Pengaruh Metode Sintesis secara Solvo-Hidrotermal dan Elektrokimia terhadap Morfologi Struktur HKUST-1 sebagai Katalis Heterogen dalam Reaksi Esterifikasi Asam Palmitat

Witri Wahyu Lestari, Joni Hartono, Dian Wahyu Tri Wulansari, Enri Pramuja, Fauziyah Azhari, Triana Kusumaningsih

Abstract

Pemilihan metode sintesis akan berpengaruh terhadap karakter material yang dihasilkan yang meliputi kristanilitas, morfologi, luas permukaan, maupun kinerja dalam aplikasinya. Pada penelitian ini telah disintesis HKUST-1 secara solvo-hidrotermal dan elektrokimia dalam pelarut EtOH:H2O (1:1 (v/v)) dan diujicobakan sebagai katalis heterogen dalam esterifikasi asam palmitat. Sintesis secara solvo-hidrotermal, berlangsung dalam autoklaf selama 12 jam pada suhu 120 °C. Sementara itu, sintesis HKUST-1 secara elektrokimia digunakan elektroda tembaga, tegangan sel 15 V selama 90 menit dengan bantuan elektrolit TBATFB pada suhu dan tekanan ambien. Uji katalitik reaksi esterifikasi asam palmitat dilakukan dengan metode refluks selama 2 jam. HKUST-1 hasil sintesis menunjukkan kesesuaian puncak dengan pola difraksi standar CCDC 112954. Hasil refinement menunjukkan HKUST-1 yang diperoleh melalui metode solvo-hidrotermal memiliki kemurnian lebih tinggi. Analisis morfologi menggunakan citra SEM menunjukkan HKUST-1 yang disintesis secara solvo-hidrotermal bergeometri oktahedral sempurna dengan ukuran partikel rata-rata 10,28±1,5 μm, sedangkan HKUST-1 yang disintesis secara elektrokimia berbentuk oktahedral cacat (defect) dengan ukuran partikel rata-rata 4,5±1,6 μm. Analisis termal menunjukkan bahwa HKUST-1 hasil sintesis memiliki stabilitas hingga 300 °C. Uji katalitik dalam reaksi esterifikasi asam palmitat dengan etanol dengan keberadaan katalis HKUST-1 (0,6% berat) menunjukkan peningkatan konversi produk dengan konversi yang paling tinggi ditunjukkan pada HKUST-1 yang disintesis dengan metode elektrokimia (mencapai 43,3%).

Effect of Solvo-Hydrothermal and Electrochemical Synthesis Methods on the Structural Morphology of HKUST-1 as a Heterogeneous Catalyst in Palmitic Acid Esterification Reaction. Selection of synthesis method will influence the materials properties including crystallinity, morphology, surface area, and application performance. In this research HKUST-1 was successfully synthesized under solvo-hydrothermal and electrochemical method, and tested as a heterogeneous catalyst in esterification reactions of palmitic acid. Synthesis under solvo-hydrothermal condition was performed in an autoclave at 120 °C for 12h. In addition, the electrochemical synthesis of HKUST-1 using copper electrodes was performed at 15 V in ambient temperature and pressure, for  90 minutes with TBATFB as an electrolyte. The catalytic test in palmitic acid esterification reaction was carried out by reflux for 2h. The HKUST-1 showed conformity with the standard diffraction pattern CCDC 112954. The refinement results shows that solvothermal product has higher purity. Morphological analysis using SEM imaging showed HKUST-1 obtained from solvo-hydrothermal method possess perfect octahedral geometry with average particle size 10.28±1.58 μm, meanwhile electrochemically-synthesized possess a defect octahedral geometry with average particle size  4.5±1.6 μm. Thermal analysis showed that HKUST-1 is stable up to 300 °C. Catalytic test in esterification reaction of palmitic acid with ethanol in the presence of HKUST-1 as catalyst (0.6% wt) showed an enhanced product conversion with highest conversion was achieved in the presence of electrosyntehsized HKUST-1 (up to 43.3%).

Keywords

electrochemical; esterification; HKUST-1; catalytic; solvothermal.

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References

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DOI: https://doi.org/10.20961/alchemy.19.1.62466.1-13

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