhazmat.2010... ^] and Wan et al.^[²¹21 Wan, D., Li, W., Wang, G., Lu, L., & Wei, X. (2017). Degradation of p-Nitrophenol using magnetic Fe0/Fe3O4/Coke composite as a heterogeneous Fenton-like catalyst. The Science of the Total Environment, 574, 1326-1334. http://dx.doi.org/10.1016/j.scitotenv.2016.08.042. PMid:27519319.
http://dx.doi.org/10.1016/j.scitotenv.20... ^].

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Figure 3
(a) Effect of H₂O₂ content on degradation of MO (a: H₂O₂ content: 1-50 ppm, pH: 3, MO: 5 ppm, composite: 1%, time: 10 minutes), (b: H₂O₂ content: 10 or 20 ppm, pH: 3, MO: 5 ppm, composite: 5%, time: 1-30 minutes).

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Figure 4
(a) Effect of pH on MO degradation. Experimental conditions: pH 3-7.3, 5 ppm of MO, 5 ppm of H₂O₂, 5% of composite, and 10 minutes of reaction; (b) Effect of catalyst on the degradation of MO in the function of time. Experimental conditions: pH 3, 5 ppm of MO, 20 ppm of H₂O₂, 5% of composite, contact time range from 0-30 minutes.

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Figure 5
Color removal of MO due to adsorption and oxidation by Fenton processes. Experimental conditions: pH 3, 5 ppm of MO, 20 ppm of H₂O₂, 5%-20% wt.% of composite, contact time range from 0-20 minutes.

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Figure 6
Study of reuse of composite particles for MO removal. Experimental conditions: pH 3, 5 ppm of MO, 10 ppm of H₂O₂, 5% of composite, contact time of 5 minutes.

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Figure 6
Study of reuse of composite particles for MO removal. Experimental conditions: pH 3, 5 ppm of MO, 10 ppm of H₂O₂, 5% of composite, contact time of 5 minutes.

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Table 1
Morphological characteristics of the magnetic PMMA microspheres^[⁶6 Castanharo, J. A., Ferreira, I. L. M., Costa, M. A. S., Silva, M. R., Costa, G. M., & Oliveira, M. G. (2015). Magnetic microspheres based on poly(divinylbenzene-co-methyl methacrylate) obtained by suspension polymerization. Polímeros: Ciência e Tecnologia, 25(2), 192-199. http://dx.doi.org/10.1590/0104-1428.1666.
http://dx.doi.org/10.1590/0104-1428.1666... ^].

Thumbnail

(1)

Figure 1 (a) EDS spectrum and iron distribution map of the magnetic material, SEM image of magnetic microsphere; (b) FT-IR spectrum of the magnetic microspheres; (c) XRD spectra of the magnetic material and magnetic microspheres; (d) Transmission Mossbauer spectra of the magnetic microspheres.

Figure 2 Principal reactions involving ferrous ions in magnetite, maghemite and goethite domains. Based on the works of Panda et al.^[¹⁴14 Panda, N., Sahoo, H., & Mohapatra, S. (2011). Decolorization of methyl orange using Fenton-like mesoporous Fe2O3–SiO2 composite. Journal of Hazardous Materials, 185(1), 359-365. http://dx.doi.org/10.1016/j.jhazmat.2010.09.042. PMid:20934248.
http://dx.doi.org/10.1016/j.jhazmat.2010... ^] and Wan et al.^[²¹21 Wan, D., Li, W., Wang, G., Lu, L., & Wei, X. (2017). Degradation of p-Nitrophenol using magnetic Fe0/Fe3O4/Coke composite as a heterogeneous Fenton-like catalyst. The Science of the Total Environment, 574, 1326-1334. http://dx.doi.org/10.1016/j.scitotenv.2016.08.042. PMid:27519319.
http://dx.doi.org/10.1016/j.scitotenv.20... ^].

