The present work represents hydrogel as a composite based on sodium alginate and mesoporous SBA-15. The hydrogel was obtained by modifying mesoporous SBA-15 by a microencapsulation method of the SBA-15 in the sodium alginate matrix. The solution of CaCl2 provided a gelation complex of sodium alginate/SBA-15 in a rigid gel-like structure. The sodium alginate/SBA-15 hydrogels beads of about 3 mm diameter were prepared. Composite material was characterized by using powder X- ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. This composite material may have potential application in removal of metal ions – pollutants from aqueous solutions.XVI International Conference on Fundamental and Applied Aspects of Physical Chemistry : Proceedings, Vol. 2, September 26-30, Belgrad

Baščarević, Z.

Grce, Ana

Ilić, Svetlana

Katnić, Đurica

Kokunešoski, Maja

Pošarac-Marković, Milica B.

Šaponjić, Aleksandra

The present work represents hydrogel as a composite based on sodium alginate and mesoporous SBA-15. The hydrogel was obtained by modifying mesoporous SBA-15 by a microencapsulation method of the SBA-15 in the sodium alginate matrix. The solution of CaCl2 provided a gelation complex of sodium alginate/SBA-15 in a rigid gel-like structure. The sodium alginate/SBA-15 hydrogels beads of about 3 mm diameter were prepared. Composite material was characterized by using powder X- ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. This composite material may have potential application in removal of metal ions – pollutants from aqueous solutions.XVI International Conference on Fundamental and Applied Aspects of Physical Chemistry : September 26-30, Belgrade

