Preparation and modification of zeolite A from kaolin for catalytic methanation of carbon dioxide

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In this research, in an attempt to make use of the kaolin resources in Vietnam, we present a synthetic process of zeolite A via hydrothermal from kaolinite, together with the modification process of zeolite A using different metallic cations. The characteristics of the prepared zeolite LTAs such as chemical composition and crystalline structure, as well as their catalytic activity in the methanation reaction of carbon dioxide (CO2) to methane (CH4) were extensively investigated.

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Nội dung Text: Preparation and modification of zeolite A from kaolin for catalytic methanation of carbon dioxide

Cite this paper: Vietnam J. Chem., 2023, 61(2), 170-177 Research article DOI: 10.1002/vjch.202200027 Preparation and modification of zeolite A from kaolin for catalytic methanation of carbon dioxide Do Cao Son1,2, Vo Thi Kieu Anh4, Nguyen Thi Thom4, Huynh Le Thanh Nguyen2,3*, Le Viet Hai2,3, Co Thanh Thien2,3, Nguyen Thai Hoang2,3, Tran Dai Lam4, Pham Thi Nam4, Nguyen Thi Thu Trang1,4* 1 Graduate University of Sciences and Technology, Vietnam Academy of Science and Technology (VAST), 18 Hoang Quoc Viet road, Cau Giay district, 10000 Hanoi, Viet Nam 2 University of Science, 227 Nguyen Van Cu road, district 5, 70000 Ho Chi Minh City, Viet Nam 3 Vietnam National University of Ho Chi Minh City, Vo Truong Toan road, Linh Trung district, Thu Duc City, 70000 Ho Chi Minh City, Viet Nam 4 Institute of Tropical Technology, Vietnam Academic of Science and Technology (VAST), 18 Hoang Quoc Viet road, Cau Giay district, 10000 Hanoi, Viet Nam Submitted February 28, 2022, Revised April 28, 2022, Accepted May 24, 2022 Abstract Different types of zeolite including Zeolite A are prepared from natural kaolin originated in Vietnam. Raw kaolin was collected from Phu Tho, Vietnam, underwent metakaolization at 650 °C within 2 hours and alkalination with NaOH to synthesize various zeolitic samples. Various characterization techniques were performed, including X- Ray Diffraction, Fourier-transform infrared spectroscopy, and Scanning Electron Microscopy. Different concentrations of NaOH were utilized to study the difference of the prepared zeolite. Nickel-doped zeolite A samples with different nickel loading were also prepared via ion exchange method and were employed as catalyst for the hydrogenation of carbon dioxide (CO2) to obtain methane (CH4). The best catalytic activity of 55.2 %CO2 conversion and 92.7 %CH4 selectivity was achieved with 10 %Ni/ZM1 at 350 °C, 1 atm, H2:CO2 ratio of 4:1, and gas hourly space velocity of 9,000 mL.g-1.h-1. This study demonstrates a promising pathway of modifying Vietnamese natural kaolin as a low-cost but an effective alternative material for the preparation of zeolite A and its application in the carbon dioxide methanation reaction. Keywords. Zeolite A, kaolin, carbon dioxide, methane, methanation. 1. INTRODUCTION linked with the oxygen atoms, making up a porous framework and a highly ordered channel structure.[8] Situated in the central part of Southeast Asia and The cations present in the channels can be replaced belonging to the Eurasian lithosphere plate, Vietnam by other cations via adsorption or ion exchange, thus is blessed with a rich diversity of mineral resources, the adsorption capability as well as the catalytic possessing more than 5000 mineral deposits properties of zeolite.[9] As a result, zeolites have been consisting of more than 60 types of minerals.[1] attracting a lot of interest among researchers all Recently, many of them are being exploited, around the world. Zeolites are commonly prepared by including oil, natural gas, coal, kaolin, silica sand, hydrothermal reaction from various sources of lead, zinc, copper, gold, phosphate, fluorite, etc. as amorphous or soluble Si and Al, both academically well as mineral and thermal springs.