Figure 3 (a) Effect of H₂O₂ content on degradation of MO (a: H₂O₂ content: 1-50 ppm, pH: 3, MO: 5 ppm, composite: 1%, time: 10 minutes), (b: H₂O₂ content: 10 or 20 ppm, pH: 3, MO: 5 ppm, composite: 5%, time: 1-30 minutes).

Figure 4 (a) Effect of pH on MO degradation. Experimental conditions: pH 3-7.3, 5 ppm of MO, 5 ppm of H₂O₂, 5% of composite, and 10 minutes of reaction; (b) Effect of catalyst on the degradation of MO in the function of time. Experimental conditions: pH 3, 5 ppm of MO, 20 ppm of H₂O₂, 5% of composite, contact time range from 0-30 minutes.

Figure 5 Color removal of MO due to adsorption and oxidation by Fenton processes. Experimental conditions: pH 3, 5 ppm of MO, 20 ppm of H₂O₂, 5%-20% wt.% of composite, contact time range from 0-20 minutes.

Figure 6 Study of reuse of composite particles for MO removal. Experimental conditions: pH 3, 5 ppm of MO, 10 ppm of H₂O₂, 5% of composite, contact time of 5 minutes.

Figure 3 (a) Effect of H₂O₂ content on degradation of MO (a: H₂O₂ content: 1-50 ppm, pH: 3, MO: 5 ppm, composite: 1%, time: 10 minutes), (b: H₂O₂ content: 10 or 20 ppm, pH: 3, MO: 5 ppm, composite: 5%, time: 1-30 minutes).

Figure 4 (a) Effect of pH on MO degradation. Experimental conditions: pH 3-7.3, 5 ppm of MO, 5 ppm of H₂O₂, 5% of composite, and 10 minutes of reaction; (b) Effect of catalyst on the degradation of MO in the function of time. Experimental conditions: pH 3, 5 ppm of MO, 20 ppm of H₂O₂, 5% of composite, contact time range from 0-30 minutes.

Figure 5 Color removal of MO due to adsorption and oxidation by Fenton processes. Experimental conditions: pH 3, 5 ppm of MO, 20 ppm of H₂O₂, 5%-20% wt.% of composite, contact time range from 0-20 minutes.

Figure 6 Study of reuse of composite particles for MO removal. Experimental conditions: pH 3, 5 ppm of MO, 10 ppm of H₂O₂, 5% of composite, contact time of 5 minutes.

Table 1 Morphological characteristics of the magnetic PMMA microspheres^[⁶6 Castanharo, J. A., Ferreira, I. L. M., Costa, M. A. S., Silva, M. R., Costa, G. M., & Oliveira, M. G. (2015). Magnetic microspheres based on poly(divinylbenzene-co-methyl methacrylate) obtained by suspension polymerization. Polímeros: Ciência e Tecnologia, 25(2), 192-199. http://dx.doi.org/10.1590/0104-1428.1666.
http://dx.doi.org/10.1590/0104-1428.1666... ^].

S (m² g^-1)	Vp (cm³ g^-1)	P. S.(μm)	M_S (emu g^–1)	M_R (emu g^–1)	IC. (% m.m.)
48.30	0.35	20-104.00	4.76	0.21	4.13 ± 0.02

S: specific surface area (determined by nitrogen physisorption, by employing the BET equation); Vp: pore volume (determined by nitrogen physisorption, by employing the BJH equation); P.S.: Particle size range (determined by Malvern Mastersizer), M_S: saturation magnetization (determined by employing vibrating sample magnetometry), M_R.: remaining magnetization (determined by employing vibrating sample magnetometry), I.C.: iron content incorporated in the polymeric particles (determined by AAS after acid digestion of the particles)

(1)

R (%) = \frac{(C_{0 -} C_{t})}{C o} \times 100

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Evaluation of magnetic poly(methyl methacrylate) microspheres as catalysts in heterogeneous Fenton processes

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[1] * luciana.cunha.costa@gmail.com