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      PHYSICAL CHEMISTRY 2022  16th International Conference on Fundamental and Applied Aspects of Physical Chemistry    Proceedings Volume II                    September 26-30, 2022 Belgrade, Serbia II Title: PHYSICAL CHEMISTRY 2022, 16th International Conference on Fundamental and Applied Aspects of Physical Chemistry (Proceedings) ISBN 978-86-82475-41-5 Volume II: ISBN 978-53-82475-43-9 Editors: Željko Čupić and Slobodan Anić Published by: Society of Physical Chemists of Serbia, Studentski Trg 12-16, 11158, Belgrade, Serbia Publisher: Society of Physical Chemists of Serbia For Publisher: S. Anić, President of Society of Physical Chemists of Serbia Printed by: ʺJovanʺ, <Printing and Publishing Company, Ilije Đuričića 19, Belgrade,  200 Copies Number of pages: 6+320, Format A4, printing finished in December 2022 Text and Layout: ʺJovanʺ Neither this book nor any part may be reproduced or transmitted in any form or by any means, including photocopying, or by any information storage and retrieval system, without permission in writing from the publisher.       200 - Copy printing III CONTENT Volume II  Organizer IV Comittes V Sponsors VI Material Science 321 Photochemistry, Radiation Chemistry, Photonics 391 Macromolecular Physical Chemistry  395 Environmental Protection, Forensic Sciences, Geophysical Chemistry, Radiochemistry, Nuclear Chemistry 437 Phase Boundaries, Colloids, Liquid Crystals, Surface-Active Substances 513 Complex Compounds 517 Food Physical Chemistry 535 Pharmaceutical Physical Chemistry 565 Index 633  IV  PHYSICAL CHEMISTRY 2022  16th International Conference on  Fundamental and Applied Aspects of Physical Chemistry     Organized by  The Society of Physical Chemists of Serbia  in co-operation with  Institute of Catalysis Bulgarian Academy of Sciences  and  Boreskov Institute of Catalysis Siberian Branch of   Russian Academy of Sciences  and  University of Belgrade, Serbia: Faculty of Physical Chemistry Institute of Chemistry, Technology and Metallurgy Vinča Institute of Nuclear Sciences Faculty of Pharmacy  and  Institute of General and Physical Chemistry, Belgrade, Serbia V International Organizing Committee  Chairman:  S. Anić (Serbia) Vice-chairman:   M. Gabrovska (Bulgaria)                             A. A. Vedyagin (Russia)        S. N. Blagojević (Serbia) Members:  N. Cvjetićanin (Serbia), S. M. Blagojević (Serbia), M. Daković (Serbia), J. Dimitrić-Marković (Serbia), T. Grozdić (Serbia), Lj. Ignjatović (Serbia), A. Ivanović-Šašić(Serbia), D. Jovanović (Serbia), N. Jović-Jovičić (Serbia), M. Kuzmanović (Serbia),S. Maćešić (Serbia), D. Marković (Serbia), B. Milosavljević (USA), M. Mojović(Serbia), N. Pejić (Serbia), M. Petković (Serbia), A. Popović Bijelić (Serbia), B.Simonović (Serbia), B. Šljukić (Serbia), G. Tasić (Serbia), S. Veličković (Serbia),N. Vukelić (Serbia), International Scientific Committee   Chairman:     Ž. Čupić (Serbia) Vice-chairman:   V. Bukhtiyarov (Russia) S. Todorova (Bulgaria) B. Adnađević (Serbia) Members:  S. Anić (Serbia), A. Antić-Jovanović (Serbia), A. Azizoğlu (Turky), R. Cervellati(Italy), A. Clayton (Australia), A. Cristina Silva (Portugal) G. Ćirić-Marjanović(Serbia), V. Dondur (Serbia), R. Faria (Brasil), M. Fronczak (Poland), I. Grinvald (Russia), P. Humpolíček (Czech), M. Jeremić (Serbia), I. Kiss (USA), E. Kiš(Serbia), A.V. Knyazev (Russia), Lj. Kolar-Anić (Serbia), T. Kowalska (Poland), G. Kyzas (Greece), G. Lente (Hungary), Z. Marković (Serbia), S. Mentus (Serbia), K. Novaković (UK), N. Ostrovski (Serbia), V. Parmon (Russia), J. Pérez-Mercader (USA) Z. Petkova Cherkezova-Zheleva (Bulgary), M. Plavšić (Serbia), J. Savović(Serbia), G. Schmitz (Belgium), I. Schreiber (Czech), L. Schreiberova (Czech), D. Stanisavljev (Serbia), N. Stepanov (Russia), Zs. Szakacs (Romania), Z. Šaponjić(Serbia), Á. Tóth (Hungary), M. Trtica (Serbia), H. Varela (Brasil), V. Vasić(Serbia), Nadezda Vasilyeva (Russia), D. Veselinović (Serbia), V. Vukojević(Sweden), A. De Wit (Belgium) Local Executive Committee  Chairman:       S. N. Blagojević Vice-chairman:    A. Ivanović-Šašić Members:  M. Ajduković, I. N. Bubanja, D. Dimić, J. Dostanić, D. Drakulić, S. Jovanović, Z.Jovanović, D. Lončarević, J. Krstić, B. Marković, J. Maksimović, S. Marinović, D. Milenković, T. Mudrinić, M. Pagnacco, N. Potkonjak, B. Stanković, I. Stefanović,A. Todorović, M. Vasić, F. Veljković, M. Pejčić, G. Stevanović, H.