SYNTHESIS AND CHARACTERIZATION OF NOVEL ZEOLITE-X FOR SMALL MOLECULE ADSORPTION

Year 2024, , 1 - 16, 03.04.2024

Abdulrazak Shittu

https://doi.org/10.55549/zbs.1427878

Abstract

Zeolite Na-X was successfully synthesized from Oke-Ako raw kaolin clay. The clay was soaked in water, beneficiated and calcined at 650oC for three hours, to obtain a more reactive amorphous metakaolin. The metakaolin was dealuminated using 60wt% tetraoxosulphate (VI) acid, washed to neutrality using gravimetric method after reactions for five, ten and fifteen minutes respectively. The gel formed was aged for five days at room temperature and subjected to crystallization at a temperature of 110oC for reaction times of 8 hrs. The samples of raw, beneficiated, metakaolin and the synthesized zeolite-X were characterized using XRF, XRD, SEM, FT-IR and (Brunauer-Emmett-Teller (BET) analytical techniques. The XRF analysis confirmed the status of the raw kaolin and gave a positive status of the pretreatment and zeolitization processes. The intensity of crystalinity value from XRD were recorded for beneficiated, metakaolin and zeolite-X at 8hrs crystallization reaction time, while the SEM of the synthesized zeolite-X at 8hrs tends to be more desirable. Determination of the chemical and elemental compositions by X-ray Fluorescence (XRF), crystalline phases by X-ray Diffraction (XRD), surface morphology by Scanning Electron Microscopy (SEM) and molecular vibration of units by Fourier Transform Infrared Spectrophotometry (FT-IR) were done. The results showed that the zeolite-X synthesized from the Oke-Ako kaolin (OAK) was more crystalline/larger with sharper peaks on both XRD and FTIR. The XRF of Si/Al values of 1.95 and 1.78 were obtained for D5ZNa-X and ZNa-X respectively from Oke-Ako kaolin samples. XRD results supported the XRF values. Sharper zeolitic characteristic O-H stretching bands at 3362 cm−1 was recorded and Si-O Stretching band at 969 Cm-1 for both samples. The specific surface area of 266.97 m2/g was observed in ZNa-X sample with larger surface area than D5ZNa-X of specific surface area of 105.747m2/g. The results confirmed that zeolites-X was produced from Oke-Ako kaolin samples when compared with other results from literature. Generally the performance evaluation could be summarized that, these results illustrate the intricate interplay of different parameters on ammonia adsorption capacity using zeolites, providing valuable insights into the behaviour of zeolite as adsorbents in ammonia removal processes for optimizing ammonia removal applications and developing efficient, sustainable environmental remediation solution.

Keywords

Beneficiation, Metakaolin, Dealumination, X-Ray Flouresence, (Brunauer-Emmett-Teller (BET), Crystalization, Zeolitization

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