[2] Especially, and industrially. Currently, different natural sources, kaolinite-rich minerals can be extracted from the soils namely kaolin, clay, fly ash, bauxite, feldspar, natural originating from the minerals in the Red River Delta oxides and other silica sources,[10,11] were employed region, the North Midland and the Mountainous to synthesize zeolites in order to benefit from their region of Vietnam.[3] highly porous structures, large specific surface area, Zeolites are materials with a broad range of high ionic exchange capacity, inexpensiveness and applications, for example, catalysis,[4] ion-exchange easy availability.[12] membranes,[5] chemical separation,[6] and gas Kaolinite (Al2O3.2SiO2.2H2O) has largely been sorption.[7] They belong to aluminosilicate mineral utilized as an alternative source of aluminum and family in which the tetrahedral Si and Al atoms are silicon in zeolite synthesis due to its abundance in 170 Wiley Online Library © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH
25728288, 2023, 2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202200027 by Readcube (Labtiva Inc.), Wiley Online Library on [02/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Huynh Le Thanh Nguyen et al. nature and its ability to synthesize zeolite without employed as the reactant gases and carrier gas for the much need of purification, including zeolites Linde catalytic testing. Type A, X and Y, as well as several other types of zeolites.[13] Zeolite LTA was prepared by 2.2. Preparation of zeolite from metakaolin hydrothermally treating metakaolinite with alkaline.[14] Zeolite N was synthesized by In a typical process, different calculated amounts of hydrothermal treatment of kaolinite or metakaolinite NaOH pellets was put into distilled water to prepare with KOH, KCl, and H2O.[15] Hydrothermal x M NaOH solutions, then metakaolin was added transformation of kaolinite-rich clay was performed (Na:Al:Si = x:1:1). The reaction mixture was kept to prepare sodalite and cancrinite.[16] Zeolite LTJ was stirring at room temperature for 1 h, then at 65 ºC for synthesized from raw kaolinite material via another 1 h. The hydrothermal treatment of the hydrothermal processes with potassium hydroxide.[17] samples was carried out in a Teflon-lined stainless- In addition, several other zeolitic materials were also steel autoclave at 120 ºC for 24 h. The samples after prepared from kaolinite or metakaolinite, such as hydrothermal treatment were collected by filtration FAU,[18] LSX zeolite,[19] NaY zeolite,[20] Beta,[21] and and washed with distilled water until neutral pH to ZSM-5,[22] etc. remove excess alkali, then were dried overnight at 80 In terms of catalysis, zeolite is recognized to be a °C, which were denoted as ZMx. highly potential catalysts or catalyst supports thanks to their large surface area, high porosity, good 2.3. Preparation of nickel-doped zeolite adsorption capacity, and easy separation from reactants and products,[23] especially in carbon The mixture containing the prepared zeolite and 100 dioxide (CO2) capture and conversion. In the last few mL solution of aqueous NiCl2 at different years, numerous researches on the utilization of concentrations was stirred for 24 hours at 65 °C. After zeolite-based materials as CO2 methanation catalysts the reaction was completed, the resultant solid was have been reported.[24] Many types of zeolite were filtered, washed with distilled water and dried at 80 employed as supports for the nickel catalyst, namely °C for 2 h. Finally, the obtained dried nickel-doped zeolite Y, ultra-stable Y zeolite (USY), BEA, MOR, zeolite was calcined at 500 °C for 4 hours, and ZSM-5, 5A, 13X, with a fairly high carbon dioxide denoted as y%Ni/ZMx. conversion (from 33 to 85 %) and a nearly absolute methane selectivity (from 75 to 100 %).