Šalipur.K.Milošević, S. Pavlović, V. Kostić, B. Milovanović.  PHYSICAL CHEMISTRY 2022                            H-11-P 363MODIFYING MESOPOROUS SBA-15 BY A MICROENCAPSULATION METHOD IN THE MATRIX OF SODIUM ALGINATE  M. Kokunešoski1, M. Pošarc-Marković1, Dj. Katnić1, Z. Baščarević2,  S. Ilić1, A. Grce1 and A. Šaponjić1  1University of Belgrade Institute of Nuclear Sciences “Vinča”, National Institute of the Republic ofSerbia, Mike Petrovića Alasa 12-14, Vinča, 11000 Belgrade, Serbia. (majako@vin.bg.ac.rs) 2Institute for Multidisciplinary Research, University of Belgrade,  Kneza Višeslava 1, 11030 Beograd, Serbia. ABSTRACT The present work represents hydrogel as a composite based on sodium alginate and mesoporous SBA-15. The hydrogel was obtained by modifying mesoporous SBA-15 by a microencapsulation method of the SBA-15 in the sodium alginate matrix. The solution of CaCl2 provided a gelation complex of sodium alginate/SBA-15 in a rigid gel-like structure. The sodium alginate/SBA-15 hydrogels beads of about 3 mm diameter were prepared. Composite material was characterized by using powder X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. This composite material may have potential application in removal of metal ions – pollutants from aqueous solutions. INTRODUCTION Mesoporous silica materials such as SBA-15 received considerable attention because of their unique large surface area, well-defined pore size and pore shape [1, 2].  Studies have shown that remarkable surface porosity and functionality strongly affect the properties and efficiency of this material and its applications as drug and gene carrier [3, 4-7], material for enzyme loading [8] as well as material for detection and adsorption of metal ions in living systems [3, 9]. Various procedures have been employed on SBA-15 to improve its adsorption capacity [10]. However, the application of SBA-15 has some limitations due to the difficulty of incorporating functional groups on its surface. These limitations can be overcome by encapsulation of mesoporous silica with alginate.  Development of the hydrogel was driven by the idea to modify the mesoporous SBA-15 by a microencapsulation method with alginate used to protect them from degrading by surrounding them with a semi-permeable biopolymeric matrix. Microencapsulation avoids or retarding their contact with, for example, harmful environmental factors.  Alginate is extracted from various species of algae. Alginate is composed of the linear macromolecule in homopolymeric blocks of each monomer. The macromolecules are composed of (1-4)-linked b-D-man urinate (M) and a- L-guluronate units (G). Properties like low cost, easy use, biodegradability, and biocompatibility make alginate suitable for encapsulation. In the presence of divalent cations, usually, Ca2+ alginate is gelling in the form of a rigid gel-like structure, by ion exchange of sodium ions from guluronic acid residues [11-13].  METHODS Sodium alginate (SA, abcr GmbH), calcium chloride anhydrous powder (CaCl2, 99.99 %, Sigma Aldrich), Pluronic P123 non-ionic triblock copolymer (BASF), tetraethoxysilane (TEOS, 98%, Alfa Aesar) hydrochloric acid and (HCl, 35-38%, MACRON) were used. The SBA-15 was synthesized according to standard procedures [14] using Pluronic P123 as a surfactant and TEOS as a source of silica. A 4.0 g of Pluronic P123 dissolved in 30 ml of distilled water and 120 g of 2M HCl and stirred at 35 °C for 1.5 h. The 8.5 g of TEOS was added dropwise PHYSICAL CHEMISTRY 2022                            H-11-P 