Optimization of Pretreatment and Hydrothermal Process of Na-X Zeolite from Kaolin and Metakaolin

Hartati Hartati, Satya Candra Wibawa Sakti, Putri Bintang Dea Firda, Chabibah Saidah

Abstract


Synthesis of Na-X zeolite was conducted from kaolin and metakaolin. Synthesis varied in its pretreatment method and hydrothermal conditions. The pretreatment methods used were: conventional alkaline, alkaline fusion and conventional fluoride. Hydrothermal conditions for the experiments were gradual temperature 40 oC  (6h), 60 oC (6h), 80 oC (12h), and constant temperature 80 oC for 24 h, 100 oC for 24 and 100 oC for 48 h. Synthesized products were characterized by X-Ray Diffraction (XRD), Fourier Transform InfraRed (FTIR), Scanning Electron Microscopy-Energy Dispersive X-Ray (SEM-EDX), and N2 Isotherm Adsorption/Desorption method. The result showed that pre-treatment by conventional fluoride could not produce Na-X zeolite, synthesis by conventional alkaline and alkaline fusion with hydrothermal at 100 oC (48h), 100 oC (24 h), and gradual temperature produce Na-X zeolite with Na-P1 or Na-A zeolite as impurities, while synthesis from metakaolin by conventional alkaline with hydrothermal at 80 oC for 24 hours produced pure Na-X zeolite. Na-X zeolite and NaP1 zeolite with hierarchical pores were synthesized through alkali fusion with hydrothermal at 100 oC for 24 hours. 

 


Keywords


NaX zeolite; kaolin; conventional alkaline; conventional fluoride; hydrothermal

References


Ayele L, Pérez-pariente J, Chebude Y, Díaz I. 2016. Applied clay science conventional versus alkali fusion synthesis of zeolite a from low grade kaolin. Applied Clay Science. 132–133: 485–490. https://doi.org/10.1016/j.clay.2016.07.019.

Bates S, Zografi G, Engers D, Morris K, Crowley K, Newman A. 2006. Analysis of amorphous and nanocrystalline solids from their X-Ray diffraction patterns. Pharm Res. 23(10): 2333-2349.

Belviso C, Cavalcante F, Lettino A, Fiore S. 2013. Applied clay science a and x-type zeolites synthesised from kaolinite at low temperature. Applied Clay Science. 80–81: 162–168. https://doi.org/ 10.1016/j.clay.2013.02.003

Byrappa KM, Kumae VS. 2007. Characterization of zeolite by infrared spectroscopy. Asian Journal of Chemistry. 19(6): 4933-4935.

Caballero I, Colina FG, Costa J. 2007. Synthesis of X-type zeolite from dealuminated kaolin by reaction with sulfuric acid at high temperature, Industrial and Engineering Chemistry Research. 46(4): 1029–1038.

Cejka J, Corma A, Zones S. 2010. Zeolites and Catalysis: Synthesis, Reactions and Applications.https://doi.org/10.1002/9783527630295

Chen D, Hu X, Shi L, Cui Q, Wang H, Yao H. 2012. Applied clay science synthesis and characterization of zeolite X from lithium slag. Applied Clay Science. 59–60: 148–151. https://doi.org/ 10.1016/j.clay.2012.02.017

Chen LH, Li XY, Rooke JC, Zhang YH, Yang XY, Tang Y, Xiao FS, Su BL. 2012. Hierarchically structured zeolites: synthesis, mass transport properties and applications. Journal of Materials Chemistry. 22(34): 17381-17403.

Condon JB. 2006. Surface area and porosity determinations by physisorption: Measurement and theory. Elsevier. Amsterdam.

Flanigen EM, Broach RW, Wilson ST. 2010. Zeolites in industrial separations and catalysis. Zeolites in Industrial Separation and Catalysis. 1–26. https://doi.org/10.1002/9783527629565

Lenarda M, Storaro L, Talon A, Moretti E, Riello P. 2007. Solid acid catalysts from clays : Preparation of mesoporous catalysts by chemical activation of metakaolin under acid conditions. Journal of Colloid and Interface Science. 311(2): 537–543. https://doi.org/10.1016/j.jcis.2007.03.015

Mohiuddin E, Makar Y, Mdleleni MM, Sincadu N, Key D, Tshabalala T. 2016. Synthesis of ZSM-5 from impure and bene fi ciated Grahamstown kaolin: Effect of kaolinite content, crystallisation temperatures and time. Applied Clay Science. 119(2): 213–221. https://doi.org/ 10.1016/j.clay.2015.10.008.

Ozdemir OD, Pişkin S. 2013. Zeolite X synthesis with different sources. International Journal of Chemical, Environmental & Biological Sciences (IJCEBS). 1(2): 229–232.

Pan F, Lu X, Wang Y, Chen S, Wang T, Yan Y. 2014. Microporous and mesoporous materials synthesis and crystallization kinetics of ZSM-5 without organic template from coal-series kaolinite. Microporous and Mesoporous Materials. 184: 134–140. https://doi.org/ 10.1016/j.micromeso.2013.10.013

Reyes CAR, Williams, Craig DW, Oscar MC. 2013. Reactivity Study of Kaolinite and Metakaolinite in Fluoride Media under Hydrothermal Conditions, University of Bobota, Columbia.

Ríos CA, Williams CD. 2012. Crystallization of low silica Na ¬ A and Na ¬ X zeolites from transformation of kaolin and obsidian by alkaline fusion. Ingeniería y Competitividad. 14(2): 125–137.

Ríos CA, Williams CD, Fullen MA. 2009. Nucleation and growth history of zeolite LTA synthesized from kaolinite by two different methods. Applied Clay Science. Elsevier B.V. 42(3–4): 446–454.

Sing KSW, Everett DH, Haul RAW, Moscou L, Pierotti RA, Rouquerol J, Siemieniewska T. 1985. IUPAC-Surface chemistry including catalysis-reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity. Pure & Appl. Chem. 57(4): 603–619.

Tanaka H, Fujii A. 2009. Effect of stirring on the dissolution of coal fly ash and synthesis of pure-form Na-A and -X zeolites by two-step process. Advanced Powder Technology. The Society of Powder Technology Japan., 20(5): 473–479.


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DOI: 10.15408/jkv.v5i2.11326

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