Synthesis and structure determination via ultra-fast electron diffraction of the new microporous zeolitic germanosilicate ITQ-62

[EN] Here, we present the synthesis and structure determination of the new zeolite ITQ-62. Its structure was determined via ultra-fast electron diffraction tomography and refined using powder XRD data of the calcined material. This new zeolite contains a tridirectional channel system of highly distorted 8-rings, as well as a monodirectional 12-ring channel system.The authors gratefully acknowledge financial support from the Spanish Government (MAT2015-71842-P and MAT2015-71261-R MINECO/FEDER and Severo Ochoa SEV-2016-0683). The authors thank ALBA Light Source for beam allocation at the beamline MSPD, and specially thank the Electron Microscopy Service of the Universitat Politecnica de Valencia. Finally, the authors thank Dr Alejandro Vidal and Dr Teresa Blasco for helping in the NMR data discussion.Bieseki, L.; Simancas Coloma, R.; Jorda Moret, JL.; Bereciartua-Pérez, PJ.; Cantin Sanz, A.; Simancas-Coloma, J.; Pergher, SB.... (2018). 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Zeolite A synthesis employing a brazilian coal ash as the silicon and aluminum source and its applications in adsorption and pigment formulation

Zeolite A was synthesized using the coal ash from Siderópolis/RS - Brazil. The synthesis was based on a standard IZA synthesis using coal ash as the Si and Al source. XRF analysis showed that the coal ash has a Si/Al ratio of 1.52, which is close to the Si/Al ratio required to produce zeolite A (1.0). The synthesized materials were analyzed by XRD, SEM and N2 adsorption. More crystalline materials were obtained during synthesis when an additional treatment was applied at a temperature of 353 K at the dissolution of NaOH step. The product formed after 4 hours was the most crystalline, but even the product formed after 1 hour proved to be better than that formed using the standard 4 hours IZA synthesis. The zeolites synthesized by this method had an adsorption capacity of 120 mg.g-1 for Ca2+, half the capacity of commercial zeolite A (300 mg.g-1). It was not possible to obtain blue or green pigments using the synthesized zeolite A

Development of a Zeolite A/LDH Composite for Simultaneous Cation and Anion Removal

Wastewater from the oil industry is a major problem for aqueous environments due to its complexity and estimated volume of approximately 250 million barrels per day. The combination of these petroleum pollutants creates risks to human health, and their removal from the environment is considered a major problem in the world today. Thus, this work has the objective of studying the treatment of this type of effluent through the adsorption method using the following exchange materials: cationic, anionic, their combination by a sequential method, and a composite material. Zeolite A, a layered double hydroxide (LDH), and the new composite material formed by zeolite A and LDH structures were synthesized for this study. All were used for the simultaneous treatment of cations and anions in a complex sample such as water produced from petroleum production. The composite demonstrated an excellent ability to simultaneously remove cations and anions. The results obtained after the different treatment modes of the effluent using different materials varied from 85% to 100% for the removal of cations and from 56% to 99.7% for the removal of anions

Organic-Free Synthesis of Finned Mordenite Zeolite

Mordenite is a well-known zeolite widely used for industrial processes. However, its pore architecture can be inconvenient due to diffusional issues. A study of the synthesis parameters from an organic-free dense gel was carried out to control the crystal morphology, which resulted in finned mordenite zeolite particles. The obtained materials were characterized by XRD, FTIR, 29Si and 27Al MAS-NMR, elemental analysis, nitrogen physisorption, SEM, and TEM. We found that careful manipulation of the hydrothermal parameters directly affected the sizes and morphologies of the crystallites and particles, as well as the textural properties of the final products. Additionally, it was found that mordenite could exhibit a fin morphology with additional mesoporosity, which is a promising means to reduce the diffusional problems of one-dimensional-channel zeolites

Hydrothermal Synthesis of Silicoaluminophosphate with AEL Structure Using a Residue of Fluorescent Lamps as Starting Material