364into the solution and vigorously stirred at the same temperature for 1.5 h. This was followed by prolonged stirring and subsequent ageing. According to the method proposed by Zhao et al. [14], the mixture was aged in two steps. Firstly, it has aged at 35 oC for 20 h and then at 80 °C for 48 h. The final product is filtered, washed with distilled water until pH was neutral, and dried at room temperature. Calcination has been carried out in flowing air by slowly increasing the temperature from room temperature to 500 °C for 8 h and holding it at 500 °C for 6 h to decompose the remaining triblock copolymer. Fabrication of sodium alginate/SBA-15 hydrogels in the form of beads (SA/SBA-15) was done. The suspension of 1.5 g of SBA-15 powder and 15 ml distilled water was sonicated for 30 min. One and a half grams of alginic acid sodium salt (SA) was added to 110 mL of water at 35 °C while stirring. The suspension of SBA-15 was added into alginate and then homogenized on a magnetic stirrer (600 rpm) for 2 h at 35 oC.  The obtained new suspension was added in drops into CaCl2 solution through a Pasteur pipette as the next step of synthesizing beads. Gel-type spherical beads were formed during this process. After 3 h of gelation, beads were filtrated and washed with distilled water until pH was neutral. The size of wet beads after filtration was about 3 mm (Figure 1a). After drying at 60 oC, the size of hydrogel beads was about 2 mm. Aqueous CaCl2 solution was prepared by dissolving 0.623 g of CaCl2 in 50 ml distilled water under stirring to neutralize the carboxyl-site covalent bond of alginate  with the intention to induce inter-molecular ionic bonds between polymeric chains of alginate [11-13].    a) 10 20 30 40 50 60SBA-15SA/SBA-15SAIntensity (a.u.)2 (  ) b)  c)       d) Figure 1. a)  Beads of sodium alginate/SBA-15 hydrogel (SA/SBA-15), b) XRD patterns of: SBA-15, SA/SBA-15 and SA and SEM images of c) SBA-15 and d) SA/SBA-15. PHYSICAL CHEMISTRY 2022                            H-11-P 365X-ray diffraction (XRD) analysis of SBA-15, SA/SBA-15 and SA was performed at room temperature using Ultima IV Rigaku diffractometer, equipped with Cu Kα1,2 radiations, with generator voltage 40.0 kV and generator current 40.0 mA. The range of 10°-60° 2Ѳ was used in a continuousscan mode with a scanning step size of 0.02° at a scan rate of 10 °/min. Microstructure analysis is performed by scanning electron microscope (SЕМ, VEGA TS 5130 MM, Tescan). Energy-dispersive X-ray analysis (EDS) was carried out with INCA PentaFET-x3, Oxford Instruments. RESULTS AND DISCUSSION The XRD patterns of SBA-15, SA/SBA-15 and SA are shown in Figure 1b. Samples SBA-15 and SA/SBA-15 exhibit a single very broad peak at about 2  = 23°, which is the characteristic of amorphous silica. In contrast, XRD of the SA pattern exhibits very broad peaks at about 2  = 14° and 22°.   A glimpse at the SEM micrographs of SBA-15 and SA/SBA-15 and (Figure 1c and Figure 1d) discloses the presence of many rod-like agglomerates were approximately 20 μm in length in all studied samples. As the SEM images showed, the average size of grains in all samples was about 1 μm, in which particles have placed themselves along the agglomerated ones like chains. Same chain agglomerate structures (Figure 1c) were reported in an earlier paper [15, 16].  The EDS analysis showed the chemical composition of SBA-15, SA/SBA-15 and SA. The EDS analysis demonstrated that the particles in the SBA-15 sample consist of SiO2. High levels of carbon (~ 36 at. %) and oxygen (~58 at. %) originate from gases from the air adsorbed by the surface of the SBA-15 [17].  The EDS analysis of SA and SA/SBA-15showed the presence of C, O, Na, K and Cu in SA (Table 1.) and confirmed the presence of C, O, Si, Cl, and Ca in the sample SA/SBA-15. Elements Ca, and Cl originates from CaCl2 solution, used as an agent for sphere formation. However, high levels of carbon (~22 at. %) and oxygen (~59 at. %) originated from SA and air adsorbed by the surface of the samples.  