[24] However, 2.4. Catalyst characterization method the use of zeolite A as a support for the hydrogenation of CO2 to yield CH4 is still limited. The phase component of the materials was In this research, in an attempt to make use of the investigated with X-ray diffraction (XRD) analysis kaolin resources in Vietnam, we present a synthetic using a D8-Advances (Bruker) diffractometer with process of zeolite A via hydrothermal from kaolinite, CuKα radiation (wavelength λ = 1.5416 Å). FT-IR together with the modification process of zeolite A spectra were examined on Nicolet iS10, (Thermo using different metallic cations. The characteristics of Scientific). Surface morphology together with the prepared zeolite LTAs such as chemical elemental analysis were performed on JSM-6510LV composition and crystalline structure, as well as their instrument coupled with Oxford EDX analysis. catalytic activity in the methanation reaction of carbon dioxide (CO2) to methane (CH4) were 2.5. Carbon dioxide (CO2) methanation extensively investigated. CO2 hydrogenation to methane was performed in a 2. MATERIALS AND METHODS fixed-bed tubular reactor with 0.5 g of catalysts at atmosphere pressure. CO2 and H2 were supplied with 2.1. Materials and chemicals H2:CO2 ratio of 4:1 and GHSV (gas hourly space velocity) of 9,000 mL.g-1.h-1. Gas chromatography Kaolin was collected from Hung Vuong Mineral Joint with FID and PDD detector was used for analyzing Stock Company, Phu Tho province. NaOH pallets (97 the products and effluent gas. Conversion of CO2 and %) and NiCl2.6H2O (95 %) was purchased Fischer selectivity of CH4 were determined using the Chemicals (USA). Distilled water was utilized in all following equations: of the catalyst preparation. Metakaolin was obtained FCO2 in −FCO by kaolin calcination at 650 ºC for 3 h. Ultra-high CO2 conversion (%) = 2 out × 100 purity CO2, H2, and He (purity > 99.5 %) was FCO2 in © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 171
25728288, 2023, 2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202200027 by Readcube (Labtiva Inc.), Wiley Online Library on [02/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Preparation and modification of zeolite A… FCH4 out The conversion of kaolin to metakaolin as well as CH4 selectivity (%) = × 100 the transformation of metakaolin to different types of FCO2 in − FCO2 out where F is the molar flow rate for a particular zeolite was also elucidated through FT-IR in figure 2. compound. First, kaolin exhibits the 3691 and 3623 cm-1 bands, which are ascribed to the stretching vibrations of 3. RESULTS AND DISCUSSION hydroxyl groups of kaolinite.[33] Other than that, the peak at 1105 cm-1 is accredited to the Si-O stretching 3.1. Characterization of the synthesized zeolites vibrations, whereas the peaks at 1036 and 1010 cm-1 are attributed to the the Si-O-Si and Si-O-Al lattice XRD diagrams of the untreated and thermally treated vibration, respectively.[34] The OH bending vibration kaolin (figure 1) exhibited the peaks at 2θ = 12.2, modes are situated at 939 and 916 cm-1.[35] 19.6, 20.2, 21.0, 22.8, 24.6, 26.1, 34.8, 35.7, 38.1, Furthermore, the bands at 752, 697 and 536 cm-1 38.9 and 45.4º, which is similar to the technical belong to different Si-O or Al-O vibrations, with the kaolin.[25] Besides the peaks of kaolin Al2Si2O5(OH)4 former two associated to the deformation of the at 12.2, 20.2, 24.6, 35-40º and 45.4º,[26] there are other tetrahedral and octahedral layers, respectively.[36] impurity peaks of chlorite at 19.8º, quartz at 21.0 and 26.1º, and cristobalite at 22.8º. After heat treatment at 650 ºC, metakaolin Al2Si2O7 is formed, signaled by the vanishing of kaolinite XRD peaks, together with the emergence of an amorphous aluminosilicate phase (the broad peaks at 2θ = 25-35º).[27] 650 ºC was chosen to be the temperature of the heat treatment, as higher temperature calcination might result in the formation of different undesired products, namely mullite or cristobalite.[28] The activation of kaolin at 650 ºC yielded amorphous metakaolin, thus promoting its reactivity for further zeolitic material synthesis. ZM5 sample was prepared via thermal treatment in autoclave of metakaolin with 5M NaOH at 120 ºC for 24 h. In the XRD patterns (Figure 1), there were new peaks appeared at 13.7, 24.1, 34.3, 42.5, 51.8, Figure 1: X-ray diffraction patterns of different 57.8, 61.7, 63.7 and 69.2º, which are attributed to synthesized zeolites hydrosodalite, or sodalite octahydrate[29] – a type of zeolite of formula [Na6(H2O)8][Si6Al6O24], as Next, kaolin transformation to metakaolin is reported by Treacy and Higgins.