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Effective Synthesis of n-butyl Salicylate Over Wash Coated Cordierite

Honeycomb by Zirconia And Its Mixed Oxides: A Kinetic Study


ABSTRACT
Cordierite honeycombs were coated with solid acid catalysts such as ZrO2
(Z), Mo(VI)/ZrO2 (MZ) and Pt-SO42-/ZrO2 (PSZ) were prepared and
characterized for their physico-chemical properties. These catalytic materials were
characterized for their total surface acidity, crystallinity, functionality, elemental
analysis and morphology by using techniques such as NH3 -TPD, PXRD, FTIR,
ICP-OES, SEM and TEM respectively. These honeycomb catalysts were used for
the liquid phase transesterification reaction of methyl salicylate (MS) with n-
butanol (n-BA). Optimization of reaction conditions such as reaction temperature,
reaction time, amount of catalysts and molar ratio of the reactants were carried out
to obtain maximum yield of transester (n-butyl salicylate). n-butyl salicylate is
obtained as major product and di-butyl ether is obtained as minor product. Highest
total transester 70 % obtained by MZ and 80 % n-butyl salicylate and 10 %
selectivity of di-butyl ether obtained in the presence of 0.4 g of honeycomb coated
catalysts at a molar ratio of MS: n-BA 2:1, reaction temperature 403 K and
reaction time 4 h. The energy of activation (16.81 and 14.92 kJ mol-1) and
temperature coefficient (1.36 and 1.12) values of the MZ and PSZ were obtained
from the kinetic studies. Pre-adsorption studies showed that the transesterification
reaction methyl salicylate with n-butyl alcohol over honeycomb catalysts follows
Langmuir-Hinshelwood mechanism. A reaction mechanism for transesterification
is proposed based on the kinetic data. Reactivation and reusability studies of the
honeycomb coated as well as powder form of catalysts up to 6 reaction cycles
were also studied.

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Sintesis Efektif n-butyl Salicylate Over Wash Coated Cordierite Honeycomb
oleh Zirconia Dan Oksida Campurannya: Studi Kinetik

ABSTRAK
Sarang lebah Cordierite dilapisi dengan katalis asam padat seperti ZrO2
(Z), Mo (VI) / ZrO2 (MZ) dan Pt-SO42- / ZrO2 (PSZ) disiapkan dan
dikarakterisasi untuk sifat fisiko-kimianya. Bahan katalitik ini dikarakterisasi
untuk keasaman permukaan total, kristalinitas, fungsionalitas, analisis unsur dan
morfologi dengan menggunakan teknik seperti NH3 -TPD, PXRD, FTIR, ICP-
OES, SEM dan TEM masing-masing. Katalis sarang lebah ini digunakan untuk
reaksi transestifikasi fasa cair metil salisilat (MS) dengan n-butanol (n-BA).
Optimalisasi kondisi reaksi seperti suhu reaksi, waktu reaksi, jumlah katalis dan
rasio molar reaktan dilakukan untuk mendapatkan hasil maksimum dari transester
(n-butil salisilat). n-butil salisilat diperoleh sebagai produk utama dan di-butil eter
diperoleh sebagai produk minor. Total transester tertinggi 70% diperoleh oleh MZ
dan 80% n-butil salisilat dan 10% selektivitas di-butil eter yang diperoleh dengan
adanya 0,4 g katalis berlapis sarang lebah dengan rasio molar MS: n-BA 2: 1,
reaksi suhu 403 K dan waktu reaksi 4 jam. Energi aktivasi (16,81 dan 14,92 kJ
mol-1) dan koefisien suhu (1,36 dan 1,12) nilai MZ dan PSZ diperoleh dari studi
kinetik. Studi pra-adsorpsi menunjukkan bahwa reaksi transesterifikasi metil
salisilat dengan n-butil alkohol pada katalis honeycomb mengikuti mekanisme
Langmuir-Hinshelwood. Mekanisme reaksi untuk transesteri fi kasi diusulkan
berdasarkan pada data kinetik. Studi reaktivasi dan reusabilitas dari dilapisi sarang
lebah serta bentuk bubuk katalis hingga 6 siklus reaksi juga dipelajari.