Synthesis and Characterization of Acetonitrile Ligated Cu(II)-Complex and Its Catalytic Application for Transesterification of Frying Oil in Heterogeneous Phase | Pratikha | Indonesian Journal of Chemistry 21329 40415 1 PB
72
Indo. J. Chem., 2013, 13 (1), 72 - 76
SYNTHESIS AND CHARACTERIZATION OF ACETONITRILE LIGATED Cu(II)-COMPLEX
AND ITS CATALYTIC APPLICATION FOR TRANSESTERIFICATION OF FRYING OIL
IN HETEROGENEOUS PHASE
Rycce Sylviana Pratikha, Syukri*, and Admi
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Andalas University, Kampus Unand Limau Manis
Padang, 25163
Received October 5, 2012; Accepted December 17, 2012
§
ABSTRACT
§
Catalysts have played an important role in many industries because they allow the reaction occurs faster. The
aim of this work were to synthesize and characterize a Cu(II)-acetonitrile complex immobilized on modified silica and
to investigate its catalytic activity at optimal condition (catalyst concentration, stirring rate, and the duration of
reaction) in transesterification of frying oil. Fourier Transform Infrared (FTIR) and Nano Laser-Particle Size Analyzer
(NL-PSA) were used to characterized the catalyst obtained, metal loading and leaching of the copper content was
measured by Atomic Absorption Spectroscopy (AAS) and the formation of product from transesterification reaction
was analyzed by Gas Chromatography-Mass Spectroscopy (GC-MS). FTIR spectra reveal a successful synthesis of
modified silica and the immobilized Cu(II)-acetonitrile complex on it. NL-PSA Analysis showed that the catalyst
possesed smaller particle size than the parent silica. Analysis with AAS confirms the stable catalysts formed
because metal loading and leaching value were of 6.19 and 0.16%, respectively. The optimum conditions were
found to be 0.80% catalyst concentration, 300 rpm stirring rate and 10 h duration of reaction
§
Keywords§modified silica; immobilization; transesterification; methyl ester; Cu(II)-acetonitrile§
ABSTRAK
§
Katalis memainkan peranan penting dalam dunia industri karena memungkinkan reaksi berlansung lebih cepat.
Pada penelitian ini telah dilakukan sintesis dan karakterisasi kompleks Cu(II)-acetonitril yang diamobilisasi pada
silika modifikasi dan penentuan aktivitas katalitik dari katalis yang dihasilkan pada keadaaan optimum yaitu
konsentrasi katalis, kecepatan pengadukan, dan lama pengadukan. FTIR dan Nano Laser-Particle Size Analyzer
(NL-PSA) digunakan untuk mengkarakterisasi katalis yang dihasilkan; metal loading dan leaching kandungan
tembaga diukur dengan AAS; dan pembentukan metil ester dari reaksi transesterifikasi dianalisis dengan GC-MS.
Spektra FTIR menunjukan bahwa silika modifikasi dan katalis teramobilisasi sukses terbentuk. Analisis NL-PSA
menunujukan bahwa ukuran partikel dari katalis lebih kecil dibandingkan silika induk dan silika modifikasi. Analisis
dengan AAS memberikan informasi bahwa katalis yang terbentuk cukup stabil karena nilai metal loading dan
leaching adalah of 6,19 dan 0,16%. Kondisi optimum dari reaksi transestrifikasi ditemukan pada konsentrasi katalis
0,80%, kecepatan pengadukan 300 rpm dan dengan lama pengadukan 10 jam.
§
Kata Kunci§modifikasi silika; amobilisasi; transesterifikasi; metil ester; Cu(II)-asetonitril§
§
INTRODUCTION
릤䀸릤§ 䨸§ 릤䀸§ 산릤§ 산䘐산䬬§ 䨸릤§ § 릤ꮠ§ 䘐릤§
산산䀸ꮠ§산ꮠꮠꮠ릤䬬§Ὠ㮴§
苨ꮠꮠ䀸§ 䬬릤릤ꮠꮠ䀸§ 䬬산ꮠꮠ䀸§ 䀸ꮠ릤 䬬§ 산
§ 릤산䬬䀸§ §
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§ 릤
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ꮠ ꮠ䨸§§䬬릤산산릤§ 牨§ 䨸§ퟰઈ㮴§鯈
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䀸산 牨§
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Indo. J. Chem., 2013, 13 (1), 72 - 76
苨ꮠꮠ䀸§ § 릤릤갬릤
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Optimalization of the immobilized Cu(II) catalyst on
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§ퟰ§牨ꮠ
§§ §牐§ §산
§ퟰ§
§
RESULT AND DISCUSSION§
§
FTIR Analysis of the Catalyst§
§
ꮠ갬§ ퟰ§ 䬬 䘐릤 § 릤§
§ 䬬릤산§ § 산릤
§ 䬬ꮠꮠ산§
牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 산
䀸 䨸䬬§ 릤§ 䬬䨸 산릤§ 산
§
산산䀸䬬§ 산ꮠ
릤 § ⟴ꮠꮠ산§ 갬릤§ 산䬬§ 䬬릤ꮠ ꮠ§ 산 䬬ꮠ
§ 산§
ઈퟰ
왌Ὠ§ 牨 § 䘐 ꮠ § 䘐산䬬§ 산䬬䬬ꮠ갬
릤 § § 鯈ઈ§ 䬬릤 ꮠ
갬§ §
䬬ꮠꮠ산§䬬䨸 산릤§ퟰ㮴§산䬬릤 §
§ ꮠ䬬§ 산§ 릤§䬬ꮠꮠ산§䬬䬬릤䬬§
§ §§⟴ꮠઈ鯈§§
ꮠ
갬§§ 䬬ꮠ산
§갬䨸䬬§§산
§§ 䀸 䀸§§
74
Indo. J. Chem., 2013, 13 (1), 72 - 76
§
Fig 1.
