Malaysian Journal of Analytical Sciences Vol 23 No 1 (2019): 45 - 51

PRODUCTION OF ETHYL LEVULINATE VIA ESTERIFICATION REACTION OF LEVULINIC ACID IN THE PRESENCE OF ZrO₂ BASED CATALYST

(Penghasilan Etil Levulinat Melalui Pengesteran Asid Levulinik dengan Kehadiran Mangkin Berasaskan ZrO₂)

Dorairaaj Sivasubramaniam¹, Nor Aishah Saidina Amin¹*, Khairuddin Ahmad¹, Nur Aainaa Syahirah Ramli²

¹Chemical Reaction Engineering Group (CREG), Faculty of Chemical Engineering,

Universiti Teknologi Malaysia, 81300 Skudai, Johor, Malaysia

²Advanced Oleochemical Technology Division,

Malaysian Palm Oil Board (MPOB), 6, Persiaran Institusi, Bandar Baru Bangi, 43000 Kajang, Selangor, Malaysia

*Corresponding author: noraishah@cheme.utm.my

Received: 13 April 2017; Accepted: 17 April 2018

Abstract

Ethyl levulinate is widely used as a fuel additive, flavor or fragrance and as a component of fuel blending. This study focused on the production of ethyl levulinate from levulinic acid via esterification reaction in the presence of HPW/ZrO₂.The catalyst was prepared using the wet impregnation method, characterized by using FTIR, BET and NH₃-TPD and screened based on 20%, 40% and 60% HPW/ZrO₂. The 40% HPW/ZrO₂ catalyst exhibited the highest catalytic performance during the parameter screening stage which included catalyst loading (0.25‒1.25g) and volume ratio of levulinic acid to ethanol (1:4 – 1:8). The highest ethyl levulinate yield of 99% corresponded to a catalyst loading of 0.5 g and volume ratio of levulinic acid to ethanol of 1:5 with reaction conditions at 150 °C for 3 hours. The esterification reaction of levulinic acid revealed that the catalytic performance was influenced by the acid sites and surface area of the catalyst. In addition, volume ratio was also a major factor in enhancing the ethyl levulinate yield.

Keywords: levulinic acid, ethyl levulinate, wet impregnation, esterification, phosphotungstic acid

Abstrak

Etil levulinat digunakan secara meluas sebagai komponen penting dalam bahan kosmetik, bahan tambahan dalam bahan api dan campuran bahan api. Kajian ini memberi tumpuan dengan penghasilan etil levulinat daripada asid levulinik melalui tindak balas pengesteran dengan kehadiran pemangkin HPW/ZrO₂. Pemangkin ini disediakan dengan menggunakan kaedah impregnasi basah dan dicirikan dengan menggunakan FTIR, BET dan NH₃-TPD, pemangkin ini ditapis berdasarkan 20%, 40%,dan 60% HPW/ZrO₂. Akhirnya, didapati 40% HPW/ZrO₂ menunjukkan mangkinan tinggi yang sesuai digunakan untuk pemeriksaan parameter melibatkan berat pemangkin (0.25‒1.25g) dan nisbah isipadu LA kepada etanol (1:4 ‒ 1:8). Penghasilan terbaik ditunjukkan dengan muatan pemangkin (0.5 g) dan nisbah isipadu asid levulinik kepada etanol (1:5) yang diperolehi hasil 99% EL pada 150 °C selama 3 jam. Penggunaan HPW/ZrO₂ sebagai pemangkin dalam tindak balas pengesteran LA mendedahkan bahawa reaktiviti pemangkin sangat dipengaruhi oleh bahagian asid dan luas permukaan pemangkin tersebut.

Kata kunci: asid levulinik, etil levulinate, impregnasi basah, pengesteran, asid fosfotungstik

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