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Zeolitic Materials: Structure, Properties, and Applications

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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Porous Materials".

Deadline for manuscript submissions: closed (20 December 2022) | Viewed by 26567

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Prof. Dr. Bruno De Gennaro

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ACLabs-Laboratories of Applied Chemistry, Department of Chemical, Materials and Industrial Production Engineering, University of Naples Federico II, P.le V. Tecchio 80, 80125 Naples, Italy
Interests: natural and synthetic zeolites; adsorption and ion exchange properties; wastewater treatments; zeolite surface modification; drug delivery; emerging contaminant treatment
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Prof. Dr. Barbara Liguori

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ACLabs—Applied Chemistry Labs, Department of Chemical, Materials and Industrial Production Engineering, University of Naples Federico II, P.le V. Tecchio 80, 80125 Naples, Italy
Interests: materials engineering; porous materials; zeolites; construction materials; hybrid foams; geopolymers; sustainable building materials; material recycling
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Dr. Abner Colella

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Department of Earth Sciences, Environment and Resources, Federico II University, Monte Sant\'Angelo Campus (L Building), Via Cinthia, 21-80126 Naples, Italy
Interests: natural zeolites and their applications, such as wastewater treatment and soil remediation; geomaterials; construction and building stone materials; minerogenetic processes in pyroclastic deposits of central-southern Italy
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Prof. Dr. Domenico Caputo

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ACLabs—Applied Chemistry Labs, Department of Chemical, Materials and Industrial Production Engineering, University of Naples Federico II, P.le V. Tecchio 80, 80125 Naples, Italy
Interests: materials engineering; porous materials; zeolite and related materials for energy and environmental applications; adsorption and ion exchange; sustainable construction materials
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Special Issue Information

Dear Colleagues,

As is well known, zeolites have received a great deal of attention from the scientific community in recent decades thanks to their easy accessibility and their peculiar properties. Zeolites, aluminosilicates of alkaline, and alkaline earth metals are characterized by open structures with tetrahedral geometry that give rise to an ordered three-dimensional framework with a negative charge, typically balanced by cations placed together with water molecules in cavities and/or channels of microporosity dimensions. Due to these outstanding features, zeolites, both of sedimentary origin or synthetic, modified or as such, have a variety of physical and chemical properties, i.e., ion exchange, adsorption, alkali metals reactivity, expansion tendency and thermal insulation, compressive strength, and durability, which have allowed their application in various sectors, such as environmental protection, agricultural and industrial fields, pharmaceutics, and medicine. More in detail, zeolites can be used in wastewater and gas purification, soil remediation, building materials production, catalysis, energy storage, and drug delivery.

The several application opportunities of zeolites have led to an in-depth study of their mineralogical, crystal structure and chemical properties, as well as their kinetic and thermodinamic behavior in the processes in which are involved, to better predict their achievements when applied in areas of technological interest.

Based on the long-term interest that zeolites have received from the scientific community, this Special Issue of Materials aims to highlight the present state of research on the characterization of zeolite materials, as well as of their applications in both traditional and innovative fields.

We are then very pleased to invite you to submit a manuscript to this Special Issue on “Zeolitic Materials: Structure, Properties, and Applications”.

Full research articles, short communications, and comprehensive review papers covering all aspects of research on zeolitic materials are welcome.

Prof. Dr. Bruno De Gennaro
Prof. Dr. Barbara Liguori
Dr. Abner Colella
Prof. Dr. Domenico Caputo
Guest Editors

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Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Materials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

Zeolite structure
Ion exchange
Adsorption
Thermodynamic and kinetic studies
Thermodynamic and kinetic modeling
Environmental applications
Building materials
Energy storage
Sustained drug release
Catalysis

Related Special Issue

Zeolitic Materials: Structure, Properties, and Applications II in Materials (1 article)

Published Papers (11 papers)

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Research

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14 pages, 4003 KiB

Open AccessArticle

Cenosphere-Based Zeolite Precursors of Lutetium Encapsulated Aluminosilicate Microspheres for Application in Brachytherapy

by Tatiana Vereshchagina, Ekaterina Kutikhina, Sergei Vereshchagin, Olga Buyko and Alexander Anshits