§䬬릤산§ 산§산릤
§䬬ꮠꮠ산§ §牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§
§산
䀸 䨸䬬§릤§䬬䨸 산릤§산
§ §산산䀸䬬§산ꮠ
릤 §
§
§
Fig 2. ꮠ䬬ꮠ䨸ꮠ
§ 산
§ 산ꮠ릤§ 䬬ꮠ 릤§ § 산릤
§ 䬬ꮠꮠ산§ 갬릤§
牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§산
§산산䀸䬬§산ꮠ
릤 §
§
갬䨸䬬§ 牨§ 산 䬬릤 §䘐산릤§ퟰὨ㮴§
릤§䬬릤
䬬§산
§ 산§
ퟰ牐§ 牨 ઈퟰ§ 䘐산䬬§ 산䬬䬬ꮠ갬
릤 § § 䬬ꮠ 산
릤§ 갬䨸䬬§ ⟴ꮠઈ鯈ઈ⟴ꮠ§
ઈퟰ
ઈퟰ
苨 ꮠꮠ
산§산
䬬§산릤산§산§牐§牨 §산
§Ὠ牐§牨 § 䨸릤§§
릤ꮠ§ 릤 牨산ꮠ
§ §⟴ꮠઈ鯈§
ꮠ
갬§ 牨§⟴ꮠ鯈§
산
§ § 牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 산릤산릤 § 䘐ꮠ § 䘐릤산§
ઈퟰ
ꮠ
릤
䬬ꮠ䀸§산§牐§牨 §§ꮠ
ꮠ산릤 § 릤§산릤산산
릤§ §⟴ꮠઈ鯈§
䘐ꮠ § 牨릤산䬬§
ꮠ
갬§ ⟴ꮠઈ鯈ઈ苨§ 산
§ 산§ Ὠ§ 牨 ઈퟰ§ 䘐산䬬§
산䬬䬬ꮠ갬
릤 §§ઈઈ§䘐산갬갬ꮠ
갬§ §산
ꮠꮠ
ꮠ䨸牨§산ꮠ
§산
䬬§ §
산산䀸䬬䬬§ 산ꮠ
릤 § 산릤산§ 산§ 왌왌§ 牨 ઈퟰ§ 䨸 § 릤§
산䬬䬬ꮠ갬
릤 §§
ꮠꮠ릤§ ≡§ 갬䨸§ꮠ산ꮠ
䬬§ § 릤§갬산 릤 §
牨䨸
䬬§
릤§ υ § ꮠ산ꮠ
§ § 릤릤§ 왌§ 䘐䨸 §
릤§ 릤 릤릤 § 산§ 뀨왌§ 산
§ 牐왌§ 牨 ઈퟰ§ ퟰઈ㮴§
§ 산산䀸䬬§
ઈퟰ
ઈퟰ§
䬬릤산§ ꮠ䬬산릤산산
릤§ § 산
䬬§ 산§ Ὠ§ 牨 § ퟰퟰ§ 牨
鮼§
ઈퟰ§
산
§ ퟰ牐§ 牨 牨 §뀨왌 ꮠ
§ 䨸 릤牨릤§ 산
䬬§
ꮠ
릤
䬬ꮠ䀸§산§Ὠ牐§牨ઈퟰ§ 牨§⟴ꮠઈ鯈§릤
ꮠ
갬§ꮠ
§䬬䨸 §산산䀸䬬§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
䘐릤산릤§ 산
§ 릤§
릤§ ꮠ
§ 산릤
§ 䬬ꮠꮠ산§ 산䨸䬬릤 § 䀸§
ꮠ
릤산ꮠ
§ 릤䘐릤릤
§ 䬬ꮠ산
§ 갬䨸䬬§ 䘐ꮠ § 䨸 § 牨릤산§
릤
릤§
릤§ 산산ꮠ산ꮠꮠ䀸§ § 䬬 ꮠ 릤 § § 䬬릤 ꮠ
갬§
ꮠ산ꮠ
§산䬬§䨸 §릤§ 산갬䨸릤 § 산䬬§산§䬬䨸릤䬬䬬 䨸§ 갬산 릤 §
§䨸 §산릤
ꮠꮠ릤§牨릤 §
§ 릤§牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§ퟰ㮴§
§
NL-PSA Analysis§
§
ઈ⟴苨§ 갬산릤§ ꮠ
牨산ꮠ
§ 산䨸§ 䬬ꮠ 릤§ 산
§
ꮠ䬬ꮠ䨸ꮠ
§ § 산ꮠ릤§ § 산
§ 릤§ 䬬릤릤
§ 牨§ ꮠ갬§ § 산§
산 릤
ꮠ
갬§ § 산릤
§ 䬬ꮠꮠ산§ ꮠ䬬ꮠ䨸ꮠ
§ ꮠ
§ ퟰ뀨ઈ§ �牨§
산
갬릤§ 䘐ꮠ § 牨ꮠ
산릤 § 䀸§ ퟰ§ �牨§ 산ꮠ릤§ 䬬ꮠ 릤§ 苨§
산 릤
ꮠ
갬§ ꮠ䬬ꮠ䨸ꮠ
§ § ꮠ䬬§ 牨산릤ꮠ산§ ꮠ
ꮠ산릤 § 산§
릤§䬬ꮠꮠ산§䘐산䬬§산牨 䨸䬬§§
સ ꮠ ꮠ릤 §䬬ꮠꮠ산§ 산䬬§
산䘐§ ꮠ䬬ꮠ䨸ꮠ
§산
§䬬牨산릤§
산ꮠ릤§䬬ꮠ 릤§ 산
§ꮠ䬬§산릤
§䬬ꮠꮠ산§䘐 ꮠ §䬬릤릤牨ꮠ
갬䀸§산䬬§산§
䬬릤ɬ䨸릤
릤§ § 릤§ ꮠ
릤산ꮠ
§ 릤䘐릤릤
§ 苨왌§ 산䬬§
牨 ꮠ ꮠ릤§ 䘐ꮠ § 䬬ꮠꮠ산§ 䬬䨸 산릤§ 릤
§ 갬산 릤 § 䨸 §
牨릤 §
§ 牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 릤§ 산ꮠ릤§ 䬬ꮠ 릤§ 산
§
ꮠ䬬ꮠ䨸ꮠ
§䬬ꮠ갬 䀸§ 릤릤산䬬릤 § 산§산
§릤§ 산산릤§ §
ꮠ䬬§산산䀸ꮠ§산ꮠꮠ䀸§ 䨸릤§§산갬릤§䬬릤ꮠ ꮠ§䬬䨸 산릤§산릤산§
§
Atomic Absorption Spectroscopy (AAS)§
§
苨苨⟴§ 산
산䀸䬬ꮠ䬬§ ꮠ 릤 § 릤§ 산牨䨸
§ § 牨릤산§
산 ꮠ
갬§ 산
§ 牨릤산§ 릤산 ꮠ
갬§ 산릤§ § 䘐산䬬§ 䨸
§ 산§ 릤§
牨릤산§ 산 ꮠ
갬§ § 䨸§ ꮠ
§ 릤§ 산산䀸䬬§ 䘐릤릤§ ퟰ牐Ⳉ§ 䀸§
牨산䬬䬬§산
§
䀸§䨸
릤갬릤䬬§ퟰⳈ§䬬䬬§ꮠ
§ 릤§䬬릤
§
산 릤§§ §릤산 ꮠ
갬§릤䬬§
ꮠ䬬§䬬牨산§산䨸릤§ꮠ
ꮠ산릤 § 산§
릤§ 䨸 § 牨릤산§ 릤
릤§ 䘐산䬬§ 䬬
갬䀸§ 䨸
릤 §
§ 릤§
牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§ 䨸갬 §릤릤䬬산ꮠ§ꮠ
릤산ꮠ
§
§
Catalytic Application at Optimal Conditions§
§
Catalyst concentrations
릤§ 䨸§ § 산산䀸䬬§
릤
산ꮠ
§ 䘐산䬬§
산
산䀸 릤 § 䀸§ ઈસ⟴§
§ ꮠ갬§ 왌§ 䀸§ 산 ꮠ
갬§ ퟰ뀨Ⳉ§
산산䀸䬬§ ꮠ
§ 릤§ 牨ꮠ 䨸릤§ § 牨릤 산
§ 산
§ 䀸ꮠ
갬§ ꮠ§ 릤§
䀸ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ 릤릤 §ꮠ
릤산䬬릤䬬§䨸
ꮠ§ 산䨸§ §
Ⳉ§ 䘐 ꮠ §
산ꮠ
§ Ὠ牐Ⳉ§ 䨸§
릤§ 䨸§
산ꮠ
릤 § 䘐릤릤§ 牨릤 䀸§ 릤䬬릤§ 䘐 ꮠ § 䨸
§ 왌ퟰⳈ§牨릤 䀸§
산牨ꮠ산릤§ 산§ ퟰퟰ牐§ 牨ꮠ
§ 릤릤
ꮠ
§ ꮠ牨릤§ 산
§ 왌牐Ⳉ§
牨릤 䀸§ 릤산릤§ 산§ ퟰ§ 牨ꮠ
§ 릤릤
ꮠ
§ ꮠ牨릤§ 苨§ ꮠ䬬§
ꮠ
§ ꮠ갬 릤§ § 䀸ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ 䨸릤§ § 릤§ 牨䬬§
䨸산릤 § 牨산ꮠ
§ § 牨릤 ꮠ 릤§ 산
ꮠ
§ 䘐 ꮠ § ꮠ䬬§ 릤䀸§
ꮠ牨산
§ § ꮠ