[30] When increasing proven as the kaolinite characteristic peaks the NaOH solution concentration to 10 M and 20 M, disappeared along with the appearance of the the ZM10 and ZM20 samples exhibited some more characteristic bands of metakaolin at 1041, 792, 635 peaks at 19.7º, 28.1, 31.5, 37.5, and 49.9º, together and 579 cm-1.[37] A red shift was observed for the with the repeating peaks of hydrosodalite,[31] which is Si-O vibration peaks, from 1036 and 1010 cm-1 in ascribed to hydroxysodalite, Na6[AlSiO4]6.(H2O)4, kaolin to 1041 cm-1 in metakaolin, belonging to the signaling the lack of H2O group in the structure of amorphous SiO2.[38] Additionally, the Al(O,OH)6 hydrosodalite when synthesized at high alkaline octahedron stretching vibration in kaolin at 536 cm-1 concentration. is also replaced by that of AlO4 tetrahedron in The XRD pattern of ZM1, synthesized from 1 M metakaolin at 792 cm-1.[39] NaOH solution, matched the characteristic peaks of The previously mentioned alkaline concentration zeolite A, Na12[(AlO2)12(SiO2)12].27H2O, at 2θ values effect can also be elucidated by FT-IR. At low NaOH of 10.3, 12.6, 16.2, 21.8, 24.0, 26.2, 27.2, 30, 30.9, concentration (1 M), zeolite A was synthesized, as 31.1, 32.6, 33.4, 34.3, 40.1, 41.2, 44.2 and 47.6º.[30] proven by the appearance of the characteristic Therefore, it can be reasonably concluded that the vibration of the double four rings of zeolite A at 560 types of the synthesized zeolites mainly depends on cm-1. Furthermore, the SiO4 and AlO4 units of zeolite the amount of water or the sodium hydroxide A displayed the internal asymmetric stretching concentration in the reaction mixture, as similarly vibration at 1005 cm-1 and the internal symmetric one proven in another previous study. [32] at 664 cm-1.[40] In addition, the presence of H2O and © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 172
25728288, 2023, 2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202200027 by Readcube (Labtiva Inc.), Wiley Online Library on [02/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Huynh Le Thanh Nguyen et al. OH groups in the zeolite A structure was verified by The surface morphology as well as element the two absorptions at 1651 cm-1 and 3429 cm-1, constituents of the nickel-doped zeolite were studied respectively.[41] by SEM-EDS. Figure 4a and 4b revealed the At higher NaOH concentration (5M), the appearance of the nickel oxide particles on the Zeolite synthesized zeolite was no longer zeolite A, as its A surface. Moreover, the EDS spectra of the characteristic peak at 560 cm-1 disappeared. Instead, 10%Ni/ZM1 sample is given in figure 4c, exhibiting hydrosodalite was formed, as proven by its the elemental constituents of Ni together with other characteristic absorption bands. Specifically, the 983 element such as Na, Al, Si and O (from zeolite), cm-1 peak is ascribed to the asymmetric atomic further indicating the successful incorporation of vibration, and the 727, 701, 659 cm-1 peaks are nickel into zeolite A. accredited to the symmetrical atomic vibration of the Si-O and Al-O bonds.[42] In addition, the absorption peaks at 3483 cm-1 and 1635 cm-1 can be assigned to the stretching vibration of the OH group in the structure of zeolite and the deformation vibration of water molecules, respectively, which is similar to zeolite A.[43] There is also a weak absorption band at 1440 cm-1, probably due to the excess alumina present in the zeolitic pores.[44] Further elevation of the NaOH concentration (10 M and 20 M) resulted in the formation of hydroxysodalite, which was signaled by the diminishment of the 3483 cm-1 and 1635 cm-1 absorption vibration peaks. Besides, there is not much change in other FT-IR bands which are attributed to the sodalite structure. Figure 3: XRD patterns of the different nickel- doped zeolites Wavenumber (cm-1) Figure 2: FT-IR spectra of different synthesized zeolites 3.2. Characterization of the nickel-doped zeolites Figure 4: SEM images of ZM1 (a), 10 %Ni/ZM1 As zeolite A was successfully synthesized via thermal (b), and EDS spectrum of the 10 %Ni/ZM1(c) treatment of metakaolin and 1 M NaOH, ZM1 was employed as support