Materials 2022, 15(19), 7025; https://doi.org/10.3390/ma15197025 - 10 Oct 2022

Cited by 1 | Viewed by 1573

Abstract

Coal fly ash hollow aluminosilicate microspheres (cenospheres) of stabilized composition (glass phase—95.4; (SiO₂/Al₂O₃)_glass—3.1; (Si/Al)_at. = 2.6) were used to fabricate lutetium-176 encapsulated aluminosilicate microspheres as precursors of radiolabeled microspheres applied for selective irradiation of tumors. To incorporate Lu³⁺ ions into cenosphere’s aluminosilicate material, the following strategy was realized: (i) chemical modification of cenosphere globules by conversion of aluminosilicate glass into zeolites preserving a spherical form of cenospheres; (ii) loading of zeolitized microspheres with Lu³⁺ by means of ion exchange 3Na⁺ ↔ Lu³⁺; (iii) Lu³⁺ encapsulation in an aluminosilicate matrix by solid-phase transformation of the Lu³⁺ loaded microspheres under thermal treatment at 1273–1473 K. Two types of zeolitized products, such as NaX (FAU) and NaP1 (GIS) bearing microspheres having the specific surface area of 204 and 33 m²/g, accordingly, were prepared and their Lu³⁺ sorption abilities were studied. As revealed, the Lu³⁺ sorption capacities of the zeolitized products are about 130 and 70 mg/g Lu³⁺ for NaX and NaP1 microspheres, respectively. It was found that the long-time heating of the Lu³⁺-loaded zeolite precursors at 1273 K in a fixed bed resulted in the crystallization of monoclinic Lu₂Si₂O₇ in both zeolite systems, which is a major component of crystalline constituents of the calcined microspheres. The fast heating–cooling cycle at 1473 K in a moving bed resulted in the amorphization of zeolite components in both precursors and softening glass crystalline matter of the NaX-bearing precursor with preserving its spherical form and partial elimination of surface open pores. The NaX-bearing microspheres, compared to NaP1-based precursor, are characterized by uneven Lu distribution over the zeolite-derived layer. The precursor based on gismondin-type zeolite provides a near-uniform Lu distribution and acceptable Lu content (up to 15 mol.% Lu₂O₃) in the solid phase. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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19 pages, 1568 KiB

Open AccessArticle

Use of Zeolites in the Capture and Storage of Thermal Energy by Water Desorption—Adsorption Cycles

by Bruno de Gennaro, Angelo Cappi, Maurizio de Gennaro, Nicola Bianco, Alessio Langella, Piergiulio Cappelletti, Antonello Marocco, Paolo Aprea and Michele Pansini

Materials 2022, 15(16), 5574; https://doi.org/10.3390/ma15165574 - 13 Aug 2022

Cited by 4 | Viewed by 1684

Abstract

In this work, four zeolite-bearing materials (three naturally occurring and one of synthetic origin) were considered for thermal energy capture and storage. Such materials can store thermal energy as heat of desorption of the water present therein, heat that is given back when water vapor is allowed to be re-adsorbed by zeolites. This study was carried out by determining the loss of water after different activation thermal treatments, the water adsorption kinetics and isotherm after an activation step of the zeolites, the intergranular and intragranular porosity, and the thermal conductivity of the zeolite-bearing materials. Moreover, the thermal stability of the framework of the zeolites of the four materials tested was investigated over a large number of thermal cycles. The results indicate that zeolite 13X was the most suitable material for thermal energy storage and suggest its use in the capture and storage of thermal energy that derives from thermal energy waste. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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12 pages, 3093 KiB

Open AccessArticle

Dealumination and Characterization of Natural Mordenite-Rich Tuffs

by Armando Adriano, Mauricio H. Cornejo, Haci Baykara, Eduardo V. Ludeña and Joaquín L. Brito

Materials 2022, 15(13), 4654; https://doi.org/10.3390/ma15134654 - 1 Jul 2022

Cited by 1 | Viewed by 1559

Abstract

The present study evaluates the feasibility of partially dealuminated natural mordenite as a catalyst support by studying improvement in its textural properties. This is the first study that reports the dealumination of natural zeolite-based tuffs from Ecuador. For this purpose, mordenite-rich tuffs were obtained from deposits close to Guayaquil, Ecuador. The raw material was micronized in order to increase its surface, and treated with NH₄Cl. NH₄⁺ cation-exchanged samples were finally reacted with HCl_(aq) to complete the dealumination process. The partially dealuminated samples were characterized using techniques such as XRD, FT-IR, SEM-EDS, and identification of their textural properties. Dealumination with HCl_(aq) increased the Si/Al ratio up to 9 and kept the crystallographic structure of natural mordenite, as XRD results showed that the structure of mordenite was not altered after the dealumination process. On the other hand, textural properties such as surface area and microporosity were improved as compared to natural mordenite. In view of these results, the feasibility of using natural mordenite as a catalyst support is discussed in this study. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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15 pages, 4636 KiB