Silicoaluminophosphate molecular sieves of SAPO-11 type (AEL structure) were synthesized by the hydrothermal method, from the residue of a fluorescent lamp as a source or Si, Al, and P in the presence of water and di-propyamine (DPA) as an organic template. To adjust the P2O5/SiO2 and Si/Al and ratios, specific amounts of silica, alumina, or alumina hydroxide and orthophosphoric acid were added to obtain a gel with molar chemical composition 1.0 Al2O3:1.0 P2O5:1.2 DPA:0.3 SiO2:120 H2O. The syntheses were carried out at a temperature of 473 K at crystallization times of 24, 48, and 72 h. The fluorescent lamp residue and the obtained samples were characterized by X-ray fluorescence, X-ray diffraction, scanning electron microscopy, and BET surface area analysis using nitrogen adsorption isotherms. The presence of fluorapatite was detected as the main crystalline phase in the residue, jointly with considered amounts of silica, alumina, and phosphorus in oxide forms. The SAPO-11 prepared using aluminum hydroxide as Al source, P2O5/SiO2 molar ratio of 3.6 and Si/Al ratio of 0.14, at crystallization time of 72 h, achieves a yield of 75% with a surface area of 113 m2/g, showing that the residue from a fluorescent lamp is an alternative source for development of new materials based on Si, Al, and P

Material ITQ-62, su procedimiento de obtención y su uso

[EN] The invention relates to a microporous crystalline material, a method for obtaining same and the use thereof, the material having composition: x X2O3: y YO2: z ZO2, wherein X is a trivalent element such as Al, B, Fe, In, Ga, Cr or mixtures thereof, (y+z)/x being able to take values between 9 and infinity; Y corresponds to a tetravalent element such as Ti, Sn, Zr, V or mixtures thereof, z/y being able to take values between 10 and infinity; and Z corresponds to a tetravalent element selected from Si and Ge or mixtures thereof.[ES] En la presente invención, se presenta un material cristalino microporoso, su procedimiento de obtención y uso, que tiene una composición: x X2O3: y YO2: z ZO2 en la que X es un elemento trivalente tal como Al, B, Fe, In, Ga, Cr, o mezclas de estos, donde (y+z)/x puede tomar valores entre 9 e infinito; Y corresponde a un elemento tetravalente tal como Ti, Sn, Zr, V o mezclas de ellos, donde z/y puede tomar valores entre 10 e infinito; Z corresponde a un elemento tetravalente seleccionado entre Si y Ge o mezclas de ellos.Consejo Superior de Investigaciones Científicas (España), Universitat Politécnica de ValènciaA1 Solicitud de patente con informe sobre el estado de la técnic

Memory Effect on a LDH/zeolite A Composite: An XRD In Situ Study

In this memory effect study, hydrotalcite-type compounds in the lamellar double hydroxide-like (LDH)/zeolite A composite material were analyzed using X-Ray Diffration XRD) in situ experiments. Three samples were analyzed: Al,Mg-LDH, Al,Mg-LDH/ZA composite, and a physical mixture (50/50 wt%) of zeolite A and Al,Mg-LDH. The Al,Mg-LDH sample was treated at 500 °C in an O2 atmosphere and subsequently rehydrated. The Al,Mg-LDH/ZA composites had three treatments: one was performed at 300 °C in a He atmosphere, and two treatments were performed with an O2 atmosphere at 300 and 500 °C. In the physical mixture, two treatments were carried out under O2 flow at 500 °C and under He flow at 300 °C. Both went through the rehydration process. All samples were also analyzed by energy dispersive spectroscopy (EDS) and scanning electron microscopy (SEM). The results show that the LDH phase in the Al,Mg-LDH/ZA compounds has memory effects, and thus, the compound can be calcined and rehydrated. For the LDH in the composite, the best heat treatment system is a temperature of 300 °C in an inert atmosphere