for the nickel catalyst in the 3.3. Catalytic activity of catalysts following experiments. XRD patterns of different nickel-doped zeolite powders are presented in figure The catalytic activities of all zeolitic catalysts for the 3, where the newly appeared peaks at 2θ = 37.0 and methanation of carbon dioxide, namely conversion of 43.0º can be ascribed to the face-centered cubic phase CO2 and selectivity of CH4, was investigated under a of NiO (JCPDS file No. 78-0643),[45] indicating that CO2:H2:He = 1:4:5 molar ratio with a GHSV of 9000 nickel was well loaded onto the materials. mL.g-1.h-1 at 1 atm from 150 to 500 °C. From figure © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 173
25728288, 2023, 2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202200027 by Readcube (Labtiva Inc.), Wiley Online Library on [02/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Preparation and modification of zeolite A… 5, it was observed that increasing the nickel exceeded 10 %, implying that the best catalytic percentage initially enhanced the catalytic activity, activity could be achieved with an appropriate but then the carbon dioxide conversion and methane amount of Ni loading. It was mentioned that the selectivity diminished when the nickel loading catalytic activity of the zeolite-supported nickel materials for the CO2 methanation requires the presence of metallic nickel, which may be formed in situ if the material surface can be cover completely with a nickel monolayer when the Ni loading is sufficient.[46] Higher nickel loading resulted in the formation of “bulk-like” NiO particles,[47] which can be easily reduced by H2 in the reaction mixture gas, leading to the lack of hydrogen gas and the increased carbon monoxide production. Similarly, when first elevating the temperature, the conversion of CO2 and selectivity of CH4 was enhanced, reaching maximum value of 55.2 % and 92.7 %, respectively, at 350 °C, which are nearly comparable to other published zeolite-based nickel catalysts (table 1). Then, the catalytic activity deteriorated, indicating the presence of the reverse Temperature (oC) water-gas shift (RWGS) reaction that is favorable at elevated temperature, and as a result an increased in carbon monoxide selectivity (equation 2). Additionally, high temperatures can bring about carbon deposition, thus lessening the catalytic activity.[48] CO2 + 4 H2 → CH4 + 2H2O (1) CO2 + H2 → CO + H2O (2) 4. CONCLUSIONS In this work zeolite A has successfully been synthesized from Vietnamese kaolin using 1 M NaOH solution. The importance of NaOH concentration was also established. Furthermore, nickel was also incorporated into the prepared zeolite Temperature (oC) A, and the methanation reaction of carbon dioxide Figure 5: (a) CO2 conversion and (b) CH4 selectivity using zeolite-A-supported nickel catalysts was of different nickel-doped zeolites conducted. The best catalytic activity of 55.2 % Table 1: Most performant catalysts based on zeolites reported in the literature Treduction Treaction GHSV P CO2 CH4 Catalyst H2:CO2 Ref. (ºC) (ºC) (mL.g-1.h-1) (atm) conversion (%) selectivity (%) [49] 5%Ni/Y 500 4:1 300 50000 1 49 96 [50] 15%Ni/USY 470 4:1 400 43000 1 73 97 [51] 15%Ni/BEA 470 4:1 400 43000 1 71 97 [51] 15%Ni/MOR 470 4:1 400 43000 1 66 95 [51] 15%Ni/ZSM-5 500 4:1 400 43000 1 65 95 [52] 10%Ni/ZSM-5 500 4:1 400 2400 1 76 75 [53] 5%Ni/5A 500 4.05:1 300 92 1 85 100 [53] 5%Ni/13X 500 4.05:1 300 92 1 85 100 10%Ni/ZM1 350 4:1 350 9000 1 55.2 92.7 This work © 2023 Vietnam Academy of Science and Technology, Hanoi & Wiley-VCH GmbH www.vjc.wiley-vch.de 174
25728288, 2023, 2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/vjch.202200027 by Readcube (Labtiva Inc.), Wiley Online Library on [02/05/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Vietnam Journal of Chemistry Huynh Le Thanh Nguyen et al. conversion of carbon dioxide and 92.7 % selectivity Chem Rev, 2014, 114, 4807-37. of methane was achieved with 10 % Ni catalyst, 350 12. A. E. Gaidoumi, A. C. Benabdallah, B. E. Bali, A. °C, 1 atm, H2:CO2 ratio of 4:1, and 9,000 mL.g-1.h-1. Kherbeche. 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