ꮠꮠ산릤§ 릤§ 산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ § 䀸ꮠ
갬§ ꮠ§
산ꮠ
ꮠ
갬§ ꮠ갬䀸릤ꮠ 릤§ 산§ 산§ ꮠ
§ 䘐ꮠ§ 산䬬§ 릤§
산䬬䬬䨸牨릤 § 산䬬§ 산§ 릤䀸§ 산§ ퟰ왌㮴§
릤산䬬릤 § § 산산䀸䬬§
릤
산ꮠ
§ 牨산릤§ 䀸ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ 산ꮠ
릤 §
산牨산ꮠ산䀸§䬬릤§ 䘐
§§산牨䬬§ 릤§
§
Stirring rate
�ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ ꮠ
§ 䬬ꮠꮠ
갬§ 산릤§산ꮠ산ꮠ
䬬§산䬬§
릤ꮠ릤 §ꮠ
§ ꮠ갬§§
릤§䀸ꮠ릤 §산牨䨸
§ §牨릤 䀸§ 릤䬬릤§산§
왌§牨§§ꮠ䬬§§ 릤§§릤䬬§§
ꮠꮠ
§§ 䨸릤§§§§ ꮠ갬 릤§ 䨸§§
Indo. J. Chem., 2013, 13 (1), 72 - 76
§
Fig 3. 산산䀸䬬§
릤
산ꮠ
§ 䬬§ 산䀸§ 牨릤 䀸§ 릤䬬릤§
산ꮠ
릤 §ꮠ
§ ꮠ䬬§䘐§
§
§
Fig 5. 䨸릤§ 牨릤 䀸§ 릤䬬릤§ 䨸§ 산§ 牨§ 릤산ꮠ
§
ꮠ牨릤䬬§산ꮠ산ꮠ
䬬§
§
산ꮠ
릤 §苨§ 왌§牨§ 䘐산䬬§ 䨸
§뀨Ⳉ§ § 䨸§ 산§
산ꮠ
§ 뀨ퟰⳈ§ § 牨릤 䀸§ 산牨ꮠ산릤§ ퟰ왌뀨Ⳉ§ 牨릤 䀸§
릤산릤§ 산
§ 왌Ⳉ§ 牨릤 䀸§ 䬬릤산산릤§ 산§ ퟰퟰ§ 牨ꮠ
§
릤릤
ꮠ
§ꮠ牨릤§
ꮠ䬬§ 릤
牨릤
§산
§릤§산갬䨸릤 § 산§산§
ꮠ䬬§ 산릤§ 릤§ 산 䬬ꮠ
ઈ 릤䬬ꮠ
§ § 䬬䨸䬬산릤䬬§
§
산산䀸䬬§ 䬬䨸 산릤§ 릤산 릤䬬§ ꮠ䬬§ 릤ɬ䨸ꮠꮠꮠ䨸牨§ 산§ 산䘐䬬§ 릤§
산산䀸䬬§§䘐§ꮠ牨산䀸§
§
The duration of the reaction
苨䬬§산
§릤§䬬릤릤 §ꮠ
§ ꮠ갬§뀨§ 릤§
갬릤§ § 䨸산ꮠ
§
§ 릤산ꮠ
§䘐산䬬§䨸
§ꮠ
§ ꮠ갬 릤§ 䨸§산ꮠ
릤 §
§ ꮠ䬬§
산릤§ 릤§
갬릤§ § 䨸산ꮠ
§ꮠ牨릤§ § 릤산ꮠ
§䘐릤릤§§ 牐§
산
§ ퟰ§ § § 䘐산䬬§ 䨸
릤 § 牐牐§ 뀨§ 산
§ 뀨ퟰⳈ§ §
䨸§
ꮠ䬬§ 산§ 䬬 䘐릤 § 산§ 䬬ꮠ갬
ꮠ ꮠ산
§ 릤 릤§ § 릤§
䨸산ꮠ
§ § 산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ 릤산ꮠ
§ § 산䘐§ 牨릤§
䬬䨸䬬산릤§§ꮠ
릤산§䘐ꮠ § 릤§䬬䨸 산릤§ §䬬䨸 §ꮠ牨牨ꮠꮠ 릤 §
䨸§산산䀸䬬§
§
CONCLUSION
§
牨牨ꮠꮠ 산ꮠ
§ § 䨸 ઈ산릤
ꮠꮠ릤§ 牨릤 §
§
牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§산
§릤§릤 牨릤 §산
§牨ꮠ䬬ꮠ
갬䀸§산
§릤§
산ꮠ릤 § ꮠ
§ 산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ § 䀸ꮠ
갬§ ꮠ§
릤§ 산산䀸䬬§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
75
§
Fig 4. ⟴ꮠꮠ
갬§ 릤ꮠ䀸§ 갬ꮠ릤䬬§ 䬬ꮠ갬
ꮠ ꮠ산
§ ꮠ牨산§
§
산산䀸ꮠ§산ꮠꮠ䀸§ § 릤§산산䀸䬬§䨸䬬릤 §ꮠ
§ ꮠ䬬§릤산ꮠ
§
䬬 䘐䬬§ ꮠ䬬§ ꮠ牨산§
ꮠꮠ
䬬§ 산§ Ⳉ§ 산산䀸䬬§
릤
산ꮠ
§ 산
§ 왌§ 牨§ 䬬ꮠꮠ
갬§ 산릤§ 䘐릤릤§ ꮠ䬬§
릤릤
릤
릤§
§ 릤§ 䨸산ꮠ
§ § 릤산ꮠ
§ꮠ牨릤§䬬ꮠ§ §릤§
䬬릤§ꮠ
§ 릤§
릤 §릤䬬릤산 §
§
ACKNOWLEDGEMENT§
§
릤§ 䘐䨸 § ꮠ릤§ 산
䬬§ § સ산릤ꮠ산§ 릤牨ꮠ䬬䀸§
산산䀸§䬬산 § § 릤ꮠ§ 릤§ꮠ
§ 릤§
§산
§ઈ⟴苨§
牨릤산䬬䨸릤牨릤
§
릤
§ 䨸§ 산
䬬§ 갬§ § 릤
산§ 쀔
산
§
산산䀸§ 산
§ 苨﵌魤⟴§ 산 산
갬§ 산산䀸§ § 릤ꮠ§
릤§ꮠ
§苨苨⟴§산
§ઈસ⟴§牨릤산䬬䨸릤牨릤
§릤䬬릤ꮠ릤䀸§
§
REFERENCES
§
ퟰ§ ⟴䀸䨸ꮠ§⟴§ꮠ산 ꮠ§苨⟴§﵌산 ꮠ릤§苨§苨ઈ牨산ꮠ 릤릤
§
苨§ 산
§ §
﵌魤§ Ὠ§ Inorg. Chim. Acta§ §
왌§ퟰ§ퟰ牐Ὠ§
§ ⟴䀸䨸ꮠ§ ⟴§ ꮠ䬬 릤§ 魤§苨ઈ牨산ꮠ 릤릤
§苨§ ꮠ§�§
릤
갬§ �§ 산
§ §
﵌魤§ § Microporous
Mesoporous Mater.§ퟰퟰ왌§ퟰઈ왌§ퟰὨퟰퟰὨ§
왌§ ⟴산 ꮠ릤§ 苨§ ꮠ산 ꮠ§ 苨 §﵌산
ꮠ§ સ§ ꮠ산
갬§
苨⟴
§산
§ §
﵌魤§뀨§ Appl. Catal., A§牐§
§ퟰퟰퟰὨ§
§ ⟴산 ꮠ릤§苨§⟴䀸䨸ꮠ§⟴§ꮠ산 ꮠ§苨§§﵌산
§§ §
﵌
魤§§Catal. Lett§ퟰퟰퟰ§ퟰઈ§왌牐§
뀨§ 산§⟴§산§�§䨸§§산
§릤릤§ �§§
Mater. Today§牐§왌§왌왌
§ 산
§ ⟴§ 왌§ Jurnal Ilmu Dasar§ § §
ὨὨ
Ὠ§ ꮠ릤§ સ§ 산§ § 산
§ સ산ɬ䨸산ꮠ릤§ §
§J. Chem. Soc., Dalton Trans.§§ퟰퟰઈퟰퟰ
§
릤䀸§
§산
§⟴산§
§§J. Am. Chem.
Soc.§ퟰ왌§ퟰ§牐뀨牐뀨왌
牐§ 䬬ꮠ갬牨
§苨§갬§§﵌산
§ 릤ꮠ䬬 § §왌§J.
Catal.§ퟰ왌§ퟰ§ퟰ왌ퟰ
ퟰ§ 릤䨸䬬 牨산
§ 鯈§
﵌ꮠ
갬릤§ 鯈§ ﵌ 릤 § §﵌
산
§
䨸릤§
§牐§ Heterogeneous Catalysis and
Solid Catalyst§ꮠ릤䀸ઈ§릤산갬§릤牨산
76
Indo. J. Chem., 2013, 13 (1), 72 - 76
ퟰퟰ§ 산 牨산
§
§ 산
§ 䨸릤
ꮠ§ §﵌牐§ Iran. Polym.
J.§ퟰ§왌§ퟰ牐ퟰ
ퟰ§ ⟴ ꮠ산
산§ ⟴§ 산
§
산산§ § 뀨§ J. Sci.