Open AccessArticle

Surface Modification of Synthetic Zeolites with Ca and HDTMA Compounds with Determination of Their Phytoavailability and Comparison of CEC and AEC Parameters

by Michał Łach, Agnieszka Grela, Kinga Pławecka, Martin Duarte Guigou, Janusz Mikuła, Norbert Komar, Tomasz Bajda and Kinga Korniejenko

Materials 2022, 15(12), 4083; https://doi.org/10.3390/ma15124083 - 8 Jun 2022

Cited by 8 | Viewed by 1740

Abstract

Zeolites obtained from fly ash are characterized by very good anion- and cation-exchange properties and a developed porous structure. This paper presents the results of surface modification studies of synthetic zeolites obtained from calcined coal shale (clay materials). Calcium compounds and hexadecyltrimethylammonium bromide (HDTMA) were used as modifying substances. The characteristics of the raw material and the zeolite obtained as a result of its synthesis are presented. The surface modification method is described. Furthermore, the results of sorption and desorption of NO₃, PO₄, and SO₄ from raw and modified samples are presented. The results of anion- and cation-exchange capacities for other zeolite types were also compared. Modification of the materials with Ca ions and HDTMA surfactant only improved the sorption of sulfates. The 90% desorption of nitrates, phosphates, and sulphates from the zeolite material without modification indicates a good release capacity of these compounds and their potential use as fertilizer additives. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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14 pages, 2980 KiB

Open AccessArticle

Mineralogical and Technological Characterization of Zeolites from Basin and Range as Pozzolanic Addition of Cement

by Giovanna Montesano, Piergiulio Cappelletti, Domenico Caputo, Barbara Liguori, Assunta Campanile and Concetta Rispoli

Materials 2022, 15(7), 2684; https://doi.org/10.3390/ma15072684 - 6 Apr 2022

Cited by 3 | Viewed by 1887

Abstract

The present paper assesses petrographic, mineralogical, chemical, and technological features of different zeolitic tuff samples from various western USA districts of the Basin and Range Province containing mainly erionite, mordenite, clinoptilolite/heulandite and phillipsite. The aim of this characterization is to evaluate the pozzolanic activity of these samples according to European normative UNI-EN 196/5 (Fratini test) to program a possible use as addition for blended cements. Petrographic and mineralogical results show that the two phillipsite-bearing tuffs have a higher theoretical Cation Exchange Capacity (CEC) than the other samples; technological characterization shows a pozzolanic behavior for all the samples but higher for the tuff samples containing phillipsite, which shows a higher reactivity with CaO. All the samples could be thus advantageously employed for the preparation of blended cements, potentially reducing CO₂ emissions by 70–90%. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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18 pages, 6058 KiB

Open AccessArticle

Application of Surfactant Modified Natural Zeolites for the Removal of Salicylic Acid—A Contaminant of Emerging Concern

by Danijela Smiljanić, Aleksandra Daković, Milena Obradović, Milica Ožegović, Francesco Izzo, Chiara Germinario and Bruno de Gennaro

Materials 2021, 14(24), 7728; https://doi.org/10.3390/ma14247728 - 14 Dec 2021

Cited by 10 | Viewed by 2682

Abstract

This work aimed to test composites (surfactant modified zeolites prepared by treatment of natural zeolites—clinoptilolite (IZ CLI) and/or phillipsite (PHIL75)-rich tuffs with two different amounts of cationic surfactants: cetylpyridinium chloride (CPyCl) and Arquad^® 2HT-75 (ARQ)) for the adsorption of salicylic acid (SA)—a common contaminant of emerging concern. Adsorption of SA was studied at different initial drug concentrations (in the range of 2–100 mg/L) in water solution. The Langmuir isotherm model showed the highest adsorption was achieved by bilayer composite of IZ CLI and CPyCl—around 11 mg/g. Kinetic runs were performed by using the initial drug concentration of 20 mg/L in the time interval from 0 to 75 min and pseudo-second order had good correlation with experimental data. The influence of the four different temperatures on the SA adsorption was also investigated and thermodynamic parameters suggested that the adsorption drug onto composites is an exothermic and nonspontaneous process, followed by the decrease of randomness at the solid/liquid interface during the adsorption. Zeta potential and Fourier-transform infrared spectroscopy with attenuated total reflectance (FTIR-ATR) had been performed for the characterization of composites after adsorption of SA confirming the presence of the drug at composite surfaces. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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9 pages, 2215 KiB

