Pemantapan Proses Sintesis Ligan Dibutilditiokarbamat (DBDTK) Sebagai Pengekstrak Logam Tanah Jarang Berdasarkan Desain Eksperimen

Abstract

<p>Gadolinium (Gd) merupakan salah satu logam tanah jarang, dimana logam tanah jarang dapat diekstrak dari mineral salah satunya mineral monasit. Logam Gd biasanya digunakan sebagai bahan dasar <em>contrast agent</em> dalam dunia kesehatan. Ligan dibutilditiokarbamat mampu membentuk senyawa kompleks dengan cara mengikat logam sehingga membentuk khelat yang dapat digunakan untuk ekstraksi. Tujuan dari penelitian ini adalah memantapkan sintesis ligan dibutilditiokarbamat berdasarkan desain eksperimen dan karakterisasi kompleks antara Gd(III) dengan ligan dibutilditiokarbamat hasil sintesis. Penelitian ini diawali dengan pembuatan desain eksperimen untuk sintesis ligan dan ekstraksi Gd(III) dengan ligan, kemudian proses sintesis dan ekstraksi dilakukan sesuai dengan desain eksperimen, hasil sintesis dan ekstraksi dikarakterisasi menggunakan metode spektroskopi serta diuji kelarutannya dalam pelarut organik. Data yang diperoleh menunjukkan bahwa sintesis ligan dibutilditiokarbamat optimal pada suhu 4 °C, perbandingan dibutilamin dan karbondisulfida yaitu 1 : 3 dengan perbandingan mol ammonia terhadap dibutilamin yaitu 1 : 4, sedangkan kondisi optimal untuk ekstraksi Gd(III) dengan ligan yaitu pada pH 6, dengan perbandingan mol Gd(III) dan ligan yaitu 1 : 4 dan lama ekstraksi 60 menit. Oleh karena itu ligan dibutilditiokarbamat hasil sintesis berpotensi digunakan sebagai ekstraktan untuk ekstraksi Gd(III). Hasil prediksi ligan berdasarkan desain eksperimen yaitu sebesar 56,12% sedangkan prediksi ekstraksi Gd(III) dengan ligan hasil sintesis diperoleh sebesar 78,41%.</p><p><strong>The Consolidation of Dibutyldithiocarbamate (DBDTC) Synthesis as Gadolinium Metal Extraction Based On Experimental Design. </strong>Gadolinium (Gd) is one of the rare-earth elements, whereas rare-earth elements can be extracted from monazite. Gd is usually used as raw material for synthesizing contrast agent<em> </em>in medicine field. Dibuthyldithiocarbamate ligand can form a complex compound with metal. This ligand will bind a metal and then forming chelate which is used for extraction. The purpose of this research is to ensure procedure of dibuthyldithiocarbamate ligand synthesis based on the design of experiment and to study the characterization of reaction result between Gd(III) and dibuthyldithiocarbamate ligand which this ligand is synthesis result. This research begins with making design of experiment for ligand synthesis and Gd(III) extraction with ligand, then perform the process of synthesis and extraction according to the design of experiment, the result of synthesis and extraction were characterized by spectroscopy method and solubility tested in organic solvent. The data was collected indicate that the optimal condition of dibuthyldithiocarbamate ligan synthesis at 4 °C (temperature), the ratio of di-n-butylamine and carbon disulphide is 1:3 with the mole ratio of ammonia to the di-n-butylamine 1:4, while the optimal conditions for gadolinium extraction with ligand at pH 6, the mol ratio of gadolinium and ligand is 1:4 and 60 minutes extraction time. Hence, dibuthyldithiocarbamate ligand can be used as extractan for extracting Gd(III). The prediction of ligand based on the experimental design is 56.12% while the prediction of Gd(III) extraction with ligand of the synthesis result is obtained equal to 78.41%. The conclusion of this research is that the synthesis of dibuthyldithiocarbamate ligand based on the experimental design can be developed for large-scale synthesis.</p>

Karakterisasi Hasil Reaksi Ion Gadolinium (III) dengan Ligan Dibutilditiokarbamat Menggunakan Metode Mekanika Molekular (MM2)

“…Ditiokarbamat merupakan suatu senyawa yang dihasilkan dari reaksi antara amonia dan karbon disulfida. (Hendrati et al 2018). Ligan ini sering digunakan dalam penentuan ion-ion logam transisi dalam kadar runut karena mampu membentuk senyawa kompleks dengan berbagai ion logam transisi dan senyawa kompleks yang terbentuk bersifat stabil, mempunyai kelarutan yang rendah dalam air tetapi dapat larut baik dalam pelarut organik (Mueller & Lovett 1987).…”

Optimization of Large Scale Dibuthyldithiocarbamate Synthesis by Experimental Design and Application as Extractant for Gadolinium(III)

“…Based on the results of experimental design data processing on previous research [7], verification of laboratory scale ligand synthesis was done. The condition of ligand synthesis is shown in Table 1.…”

“…Based on the results of the previous experimental design data processing [7], the optimized parameters are: mole ratio of di-n-butylamine and CS 2 (1: 3) and the temperature of 4°C. The result of this synthesis is shown in Table 2.…”

“…Based on the previous research 7 , we applied the optimum parameters for synthesis of DBDTC which mole ratio of di-n-butylamine and CS 2 is 1: 3 and the temperature at the synthesis is 4 ° C. The results of scale up synthesis of DBDTC ligand is shown in Table 4.…”

“…The determination of the optimal condition often requires a considerable amount of experiments, which is particularly detrimental in terms of cost, materials and time, to avoid it, we interest to utilize an experimental design which allows the study of the effects of various factors on one or more responses and to determine the mathematical model relation between these factors and responses [6]. In our previous research [7], we success to develop a synthesis procedure for DBDTC with a combination of experimental design in order to obtain a more optimal and efficient ligand synthesis procedure compared to existing synthesis procedures. We decided to use full factorial design because it can calculate all combinations between factor levels during the experiment, and to know the effect of each factor on the response and the interaction effect between different factors [8].…”