Ind. Res.§§牐뀨왌
ퟰ왌§ 산䬬 ꮠ § 쀔§ 산
§苨
䘐산§ § § Energy Fuels§ §
ퟰ왌ઈퟰ왌ퟰ§
ퟰ§ 산 牨산
ꮠ
갬䬬ꮠ §苨
§
ꮠ䬬䨸
산䀸산
ꮠ§§산
§
산 ꮠ§§
§Indo. J. Chem§§왌§Ὠ§
ퟰ뀨§ 쀔산牨ꮠ§
⟴§ 苨ꮠ산
ꮠ§ § 산
§ 䨸 산䬬牨산
§ §
﵌ꮠ
릤ꮠ산§ 릤산䬬ꮠ§
산
䬬릤䬬릤ꮠ ꮠ산䬬ꮠ§ 鯈§ 릤 산 산§
䨸§સ릤ꮠ§산牨ꮠ산§ 산산牨§ 릤산
䨸牨산§Proc.
§
§
§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
Nat. Conf. Fundam. Appl. Technol.§
䬬ꮠ䨸§
릤
갬ꮠ§⟴릤䨸䨸 §릤牨릤§ퟰ뀨§릤牨릤§Ὠ
ퟰ§ ⟴䨸산§ § §
산릤 § ⟴릤䬬䀸:
Fundamentals and Applications§
§ ꮠ릤䀸§ §
⟴
䬬§ §§§
ퟰὨ§ 산
ꮠ산
갬산
§ ⟴ §﵌䨸산§ § ꮠ䀸산
ꮠ§ સ§
ꮠ ꮠ산§⟴§苨
갬갬산ꮠ
ꮠ§§苨ꮠ릤 §⟴§산
§산牨산䨸
§
§ ﵌산산릤ꮠ䬬ꮠ§ ﵌릤산䬬산牨산
§ ﵌산산ꮠ䬬§ 릤산䬬ꮠ䬬§ 䬬ꮠꮠ산§
䬬릤산牨§ 산 ꮠ§ 䀸산
갬§ ꮠ릤릤 § 릤
갬산
§ 릤
ꮠ§ 䬬§ 갬릤§
Proc. Nat. Conf. Sci. Technol II, 산牨䨸
갬§
쀔
ꮠ릤䬬ꮠ䀸§ퟰὨઈퟰ§릤牨릤§§
§
Indo. J. Chem., 2013, 13 (1), 72 - 76
SYNTHESIS AND CHARACTERIZATION OF ACETONITRILE LIGATED Cu(II)-COMPLEX
AND ITS CATALYTIC APPLICATION FOR TRANSESTERIFICATION OF FRYING OIL
IN HETEROGENEOUS PHASE
Rycce Sylviana Pratikha, Syukri*, and Admi
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Andalas University, Kampus Unand Limau Manis
Padang, 25163
Received October 5, 2012; Accepted December 17, 2012
§
ABSTRACT
§
Catalysts have played an important role in many industries because they allow the reaction occurs faster. The
aim of this work were to synthesize and characterize a Cu(II)-acetonitrile complex immobilized on modified silica and
to investigate its catalytic activity at optimal condition (catalyst concentration, stirring rate, and the duration of
reaction) in transesterification of frying oil. Fourier Transform Infrared (FTIR) and Nano Laser-Particle Size Analyzer
(NL-PSA) were used to characterized the catalyst obtained, metal loading and leaching of the copper content was
measured by Atomic Absorption Spectroscopy (AAS) and the formation of product from transesterification reaction
was analyzed by Gas Chromatography-Mass Spectroscopy (GC-MS). FTIR spectra reveal a successful synthesis of
modified silica and the immobilized Cu(II)-acetonitrile complex on it. NL-PSA Analysis showed that the catalyst
possesed smaller particle size than the parent silica. Analysis with AAS confirms the stable catalysts formed
because metal loading and leaching value were of 6.19 and 0.16%, respectively. The optimum conditions were
found to be 0.80% catalyst concentration, 300 rpm stirring rate and 10 h duration of reaction
§
Keywords§modified silica; immobilization; transesterification; methyl ester; Cu(II)-acetonitrile§
ABSTRAK
§
Katalis memainkan peranan penting dalam dunia industri karena memungkinkan reaksi berlansung lebih cepat.
Pada penelitian ini telah dilakukan sintesis dan karakterisasi kompleks Cu(II)-acetonitril yang diamobilisasi pada
silika modifikasi dan penentuan aktivitas katalitik dari katalis yang dihasilkan pada keadaaan optimum yaitu
konsentrasi katalis, kecepatan pengadukan, dan lama pengadukan. FTIR dan Nano Laser-Particle Size Analyzer