Open AccessArticle

The Effect of Heat Treatment on the Structure of Zeolite A

by Magdalena Katarzyna Król and Piotr Jeleń

Materials 2021, 14(16), 4642; https://doi.org/10.3390/ma14164642 - 18 Aug 2021

Cited by 22 | Viewed by 2691

Abstract

Knowledge about the thermal properties of zeolites is extremely important due to their potential application in the chemical industry. In this work, the thermal stability and the dehydration process of zeolite A were investigated by in situ high temperature Fourier transform infrared spectroscopy. The progress of thermal decomposition that zeolite A underwent during the controlled temperature increase in the range of 25–600 °C was determined by the DRIFT spectroscopic method. Infrared spectra are presented and discussed for this compound on the basis of the crystal structure. Based on the courses of the obtained DRIFT spectra, it was found that, during heating, water was gradually removed from the structure of the material, followed by dehydration and formation of hydrogen bonds. It was established that the process of thermal degradation began as early as 550 °C. The analysis of the obtained results of structural tests can be repeated on other materials from the zeolite group and complements the research work on the thermal analysis of these materials. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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16 pages, 2837 KiB

Open AccessArticle

Effects of Electronegativity and Hydration Energy on the Selective Adsorption of Heavy Metal Ions by Synthetic NaX Zeolite

by Xianyuan Fan, Hong Liu, Emmanuella Anang and Dajun Ren

Materials 2021, 14(15), 4066; https://doi.org/10.3390/ma14154066 - 21 Jul 2021

Cited by 36 | Viewed by 2613

Abstract

The adsorption capacity of synthetic NaX zeolite for Pb²⁺, Cd²⁺, Cu²⁺ and Zn²⁺ in single and multi-component systems were investigated. The effects of electronegativity and hydration energy on the selective adsorption, as well as potential selective adsorption mechanism of the NaX zeolite for Pb²⁺, Cd²⁺, Cu²⁺ and Zn²⁺ were also discussed. The maximum adsorption capacity order of the heavy metals in the single system was Pb²⁺ > Cd²⁺ > Cu²⁺ > Zn²⁺, and this could be related to their hydration energy and electronegativity. The values of the separation factors (α) and affinity constant (K_EL) in different binary systems indicated that Pb²⁺ was preferentially adsorbed, and Zn²⁺ presented the lowest affinity for NaX zeolite. The selective adsorption capacities of the metals were in the order, Pb²⁺ > Cd²⁺ ≈ Cu²⁺ > Zn²⁺. The trend for the selective adsorption of NaX zeolite in ternary and quaternary systems was consistent with that in the binary systems. Pb²⁺ and Cu²⁺ reduced the stability of the Si-O-Al bonds and the double six-membered rings in the NaX framework, due to the high electronegativity of Pb²⁺ and Cu²⁺ than that of Al³⁺. The selective adsorption mechanism of NaX zeolite for the high electronegative metal ions could mainly result from the negatively charged O in the Si-O-Al structure of the NaX zeolite, hence heavy metal ions with high electronegativity display a strong affinity for the electron cloud of the oxygen atoms in the Si-O-Al. This study could evaluate the application and efficiency of zeolite in separating and recovering certain metal ions from industrial wastewater. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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19 pages, 4072 KiB

Open AccessArticle

Thermodilatometric Study of the Decay of Zeolite-Bearing Building Materials

by Michele Pansini, Angelo Cappi, Vincenzo Monetti, Enrico Di Clemente, Maurizio de Gennaro, Marco D’Amore, Rosa Buccino, Pierpaolo Santimone Nuzzi and Bruno de Gennaro

