Indarung Clay as Ca2+ and Cu2+ Catalyst Support; Synthesis, Characterization, and Catalytic Activity in the manufacture of methyl esters

Aju, Deska (2020) Indarung Clay as Ca2+ and Cu2+ Catalyst Support; Synthesis, Characterization, and Catalytic Activity in the manufacture of methyl esters. Masters thesis, UNIVERSITAS ANDALAS.

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Abstract

The utilization method clay from Indarung Padang enriched by cation Ca2+ and Cu2+ in the transesterification reaction of Crude Palm Oil (CPO) to obtain methyl esters are reported. Some Indarung clay were heated at 110°C coded by the h-Clay while the rest is calcinated at 700ºC called the c/h-Clay. All of those were analyzed by X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Fourier Transform Infra-Red (FTIR), and Surface Area Analyzer (SAA-BET). The composition analysis by XRF showed that there is no significant difference in Si/Al ratio between h-clay and c/h-clay. The diffractogram image measured by XRD shows the dominant crystal structure of h-clay and c/h-clay is quartz, which is their type of bond is strengthened by FTIR analysis. Uniquely the results of measurements with SAA show that the transformation of h-clay becoming c/h-clay reduces the specific surface area almost doubled. Heterogeneous catalysts were prepared through employing each nitrate solution of Ca2+ and Cu2+ mixed with h-Clay and stirred for 24 hours at a speed of 500 rpm under room temperature and atmospheric pressure. Other h-clay samples were mixed with the nitrate solutions of Ca2+ and Cu2+ ions at 70ºC. The results of measurements with AAS prove that h-clay absorbs Cu2+ ions greater than its ability to absorb Ca2+ ions. Meanwhile, It is higher five times against Cu2+ if it is undergoing at higher temperatures. The results of the combination of Ca2+ with h-Clay coded Ca/h-clay, and Cu2+ with h-clay coded Cu/h-Clay. XRD analysis of Ca/h-clay and Cu/h-clay proves the loading process of both cations type employing on clay does not affect the integrity of the clay crystal structure. The catalytic activity test on the CPO transesterification reaction to form methyl esters, the heterogeneous catalysts of Ca/h-clay and Cu/h-clay were compared to the nitrate solutions of Ca2+ and Cu2+ as a homogeneous catalyst. Under the same reaction conditions (65°C, 4 h of reaction time, and 750 rpm of stirring speed), the mole ratio of CPO/methanol is 1:6, and the mole ratio of the methanol/catalyst is 1:10. It's reaction conditions shows that the heterogeneous catalyst of both is better than the homogeneous catalyst (nitrate solution of Ca2+ and Cu2+ and from h-clay itself based on the yield of produced methyl ester. The highest yields of methyl esters were Cu/h-clay(56%), Cu(NO3)2(48%), Ca/h-clay(45%), h-clay(31%), and Ca(NO3)2 (31%)

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