PEMANFAATAN LIMBAH MILL SCALE MENJADI MAGNETIT MENGGUNAKAN METODE OKSIDASI SELEKTIF UNTUK APLIKASI PENGOLAHAN LIMBAH TEKSTIL DAN SINTESA BESI MELALUI PROSES REDUKSI

NURDIYANSAH, LUKMAN FARIS (2021) PEMANFAATAN LIMBAH MILL SCALE MENJADI MAGNETIT MENGGUNAKAN METODE OKSIDASI SELEKTIF UNTUK APLIKASI PENGOLAHAN LIMBAH TEKSTIL DAN SINTESA BESI MELALUI PROSES REDUKSI. S2 thesis, Universitas Mercu Buana Jakarta.

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Abstract

The process was doed with had been milling mill scale and graphite powders had been using high energy milling (HEM) to produce homogeneous powders with sizes below 400 mesh. Next, the mill scale powder which was added graphite then was calcined at a temperature of 300°C for 0.5; 1 and 2 hours. The calcined powder was tested for X-ray diffraction (XRD), Vibrating Sample Magnetometer (VSM) and Particle Size Analyzer (PSA). In addition, the magnetite powder result was mixed and separated with a textile dye solution with 1:5 powder and solution volume ratio by centrifugation method. The processed liquid was seen for its adsorption efficiency through visually with photo comparison. In the second study, the author was carried out a mill scale reduction process through milling process, it was used High Energy Milling (HEM). The mill scale powder and graphite was milled with a mass ratio of 4:1 and 4, 6 and 12 hours milling time variations. The powder that produced was tested by XRD, VSM and (Scanning Electron Microscope-Energy Dispersive Spectroscopy) SEM-EDS. In the first study from the XRD test, it is found that the calcined powder has magnetite as main phase, then wustite and hematite as minor phases. The value of remanence, coercivity and magnetic saturation value of the calcined powder is 11.93, 12.35, 18.05 emu/g; 436.38, 457.45, 765.81 Oe and 47.14, 46.3, 48.08 emu/g. The particle size of the calcined powder is in the range of 30-40, 50-60 and 40-50 μms. From the solutions photo comparison, it can be seen that mill scale powder that has been calcined is effective for absorb textile dyes. In the second study, from XRD test, it is found that the powder with 4; 6 and 12 hours time variations consisted of Fe3C as the main phase and carbon, magnetite, wustit and Fe2 as minor phases. The percentage of wustit composition is inversely proportional to the variation of milling time, by 6.9; 6.9; 5% while the iron composition percentage is increase with the milling times, with 6; 10.9; 13%. The value of remanence, coercivity and magnetic saturation of milled powder are 2.89, 3.39, 4.98 emu/g; 209.58, 188.47, 223.65 Oe and 22.59, 30.7, 39.15 emu/g respectively. From the SEM-EDS test, it is found that the distribution of the iron composition become more uniform during the milling time. Keyword: Mill scale, textile dye, oxidation, reduction, adsorption, iron Proses yang digunakan pada riset ini diawali dengan milling serbuk mill scale dan grafit menggunakan high energy milling (HEM) untuk menghasilkan serbuk yang homogen dibawah 400 mesh. Selanjutnya, serbuk mill scale yang ditambahkan grafit dikalsinasi pada temperatur 300°C selama 0,5; 1 dan 2 jam. Serbuk yang telah dikalsinasi diuji diffraksi sinar-X (XRD), Vibrating Sample Magnetometer (VSM) dan Particle Size Analyzer (PSA). Selain itu, serbuk magnetit yang dihasilkan, dicampur dan dipisahkan dengan larutan pewarna tekstil dengan perbandingan volume serbuk dan larutan 1:5 melalui sentrifugasi. Cairan yang telah diproses dilihat efisiensi adsorpsinya melalui perbandingan foto. Pada penelitian kedua dilakukan proses reduksi mill scale melalui proses milling serbuk mill scale dan grafit dengan perbandingan massa 4:1 menggunakan High Energy Milling (HEM) dengan variasi waktu milling 4, 6 dan 12 jam. Serbuk yang dihasilkan diuji XRD, VSM dan (Scanning Electron Microscope-Energy Dispersive Spectroscopy) SEM- EDS. Pada penelitian pertama berdasarkan uji XRD diperoleh bahwa pada serbuk yang telah dikalsinasi telah terbentuk fasa utama magnetite serta fasa minor wustite dan hematite. Serbuk yang diproses dengan variasi waktu penahanan kalsinasi 0,5; 1 dan 2 jam memiliki nilai remanensi, koersifitas dan magnetik saturasi sebesar 11,93; 12,35 dan 18,05 emu/g; 436,38; 457,45 dan 765,81 Oe, dan 47,14; 46,3; 48,08 emu/g. Serbuk yang telah dikalsinasi dengan variasi 0,5; 1 dan 2 jam memiliki ukuran partikel berkisar 30-40, 50-60 dan 40-50 μm. Dari perbandingan foto larutan didapat bahwa serbuk mill scale yang telah dikalsinasi efektif untuk adsorpsi pewarna tekstil. Pada penelitian kedua, dari uji XRD diperoleh bahwa serbuk terdiri dari fasa utama Fe3C dan fasa minor karbon, magnetit, wustit and Fe2. Persentase komposisi wustit berbanding terbalik dengan variasi waktu milling, sebesar 6,9; 6,9; 5 %, sedangkan persentase komposisi besi meningkat seiring lama waktu milling sebesar 6; 10,9; 13 %. Nilai remanensi, koersifitas dan nilai magnetik saturasi serbuk adalah 2,89; 3,39; 4,98 emu/g; 209,58; 188,47, 223,65 Oe dan 22.59, 30.7, 39.15 emu/g. Dari uji SEM-EDS diperoleh bahwa distribusi komposisi Fe semakin seragam seiring dengan lama waktu milling. Kata Kunci: Mill scale, limbah tekstil, oksidasi, reduksi, adsorpsi, besi

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