Materials 2021, 14(13), 3551; https://doi.org/10.3390/ma14133551 - 25 Jun 2021

Cited by 1 | Viewed by 1253

Abstract

Six zeolite-bearing rocks, often used as building materials, were analyzed by thermodilatometry, together with a rock not bearing zeolites and a plaster covering a containing wall made of zeolite-bearing dimension stones, up to 250 °C. The main results obtained were the following: (i) the zeolite-bearing rocks exhibited very small, if any, positive variation of ΔL/L_o (%) up to about 100 °C, whereas they more or less shrank in the temperature range 100–250 °C (final values ranging from −0.21 to −0.92%); (ii) the rock not bearing zeolites regularly expanded through the whole temperature range, attaining a final value of 0.19%; (iii) the plaster showed a thermodilatometric behavior strongly affected by its water content. Obtained results were interpreted based on plain thermal expansion, shrinkage by dehydration, cation migration and thermal collapse of the zeolitic structure. The decay of the zeolite-bearing building materials was essentially related to: (i) the large differences recorded in the thermodilatometric behavior of the various rocks and the plaster; (ii) the different minerogenetic processes that resulted in the deposition of the various zeolite-bearing rocks. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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25 pages, 9684 KiB

Open AccessArticle

Preparation of Synthetic Zeolites from Coal Fly Ash by Hydrothermal Synthesis

by David Längauer, Vladimír Čablík, Slavomír Hredzák, Anton Zubrik, Marek Matik and Zuzana Danková

Materials 2021, 14(5), 1267; https://doi.org/10.3390/ma14051267 - 7 Mar 2021

Cited by 29 | Viewed by 3088

Abstract

Large amounts of coal combustion products (as solid products of thermal power plants) with different chemical and physical properties cause serious environmental problems. Even though coal fly ash is a coal combustion product, it has a wide range of applications (e.g., in construction, metallurgy, chemical production, reclamation etc.). One of its potential uses is in zeolitization to obtain a higher added value of the product. The aim of this paper is to produce a material with sufficient textural properties used, for example, for environmental purposes (an adsorbent) and/or storage material. In practice, the coal fly ash (No. 1 and No. 2) from Czech power plants was firstly characterized in detail (X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX), particle size measurement, and textural analysis), and then it was hydrothermally treated to synthetize zeolites. Different concentrations of NaOH, LiCl, Al₂O₃, and aqueous glass; different temperature effects (90–120 °C); and different process lengths (6–48 h) were studied. Furthermore, most of the experiments were supplemented with a crystallization phase that was run for 16 h at 50 °C. After qualitative product analysis (SEM-EDX, XRD, and textural analytics), quantitative XRD evaluation with an internal standard was used for zeolitization process evaluation. Sodalite (SOD), phillipsite (PHI), chabazite (CHA), faujasite-Na (FAU-Na), and faujasite-Ca (FAU-Ca) were obtained as the zeolite phases. The content of these zeolite phases ranged from 2.09 to 43.79%. The best conditions for the zeolite phase formation were as follows: 4 M NaOH, 4 mL 10% LiCl, liquid/solid ratio of 30:1, silica/alumina ratio change from 2:1 to 1:1, temperature of 120 °C, process time of 24 h, and a crystallization phase for 16 h at 50 °C. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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Review

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24 pages, 2878 KiB

Open AccessReview

A Review on the Application of Zeolites and Mesoporous Silica Materials in the Removal of Non-Steroidal Anti-Inflammatory Drugs and Antibiotics from Water

by Agnieszka Grela, Joanna Kuc and Tomasz Bajda

Materials 2021, 14(17), 4994; https://doi.org/10.3390/ma14174994 - 1 Sep 2021

Cited by 26 | Viewed by 4180

Abstract

Zeolites and mesoporous silica materials are effective adsorbents that can be useful for the removal of various pharmaceuticals including non-steroidal anti-inflammatory drugs and antibiotics from low-quality water. This paper summarizes the properties and basic characteristics of zeolites and mesoporous silica materials and reviews the recent studies on the efficacy of the adsorption of selected non-steroidal medicinal products and antibiotics by these adsorbents to assess the potential opportunities and challenges of using them in water treatment. It was found that the adsorption capacity of sorbents with high silica content is related to their surface hydrophobicity (hydrophilicity) and structural features, such as micropore volume and pore size, as well as the properties of the studied medicinal products. This review can be of help to scientists to develop an effective strategy for reducing the amount of these two groups of pharmaceuticals in wastewater. Full article

(This article belongs to the Special Issue Zeolitic Materials: Structure, Properties, and Applications)

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