(NL-PSA) digunakan untuk mengkarakterisasi katalis yang dihasilkan; metal loading dan leaching kandungan
tembaga diukur dengan AAS; dan pembentukan metil ester dari reaksi transesterifikasi dianalisis dengan GC-MS.
Spektra FTIR menunjukan bahwa silika modifikasi dan katalis teramobilisasi sukses terbentuk. Analisis NL-PSA
menunujukan bahwa ukuran partikel dari katalis lebih kecil dibandingkan silika induk dan silika modifikasi. Analisis
dengan AAS memberikan informasi bahwa katalis yang terbentuk cukup stabil karena nilai metal loading dan
leaching adalah of 6,19 dan 0,16%. Kondisi optimum dari reaksi transestrifikasi ditemukan pada konsentrasi katalis
0,80%, kecepatan pengadukan 300 rpm dan dengan lama pengadukan 10 jam.
§
Kata Kunci§modifikasi silika; amobilisasi; transesterifikasi; metil ester; Cu(II)-asetonitril§
§
INTRODUCTION
릤䀸릤§ 䨸§ 릤䀸§ 산릤§ 산䘐산䬬§ 䨸릤§ § 릤ꮠ§ 䘐릤§
산산䀸ꮠ§산ꮠꮠꮠ릤䬬§Ὠ㮴§
苨ꮠꮠ䀸§ 䬬릤릤ꮠꮠ䀸§ 䬬산ꮠꮠ䀸§ 䀸ꮠ릤 䬬§ 산
§ 릤산䬬䀸§ §
산산䀸䬬§ ꮠ䬬§ 산
§ ꮠ牨산
§ 䬬䨸䬬산
릤§ ꮠ
§ 䬬䀸
릤䬬ꮠ䬬§
릤갬릤
릤산ꮠ
§ 산릤§ ꮠ牨산
§ 산산牨릤릤䬬§ § 산산䀸䬬䬬§ §
릤䬬䬬§ 䘐 ꮠ § ꮠ䬬§ 䨸䬬릤 § § 산릤§ 릤§ 산릤§ § 릤산ꮠ
䬬 §
릤䬬ꮠ릤§ 산§ 갬 § 산
§ 䬬산릤§ 산산䀸䬬§ 㮴§
§ 牨ꮠ
릤§
산䬬릤 §
§ ꮠ§ 산䬬릤§ 릤릤§ 산릤§ 牨갬릤
릤䨸䬬§ 산
§
산 산
산갬릤䬬§ § § 산산䀸䬬䬬§ 牨ꮠ갬 § 릤§
릤§ 䀸§
릤릤갬릤
릤䨸䬬§ 산산䀸䬬䬬§
§ 牨산ꮠ䬬
§ 牨갬릤
릤䨸䬬§
릤릤갬릤
ꮠ 산ꮠ
§ § 牨갬릤
릤䨸䬬§ 산산䀸䬬䬬§ ꮠ
§
산산䀸䬬䬬§산릤§ 릤릤§ 산
§ 산§ § 릤§ 릤릤갬릤
릤䨸䬬§
릤§
䬬䨸§牨산릤ꮠ산§ퟰઈ㮴§⟴ꮠꮠ산§牨릤䬬䨸䬬§䬬ꮠꮠ산§ સસઈ
§ 릤
산
릤 § 릤산ꮠꮠ䀸§ 산
§ 䬬릤릤ꮠꮠ䀸§ 䨸§ 릤䀸§ 산릤§ 릤䀸§
ꮠ ꮠ䨸§§䬬릤산산릤§ 牨§ 䨸§ퟰઈ㮴§鯈
§ 릤§ 릤§䬬ꮠ 릤§ ퟰ§ સસઈ§ 산
§ ⟴苨ઈퟰ뀨§ 산릤§ 릤 산牨릤䬬§ § ꮠ
갬산
ꮠ§
䬬䨸䬬§䘐 ꮠ릤§䀸牨릤§§산䬬§갬산
ꮠ§䬬䨸§䘐 ꮠ §
릤릤갬릤
릤䨸䬬§산산䀸䬬䬬§산릤§牨릤§ 릤䬬ꮠ산릤§ꮠ
§ꮠ
䨸䬬ꮠ산§
산릤§䨸䬬릤 §§릤牨䀸릤§ § 산§䨸䬬릤§牐ઈퟰퟰ㮴§
릤䬬䬬§
릤䬬릤§ 산산䀸䬬䬬§ 산릤§ 릤산䬬䀸§ § 䬬릤산산릤§ 산
§
§릤䬬
ꮠ
갬§산䨸 §
릤 산 §§鮼ઈퟰ왌ὨὨ왌ퟰ§
魤牨산ꮠ§산 릤䬬䬬§§䬬䀸䨸ꮠ 산산산
䀸산 牨§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
73
Indo. J. Chem., 2013, 13 (1), 72 - 76
苨ꮠꮠ䀸§ § 릤릤갬릤
릤䨸䬬§ 산산䀸䬬§ 䘐산䬬§ 산 릤릤 §䀸§
산ꮠ릤§ 䬬ꮠ릤§ 䬬䨸 § 산䬬§ 牨릤산§ 牨릤산§ ꮠ 릤§ 산
§ 牨릤 §
牨䨸
䬬§ 牨릤 § 牨䨸
䬬§ 산䬬릤 §
§ 산
䬬ꮠꮠ
§
牨릤산䬬§ 䨸䬬릤 § § 릤§ 산산䀸䬬䬬§ ퟰ㮴§ ⟴䨸릤䬬䬬§ 䬬䀸
릤䬬ꮠ䬬§ §
산릤
ꮠꮠ릤§ꮠ갬산릤 §䨸 §牨릤 릤䬬§산
§산ꮠ릤 §ꮠ
§牨산
䀸§
릤산ꮠ
䬬§䬬䨸 §산䬬§䀸산
산ꮠ
§릤산ꮠ
䬬§릤 ꮠ
산ꮠ
§
릤산ꮠ
䬬§ ꮠ䬬䨸릤
릤§ 䀸牨릤ꮠ 산ꮠ
§ ꮠ
§ 牨갬릤
릤䨸䬬§
산
§ 릤릤갬릤
릤䨸䬬§ 산䬬릤§
쀔
ꮠ릤§ 릤릤 § 릤ꮠ䨸䬬䀸§ 㮴§ 䘐 릤릤§ 牨 ꮠ ꮠ릤 §
䬬䨸§ 䘐산䬬§ 릤산릤 § 䀸§ ꮠ
䨸ꮠ
갬§ 갬산
§ ꮠ
§
릤§䬬䨸 산릤§ § 䬬ꮠꮠ산§ꮠ
§ ꮠ䬬§䘐§ 릤§
§牨䨸
§ꮠ䬬§
릤산릤 § 䀸§ 릤산릤§ 牨 ꮠ ꮠ릤§ 산䨸牨ꮠ
ꮠ䨸牨§ ꮠ ꮠ 릤§
䘐 ꮠ § 산
§ 릤§ 牨ꮠ䬬ꮠ
갬§ 산
ꮠ 산릤§ § 릤§ 䨸䬬릤 §
ꮠ
䨸䬬ꮠ산䀸§ 䨸 릤牨릤§ 릤§산ꮠ牨§ §䬬ꮠꮠ산§牨 ꮠ ꮠ산ꮠ
§ꮠ䬬§
§牨산ꮠ
산ꮠ
§ 릤§릤䘐ꮠ䬬§산ꮠ ꮠ䀸§ §牨릤산§ 릤
릤§ §牨릤 §
산산䀸䬬§갬산 릤 §
§ꮠ§䘐ꮠ 䨸§䬬ꮠ
갬§산
䀸§ꮠ갬산
§§䨸
릤§
산
ꮠ
§ 苨릤
ꮠꮠ릤§ ꮠ
산릤 § 산
䬬ꮠꮠ
§ 牨릤산§
牨릤 릤䬬§ 산릤§ 릤䀸§ ꮠ牨산
§ 릤산䨸䬬릤§ 릤ꮠ§ 䘐릤산䀸§
ꮠ
산ꮠ
갬§ § 牨릤산§ 릤
릤§ 산
§ 릤 牨§ 릤산䬬ꮠ䀸§ § 릤§
릤산릤 § 䀸§ 䬬
갬䀸§ ꮠ
산ꮠ
갬§ ꮠ갬산
䬬§ 릤갬§
䬬䨸䬬산릤䬬§§ꮠ
ꮠꮠ산릤 §산산䀸ꮠ§릤䬬䬬§
ꮠ䬬§ 산릤§ 릤䬬ꮠ릤 § 산§ 산ꮠ
ꮠ§ 牨릤 §
鮼
䨸 왌㮴 § 䘐 ꮠ § 䘐산䬬§
릤릤 § § 릤§ 䬬䨸 산릤§ §
산䨸牨ꮠ
䨸牨§ ꮠ ꮠ 릤§ 牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ ꮠ산§ 릤릤䬬산ꮠ§
ꮠ
릤산ꮠ
§
릤§ 산ꮠ
릤 § 갬산 릤 § 牨산릤ꮠ산䬬§ 䘐릤릤§
산산릤ꮠ 릤 § 䀸§
§ ઈ⟴苨§ 산
§ 苨苨⟴§
ꮠ䬬§
릤䘐䀸§
䬬䀸
릤䬬ꮠ䬬§ § 산산䀸䬬§ 䘐산䬬§ 릤
§ 산ꮠ릤 § §
산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ 릤산ꮠ
§
릤§ 릤䬬䨸ꮠ
갬§ 䨸䬬§ 䘐릤릤§