Table 1. Average values of the chemical composition of SA and SA/SBA-15, obtained by EDS analysis (atomic %). Sample C O Si Na Cl K Cu Ca Ag Au SA 56.38 32.56 - 10.21 0.13 0.11 0.11 - 0.08 0.35 SA/SBA-15 21.50 58.71 17.28 - 0.07 - - 1.65 0.10 0.67 CONCLUSION Composite hydrogel based on sodium alginate and mesoporous SBA-15 was synthesized by a microencapsulation method of the SBA-15 in the sodium alginate matrix. A gelation complex of sodium alginate/SBA-15 is a form rigid gel-like structure was provided by the solution of CaCl2. The sodium alginate/SBA-15 hydrogels were obtained in the form of beads of about 3 mm in diameter. The X-ray diffraction patterns of SBA-15, SA/SBA-15 and SA exhibit a single very broad peak, which is the characteristic of amorphous silica. A scanning electron microscope discloses that many rod-like agglomerates of all investigated samples were approximately 20 μm in length. As the scanning electron microscope images show, the average size of grains of all investigated samples is about 1 μm.The Energy-dispersive X-ray analysis of the SBA-15 surface content has demonstrated that the particles in this sample are of SiO2. We intend to investigate the possibility of using the obtained hydrogels of sodium alginat/SBA-15 in the form of pearls to remove metal ions from an aqueous solution.  PHYSICAL CHEMISTRY 2022                            H-11-P 366Acknowledgment This work was supported by the Ministry of Education, Science and Technological Development ofthe Republic of Serbia (grant no 451-03-68/2022-14/200017). REFERENCES   [1] Kresge, C. T., Leonowicz, M. E., Roth, W. J., Vartuli, J. C., Beck, J. S., Nature 359 (1992)      710. [2] Beck, J. S., Vartuli, J. C., Roth, W. J., Leonowicz, M. E., Kresge, C. T., Schmitt, K. D., Chu, C. T. W., Olson, D. H., Sheppard, E. W., McCullen, S. B., Higgins, J. B. and Schlenker, J. L.  J. Am. Chem. Soc., 114 (1992) 1083. 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[11]  Lozano-Vazquez, G., Lobato-Calleros, C., Escalona-Buendia, H., Chavez, G., Alvarez-        Ramirez, J., Vernon-Carter, E.J., Food Hydrocolloids, 48 (2015) 301. [12] Ramdhan, T., Su Hung, C., Prakash, S., Bhandari, B., Food Hydrocolloids, 90 (2019) 232–240.  [13] Kosari, M.,  Sepehrian, H.,  Fasihi, J.,  Arabieh, M., Study, K., J. Appl. Chem. Res. 11 (2017)  135. [14] Zhao, D., Feng, J., Huo, Q., Melosh, N., Fredrickson, G. H., Chmelka, B. F., Stucky, G. D. Science, 279 (1998) 548. [15] Kokunešoski, M., Gulicovski, J., Matović, B., Babić, B., J. Optoelectron. Adv. M., 11 (2009)  1656. [16] Wang, Z., Huang, Y., Wang, M., Wu, G., Geng, T., Zhao, Y., Wu, A., Macroporous calcium   alginate aerogel as sorbent for Pb2+ removal from water media, J. Environ. Chem. Eng., 4 (3)   (2016) 3185. [17] Kokunešoski, M., Gulicovski, J., Matović, B., Logar, M., Milonjić, S. K., Babić, B., Mater.     Chem. Phys. 124 (2010) 1248.      CIP - Каталогизација у публикацији - Народна библиотека Србије, Београд 544(082) 66.017/.018(082) 502/504(082) INTERNATIONAL Conference on Fundamental and Applied Aspects of Physical Chemistry (16 ; 2022 ; Beograd)   Physical Chemistry 2022 : proceedings. Vol. 2 / 16th International Conference on Fundamental and Applied Aspects of Physical Chemistry, September 26-30, 2022, Belgrade, Serbia ; [editors Željko Čupić and Slobodan Anić]. - Belgrade : Society of Physical Chemists of Serbia, 2022 (Belgrade : Jovan). - VI str., str. 323-640 : ilustr. ; 30 cm Tiraž 200. - Bibliografija uz svaki rad. - Registar. ISBN 978-86-82475-43-9 ISBN 978-86-82475-41-5 (niz) a) Физичка хемија - Зборници b) Наука о материјалима - Зборници c) Животна средина - Зборници COBISS.SR-ID 82228745  639

Modifying Mesoporous SBA-15 by a Microencapsulation Method in the Matrix of Sodium Alginate

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Modifying Mesoporous SBA-15 by a Microencapsulation Method in the Matrix of Sodium Alginate

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