산
산䀸 릤 § 䀸§ ઈસ⟴§
릤§ 䨸§ 릤䬬ꮠ릤 § 牨§ ꮠ䬬§
릤산ꮠ
§ ꮠ䬬§ 산릤 § ꮠ ꮠ릤䬬릤§ 산
§ 牨산䀸§ 牨ꮠ䬬ꮠ
갬䀸§ 릤§
산릤
산ꮠ릤䀸§릤
릤갬䀸§䬬䨸릤§ퟰ왌ઈퟰ뀨㮴
EXPERIMENTAL SECTION
§
Materials§
§
릤§ 䘐ꮠ
갬§ 牨산릤ꮠ산䬬§ 䬬ꮠꮠ산§ 갬릤§ ⟴ꮠ鯈§ 산
ꮠꮠ
릤§
뀨§ 산䨸牨ꮠ
ꮠ䨸牨§ ꮠ ꮠ 릤§ 苨왌§ 산
䀸 䨸䬬§
릤§ 䬬䨸 산릤§ 䨸⟴鯈§ 산릤
ꮠꮠ릤§ 왌§ 䨸릤
릤§
뀨왌§ 산
§ 산ɬ䨸산 릤䬬§ ꮠ䬬ꮠ산릤 § 牨릤 산
§ 䀸ꮠ
갬§ ꮠ§
䘐릤릤§ 䨸䬬릤 § 䘐ꮠ 䨸§ 䨸ꮠ ꮠ산ꮠ
§ § 릤§ 䬬䀸
릤䬬ꮠ䬬§ § 릤§
ꮠ牨牨ꮠꮠ 릤 § 산산䀸䬬§ ꮠ䬬ꮠ산릤 § 牨릤 산
§ 산
§ 䀸ꮠ
갬§ ꮠ§
䘐릤릤§䨸䬬릤 § § 릤§산산䀸ꮠ§릤䬬
Instrumentation
§
릤§ 산ꮠ
릤 § 산산䀸䬬§ 䘐산䬬§ 산산릤ꮠ 릤 § 䀸§
§
⟴릤 牨릤릤§
산릤 §
ઈ § 릤ꮠ
§ 魤牨릤§ ퟰ§
䬬릤ꮠ릤䬬§ 산
§ 산
§ 산䬬릤§ 산ꮠ릤§ ⟴ꮠ 릤§ 苨
산䀸 릤§ ꮠ䬬 §
苨
산䀸䬬릤릤§ § 릤§ ꮠ䬬릤䬬ꮠ
§ 쀔
ꮠ§ 산
§
릤§ 䨸䬬§
릤§ 牨릤산§ 산 ꮠ
갬§
§ 牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 䘐산䬬§ 牨릤산䬬䨸릤 §
䀸§ 苨苨⟴§ �䨸
갬ꮠ
§ 苨苨⟴§ § 苨牨ꮠ§ 苨䬬ꮠ
§
⟴릤 牨릤릤§ સ릤 䀸§ 릤䬬릤§ 䀸ꮠ릤 릤 § 牨§
산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ 䘐산䬬§ 릤
§ 산
산䀸 릤 § 䀸§ ઈસ⟴§
⟴ ꮠ牨산 䨸§સ⟴ઈ꒤ퟰ§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
Procedure
Synthesis of catalyst
⟴ꮠꮠ산§갬릤§䘐산䬬§ ꮠ䬬䀸§ 릤산릤 §산§§ § §ퟰ§ § 릤
§
牨ꮠ 릤 § 䘐ꮠ § 산
ꮠꮠ
릤§ ⟴ꮠઈ鯈§ § § ഐ§ ퟰퟰ§ ꮠ
§ 뀨§ 牨§
䨸릤
릤§ 산
§ 䬬ꮠ릤 § § § § 苨
䀸 䨸䬬§ 산䨸牨ꮠ
ꮠ䨸牨§
ꮠ ꮠ 릤§ 산 ꮠꮠ
§ ꮠ
§ 릤§ 牨ꮠ 䨸릤§ 䘐산䬬§ 릤§
릤 § 䬬릤§
산
§ 䬬ꮠ릤 § 䘐산䬬§
ꮠ
䨸릤 § § 산
릤§ § §
릤§
릤䬬䨸ꮠ
갬§䬬䨸䬬릤
䬬ꮠ
§䘐산䬬§ ꮠ릤릤 §䘐산䬬 릤 §䘐ꮠ §䨸릤
릤§
산
§ ꮠ릤 § 산§ 牨§ 릤牨릤산䨸릤§ ⟴ꮠ § 산ꮠ
릤 § 䘐산䬬§
갬산䀸ꮠ䬬 §䬬§산
§산릤 §牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§
સ ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 산
䀸 䨸䬬§ 릤§ 䬬䨸 산릤§ 산
§
산릤
ꮠꮠ릤§䘐릤릤§ 䬬산ꮠ
갬§牨산릤ꮠ산䬬§ § 䬬䀸
릤䬬ꮠ䬬§ § 릤§
산산䀸䬬§ ⟴산ꮠ
갬§ 牨산릤ꮠ산䬬§ 䘐릤릤§ 牨ꮠ 릤 § 산
§ 䬬ꮠ릤 § §
§ § 䘐산䬬 릤 § 䘐ꮠ § 산릤
ꮠꮠ릤§ 산
§ ꮠ릤 § 산§ 牨§
릤牨릤산䨸릤§
릤§ 산산䀸䬬§ 산ꮠ
릤 § 䘐산䬬§ 산산릤ꮠ 릤 §
䀸§
§산
§산
§산䬬릤ઈ산ꮠ릤§⟴ꮠ 릤§苨
산䀸 릤
Leaching test
ퟰ§ 갬§ § 릤§ 䬬ꮠ § 산산䀸䬬§ 䘐산䬬§ 䬬䨸䬬릤
릤 § ꮠ
§
산릤
ꮠꮠ릤§산
§䬬ꮠ릤 § §§ § 苨 릤䘐산 § 릤§䬬䨸ꮠ
§
산§ 䘐산䬬§ 䬬릤산산릤 § 䀸§ ꮠ산ꮠ
§ 산
§ 산
산䀸 릤 § 䀸§ 苨苨⟴§
�䨸
갬ꮠ
§
苨苨⟴§
§
苨牨ꮠ§
苨䬬ꮠ
§
⟴릤 牨릤릤§§ 릤릤牨ꮠ
릤§ꮠ䬬§䨸§
릤
Optimalization of the immobilized Cu(II) catalyst on
transesterification of frying oil
산산䀸ꮠ§ 산ꮠꮠ䀸§ § 산산䀸䬬䬬§ 산ꮠ릤 § ꮠ
§
산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ § 䀸ꮠ
갬§ ꮠ§ 䘐ꮠ § 산§ 산ꮠ산ꮠ
§ §
산산䀸䬬§
릤
산ꮠ
§ 䬬ꮠꮠ
갬§ 산릤§ 산
§ 䨸산ꮠ
§ §
릤산ꮠ
§
릤§산牨䨸
§ §晸§뀨晸§뀨晸§晸§ퟰퟰ晸§ퟰ왌晸§
산
§ퟰ뀨§ 䘐릤ꮠ갬 § Ⳉ§ § 산산䀸䬬§ 䘐산䬬§릤䬬릤ꮠ릤䀸§ 산 릤 §
§ 牨릤 산
§ 산
§ 䬬ꮠ릤 § § 牨§ § § § ퟰ뀨§ 牨ꮠ
§
苨 릤䘐산 § 䀸ꮠ
갬§ ꮠ§ 䘐산䬬§ 䨸§ ꮠ
§ 산산䀸䬬䬬ઈ牨릤 산
§
䬬䨸ꮠ
§ 산
§ 䬬ꮠ릤 § § ퟰ§ §
릤§ 산릤§ 䬬䨸ꮠ
§ 䘐산䬬§
산
산䀸 릤 §䀸§ઈસ⟴§ ⟴ ꮠ牨산 䨸§સ⟴ઈ꒤ퟰ§�ꮠ릤 §
§ 牨릤 䀸§ 릤䬬릤§ 䨸§ 䘐산䬬§ 산䨸
릤 § 산䬬§ 䘐ꮠ
갬§
릤ɬ䨸산ꮠ
䀸ꮠ릤 § § 䨸§ഐ§
릤산§산릤산§ §§ §牨릤 䀸§릤䬬릤§ 䨸릤 § §ퟰⳈ
§ §ꮠ§산릤
§ § 릤§릤산ꮠ
산ꮠ산ꮠ
䬬§ § 䬬ꮠꮠ
갬§ 산릤§ 䘐릤릤§ 䨸
§ 산§ § 牨§
왌§ 牨§ § 牨§ 산
§ 뀨§ 牨§ સ릤산
䘐 ꮠ릤§ §
䨸산ꮠ
§ § 릤산ꮠ
䬬§ 䘐산䬬§ ꮠ
릤䬬ꮠ갬산릤 § § 왌§ 牨ꮠ
§ §
§牨ꮠ
§牐§牨ꮠ
§ퟰ§牨ꮠ
§§ §牐§ §산
§ퟰ§
§
RESULT AND DISCUSSION§
§
FTIR Analysis of the Catalyst§
§
ꮠ갬§ ퟰ§ 䬬 䘐릤 § 릤§
§ 䬬릤산§ § 산릤
§ 䬬ꮠꮠ산§
牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 산
䀸 䨸䬬§ 릤§ 䬬䨸 산릤§ 산
§
산산䀸䬬§ 산ꮠ
릤 § ⟴ꮠꮠ산§ 갬릤§ 산䬬§ 䬬릤ꮠ ꮠ§ 산 䬬ꮠ
§ 산§
ઈퟰ
왌Ὠ§ 牨 § 䘐 ꮠ § 䘐산䬬§ 산䬬䬬ꮠ갬
릤 § § 鯈ઈ§ 䬬릤 ꮠ
갬§ §
䬬ꮠꮠ산§䬬䨸 산릤§ퟰ㮴§산䬬릤 §
§ ꮠ䬬§ 산§ 릤§䬬ꮠꮠ산§䬬䬬릤䬬§
§ §§⟴ꮠઈ鯈§§
ꮠ
갬§§ 䬬ꮠ산
§갬䨸䬬§§산
§§ 䀸 䀸§§
74
Indo. J. Chem., 2013, 13 (1), 72 - 76
§
Fig 1.
§䬬릤산§ 산§산릤
§䬬ꮠꮠ산§ §牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§
§산
䀸 䨸䬬§릤§䬬䨸 산릤§산
§ §산산䀸䬬§산ꮠ
릤 §
§
§
Fig 2. ꮠ䬬ꮠ䨸ꮠ
§ 산
§ 산ꮠ릤§ 䬬ꮠ 릤§ § 산릤
§ 䬬ꮠꮠ산§ 갬릤§
牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§산
§산산䀸䬬§산ꮠ
릤 §
§
갬䨸䬬§ 牨§ 산 䬬릤 §䘐산릤§ퟰὨ㮴§
릤§䬬릤
䬬§산
§ 산§
ퟰ牐§ 牨 ઈퟰ§ 䘐산䬬§ 산䬬䬬ꮠ갬
릤 § § 䬬ꮠ 산
릤§ 갬䨸䬬§ ⟴ꮠઈ鯈ઈ⟴ꮠ§
ઈퟰ
ઈퟰ
苨 ꮠꮠ
산§산
䬬§산릤산§산§牐§牨 §산
§Ὠ牐§牨 § 䨸릤§§
릤ꮠ§ 릤 牨산ꮠ
§ §⟴ꮠઈ鯈§
ꮠ
갬§ 牨§⟴ꮠ鯈§
산
§ § 牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 산릤산릤 § 䘐ꮠ § 䘐릤산§
ઈퟰ
ꮠ
릤
䬬ꮠ䀸§산§牐§牨 §§ꮠ
ꮠ산릤 § 릤§산릤산산
릤§ §⟴ꮠઈ鯈§
䘐ꮠ § 牨릤산䬬§
ꮠ
갬§ ⟴ꮠઈ鯈ઈ苨§ 산
§ 산§ Ὠ§ 牨 ઈퟰ§ 䘐산䬬§
산䬬䬬ꮠ갬
릤 §§ઈઈ§䘐산갬갬ꮠ
갬§ §산
ꮠꮠ
ꮠ䨸牨§산ꮠ
§산
䬬§ §
산산䀸䬬䬬§ 산ꮠ
릤 § 산릤산§ 산§ 왌왌§ 牨 ઈퟰ§ 䨸 § 릤§
산䬬䬬ꮠ갬
릤 §§
ꮠꮠ릤§ ≡§ 갬䨸§ꮠ산ꮠ
䬬§ § 릤§갬산 릤 §
牨䨸
䬬§
릤§ υ § ꮠ산ꮠ
§ § 릤릤§ 왌§ 䘐䨸 §
릤§ 릤 릤릤 § 산§ 뀨왌§ 산
§ 牐왌§ 牨 ઈퟰ§ ퟰઈ㮴§
§ 산산䀸䬬§
ઈퟰ
ઈퟰ§
䬬릤산§ ꮠ䬬산릤산산
릤§ § 산
䬬§ 산§ Ὠ§ 牨 § ퟰퟰ§ 牨
鮼§
ઈퟰ§
산
§ ퟰ牐§ 牨 牨 §뀨왌 ꮠ
§ 䨸 릤牨릤§ 산
䬬§
ꮠ
릤
䬬ꮠ䀸§산§Ὠ牐§牨ઈퟰ§ 牨§⟴ꮠઈ鯈§릤
ꮠ
갬§ꮠ
§䬬䨸 §산산䀸䬬§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
䘐릤산릤§ 산
§ 릤§
릤§ ꮠ
§ 산릤
§ 䬬ꮠꮠ산§ 산䨸䬬릤 § 䀸§
ꮠ
릤산ꮠ
§ 릤䘐릤릤
§ 䬬ꮠ산
§ 갬䨸䬬§ 䘐ꮠ § 䨸 § 牨릤산§
릤
릤§
릤§ 산산ꮠ산ꮠꮠ䀸§ § 䬬 ꮠ 릤 § § 䬬릤 ꮠ
갬§
ꮠ산ꮠ
§산䬬§䨸 §릤§ 산갬䨸릤 § 산䬬§산§䬬䨸릤䬬䬬 䨸§ 갬산 릤 §
§䨸 §산릤
ꮠꮠ릤§牨릤 §
§ 릤§牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§ퟰ㮴§
§
NL-PSA Analysis§
§
ઈ⟴苨§ 갬산릤§ ꮠ
牨산ꮠ
§ 산䨸§ 䬬ꮠ 릤§ 산
§
ꮠ䬬ꮠ䨸ꮠ
§ § 산ꮠ릤§ § 산
§ 릤§ 䬬릤릤
§ 牨§ ꮠ갬§ § 산§
산 릤
ꮠ
갬§ § 산릤
§ 䬬ꮠꮠ산§ ꮠ䬬ꮠ䨸ꮠ
§ ꮠ
§ ퟰ뀨ઈ§ �牨§
산
갬릤§ 䘐ꮠ § 牨ꮠ
산릤 § 䀸§ ퟰ§ �牨§ 산ꮠ릤§ 䬬ꮠ 릤§ 苨§
산 릤
ꮠ
갬§ ꮠ䬬ꮠ䨸ꮠ
§ § ꮠ䬬§ 牨산릤ꮠ산§ ꮠ
ꮠ산릤 § 산§
릤§䬬ꮠꮠ산§䘐산䬬§산牨 䨸䬬§§
સ ꮠ ꮠ릤 §䬬ꮠꮠ산§ 산䬬§
산䘐§ ꮠ䬬ꮠ䨸ꮠ
§산
§䬬牨산릤§
산ꮠ릤§䬬ꮠ 릤§ 산
§ꮠ䬬§산릤
§䬬ꮠꮠ산§䘐 ꮠ §䬬릤릤牨ꮠ
갬䀸§산䬬§산§
䬬릤ɬ䨸릤
릤§ § 릤§ ꮠ
릤산ꮠ
§ 릤䘐릤릤
§ 苨왌§ 산䬬§
牨 ꮠ ꮠ릤§ 䘐ꮠ § 䬬ꮠꮠ산§ 䬬䨸 산릤§ 릤
§ 갬산 릤 § 䨸 §
牨릤 §
§ 牨 ꮠ ꮠ릤 § 䬬ꮠꮠ산§ 릤§ 산ꮠ릤§ 䬬ꮠ 릤§ 산
§
ꮠ䬬ꮠ䨸ꮠ
§䬬ꮠ갬 䀸§ 릤릤산䬬릤 § 산§산
§릤§ 산산릤§ §
ꮠ䬬§산산䀸ꮠ§산ꮠꮠ䀸§ 䨸릤§§산갬릤§䬬릤ꮠ ꮠ§䬬䨸 산릤§산릤산§
§
Atomic Absorption Spectroscopy (AAS)§
§
苨苨⟴§ 산
산䀸䬬ꮠ䬬§ ꮠ 릤 § 릤§ 산牨䨸
§ § 牨릤산§
산 ꮠ
갬§ 산
§ 牨릤산§ 릤산 ꮠ
갬§ 산릤§ § 䘐산䬬§ 䨸
§ 산§ 릤§
牨릤산§ 산 ꮠ
갬§ § 䨸§ ꮠ
§ 릤§ 산산䀸䬬§ 䘐릤릤§ ퟰ牐Ⳉ§ 䀸§
牨산䬬䬬§산
§
䀸§䨸
릤갬릤䬬§ퟰⳈ§䬬䬬§ꮠ
§ 릤§䬬릤
§
산 릤§§ §릤산 ꮠ
갬§릤䬬§
ꮠ䬬§䬬牨산§산䨸릤§ꮠ
ꮠ산릤 § 산§
릤§ 䨸 § 牨릤산§ 릤
릤§ 䘐산䬬§ 䬬
갬䀸§ 䨸
릤 §
§ 릤§
牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§ 䨸갬 §릤릤䬬산ꮠ§ꮠ
릤산ꮠ
§
§
Catalytic Application at Optimal Conditions§
§
Catalyst concentrations
릤§ 䨸§ § 산산䀸䬬§
릤
산ꮠ
§ 䘐산䬬§
산
산䀸 릤 § 䀸§ ઈસ⟴§
§ ꮠ갬§ 왌§ 䀸§ 산 ꮠ
갬§ ퟰ뀨Ⳉ§
산산䀸䬬§ ꮠ
§ 릤§ 牨ꮠ 䨸릤§ § 牨릤 산
§ 산
§ 䀸ꮠ
갬§ ꮠ§ 릤§
䀸ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ 릤릤 §ꮠ
릤산䬬릤䬬§䨸
ꮠ§ 산䨸§ §
Ⳉ§ 䘐 ꮠ §
산ꮠ
§ Ὠ牐Ⳉ§ 䨸§
릤§ 䨸§
산ꮠ
릤 § 䘐릤릤§ 牨릤 䀸§ 릤䬬릤§ 䘐 ꮠ § 䨸
§ 왌ퟰⳈ§牨릤 䀸§
산牨ꮠ산릤§ 산§ ퟰퟰ牐§ 牨ꮠ
§ 릤릤
ꮠ
§ ꮠ牨릤§ 산
§ 왌牐Ⳉ§
牨릤 䀸§ 릤산릤§ 산§ ퟰ§ 牨ꮠ
§ 릤릤
ꮠ
§ ꮠ牨릤§ 苨§ ꮠ䬬§
ꮠ
§ ꮠ갬 릤§ § 䀸ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ 䨸릤§ § 릤§ 牨䬬§
䨸산릤 § 牨산ꮠ
§ § 牨릤 ꮠ 릤§ 산
ꮠ
§ 䘐 ꮠ § ꮠ䬬§ 릤䀸§
ꮠ牨산
§ § ꮠ
ꮠꮠ산릤§ 릤§ 산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ § 䀸ꮠ
갬§ ꮠ§
산ꮠ
ꮠ
갬§ ꮠ갬䀸릤ꮠ 릤§ 산§ 산§ ꮠ
§ 䘐ꮠ§ 산䬬§ 릤§
산䬬䬬䨸牨릤 § 산䬬§ 산§ 릤䀸§ 산§ ퟰ왌㮴§
릤산䬬릤 § § 산산䀸䬬§
릤
산ꮠ
§ 牨산릤§ 䀸ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ 산ꮠ
릤 §
산牨산ꮠ산䀸§䬬릤§ 䘐
§§산牨䬬§ 릤§
§
Stirring rate
�ꮠ릤 § § 牨릤 䀸§ 릤䬬릤§ ꮠ
§ 䬬ꮠꮠ
갬§ 산릤§산ꮠ산ꮠ
䬬§산䬬§
릤ꮠ릤 §ꮠ
§ ꮠ갬§§
릤§䀸ꮠ릤 §산牨䨸
§ §牨릤 䀸§ 릤䬬릤§산§
왌§牨§§ꮠ䬬§§ 릤§§릤䬬§§
ꮠꮠ
§§ 䨸릤§§§§ ꮠ갬 릤§ 䨸§§
Indo. J. Chem., 2013, 13 (1), 72 - 76
§
Fig 3. 산산䀸䬬§
릤
산ꮠ
§ 䬬§ 산䀸§ 牨릤 䀸§ 릤䬬릤§
산ꮠ
릤 §ꮠ
§ ꮠ䬬§䘐§
§
§
Fig 5. 䨸릤§ 牨릤 䀸§ 릤䬬릤§ 䨸§ 산§ 牨§ 릤산ꮠ
§
ꮠ牨릤䬬§산ꮠ산ꮠ
䬬§
§
산ꮠ
릤 §苨§ 왌§牨§ 䘐산䬬§ 䨸
§뀨Ⳉ§ § 䨸§ 산§
산ꮠ
§ 뀨ퟰⳈ§ § 牨릤 䀸§ 산牨ꮠ산릤§ ퟰ왌뀨Ⳉ§ 牨릤 䀸§
릤산릤§ 산
§ 왌Ⳉ§ 牨릤 䀸§ 䬬릤산산릤§ 산§ ퟰퟰ§ 牨ꮠ
§
릤릤
ꮠ
§ꮠ牨릤§
ꮠ䬬§ 릤
牨릤
§산
§릤§산갬䨸릤 § 산§산§
ꮠ䬬§ 산릤§ 릤§ 산 䬬ꮠ
ઈ 릤䬬ꮠ
§ § 䬬䨸䬬산릤䬬§
§
산산䀸䬬§ 䬬䨸 산릤§ 릤산 릤䬬§ ꮠ䬬§ 릤ɬ䨸ꮠꮠꮠ䨸牨§ 산§ 산䘐䬬§ 릤§
산산䀸䬬§§䘐§ꮠ牨산䀸§
§
The duration of the reaction
苨䬬§산
§릤§䬬릤릤 §ꮠ
§ ꮠ갬§뀨§ 릤§
갬릤§ § 䨸산ꮠ
§
§ 릤산ꮠ
§䘐산䬬§䨸
§ꮠ
§ ꮠ갬 릤§ 䨸§산ꮠ
릤 §
§ ꮠ䬬§
산릤§ 릤§
갬릤§ § 䨸산ꮠ
§ꮠ牨릤§ § 릤산ꮠ
§䘐릤릤§§ 牐§
산
§ ퟰ§ § § 䘐산䬬§ 䨸
릤 § 牐牐§ 뀨§ 산
§ 뀨ퟰⳈ§ §
䨸§
ꮠ䬬§ 산§ 䬬 䘐릤 § 산§ 䬬ꮠ갬
ꮠ ꮠ산
§ 릤 릤§ § 릤§
䨸산ꮠ
§ § 산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ 릤산ꮠ
§ § 산䘐§ 牨릤§
䬬䨸䬬산릤§§ꮠ
릤산§䘐ꮠ § 릤§䬬䨸 산릤§ §䬬䨸 §ꮠ牨牨ꮠꮠ 릤 §
䨸§산산䀸䬬§
§
CONCLUSION
§
牨牨ꮠꮠ 산ꮠ
§ § 䨸 ઈ산릤
ꮠꮠ릤§ 牨릤 §
§
牨 ꮠ ꮠ릤 §䬬ꮠꮠ산§산
§릤§릤 牨릤 §산
§牨ꮠ䬬ꮠ
갬䀸§산
§릤§
산ꮠ릤 § ꮠ
§ 산
䬬릤䬬릤ꮠ ꮠ산ꮠ
§ § 䀸ꮠ
갬§ ꮠ§
릤§ 산산䀸䬬§
䀸릤§⟴䀸ꮠ산
산§산ꮠ 산§릤§산
75
§
Fig 4. ⟴ꮠꮠ
갬§ 릤ꮠ䀸§ 갬ꮠ릤䬬§ 䬬ꮠ갬
ꮠ ꮠ산
§ ꮠ牨산§
§
산산䀸ꮠ§산ꮠꮠ䀸§ § 릤§산산䀸䬬§䨸䬬릤 §ꮠ
§ ꮠ䬬§릤산ꮠ
§
䬬 䘐䬬§ ꮠ䬬§ ꮠ牨산§
ꮠꮠ
䬬§ 산§ Ⳉ§ 산산䀸䬬§
릤
산ꮠ
§ 산
§ 왌§ 牨§ 䬬ꮠꮠ
갬§ 산릤§ 䘐릤릤§ ꮠ䬬§
릤릤
릤
릤§
§ 릤§ 䨸산ꮠ
§ § 릤산ꮠ
§ꮠ牨릤§䬬ꮠ§ §릤§
䬬릤§ꮠ
§ 릤§
릤 §릤䬬릤산 §
§
ACKNOWLEDGEMENT§
§
릤§ 䘐䨸 § ꮠ릤§ 산
䬬§ § સ산릤ꮠ산§ 릤牨ꮠ䬬䀸§
산산䀸§䬬산 § § 릤ꮠ§ 릤§ꮠ
§ 릤§
§산
§ઈ⟴苨§
牨릤산䬬䨸릤牨릤
§
릤
§ 䨸§ 산
䬬§ 갬§ § 릤
산§ 쀔
산
§
산산䀸§ 산
§ 苨﵌魤⟴§ 산 산
갬§ 산산䀸§ § 릤ꮠ§
릤§ꮠ
§苨苨⟴§산
§ઈસ⟴§牨릤산䬬䨸릤牨릤
§릤䬬릤ꮠ릤䀸§
§
REFERENCES
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