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SYNTHESIS OF NiPd-NH2/LAPINDO MUD CATALYST FOR THE HYDROTREATMENT OF USED COOKING OIL INTO BIOFUEL

AFRA ALETHIANA, Prof. Dr. Iip Izul Falah; Prof. Dra. Wega Trisunaryanti, M.S, Ph.D.Eng.

2021 | Skripsi | S1 KIMIA

Telah dilakukan sintesis katalis Lumpur NiPd-NH2/ Lapindo untuk perlakuan hidro minyak goreng bekas menjadi bahan bakar hayati (biofuel). Penelitian ini bertujuan untuk mensintesis katalis dengan aktivitas dan selektifitas tertinggi dalam menghasilkan fraksi cair yang terdiri dari senyawa hidrokarbon (biofuel) dengan persentase yang tinggi. Proses pengembanan logam Ni, Pd, dan NiPd dilakukan melalui metode impregnasi basah dilanjutkan dengan kalsinasi menggunakan gas N2 pada suhu 450 �°C selama 3 jam dan reduksi di bawah aliran H2 pada suhu 500 �°C. Langkah ini menghasilkan katalis LL, Ni/LL, Pd/LL, NiPd/LL. Penambahan gugus fungsi amina pada katalis dilakukan dengan metode grafting menggunakan 3-Aminopropyl Trimethoxy Silane (3-APTMS) dalam 20 mL toluena. Tahap ini menghasilkan katalis NH2/LL, Ni-NH2/LL, Pd-NH2/LL, dan NiPd-NH2/LL. Katalis yang diperoleh kemudian dikarakterisasi menggunakan X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Fourier Transform Infrared Spectrometry (FTIR), Surface Area Analyzer (SAA), Scanning Electron Microscopy-Enegry Dispersive X-Ray (SEM- EDX), Transmission Electron Microscopy (TEM), dan uji keasaman menggunakan metode gravimetri. Katalis kemudian digunakan dalam perlakuan hidro minyak goreng bekas dalam sistem reaktor semi-batch berbahan stainless-steel dengan aliran H2 selama 2 jam. Perlakuan hidro katalis dengan kinerja terbaik dilakukan dengan variasi suhu (450, 500, dan 550 �°C) dan rasio berat katalis/umpan (1/50, 1/100, dan 1/200). Kegunaan katalis dengan kinerja terbaik dilakukan dengan penggunaan kembali katalis untuk perlakuan hidro sebanyak tiga kali. Komposisi produk cair dianalisis dengan Gas Chromatography-Mass Spectrometry (GC-MS). Katalis NiPd-NH2/LL dengan volume pori dan total keasaman 0,03 cc g-1, dan 0,07 mmol g-1 merupakan katalis dengan kinerja terbaik yang menghasilkan fraksi cair tertinggi yaitu 78,9wt% yang terdiri dari senyawa hidrokarbon (biofuel). 66.1wt% pada 550 �°C dan rasio berat katalis/umpan sebesar 1/100. Proses hydrotreatment pertama, kedua, dan ketiga menggunakan katalis NiPd-NH2/LL menghasilkan fraksi cair sebesar 71,5wt% (dengan 48,9wt% senyawa hidrokarbon), 37,0wt% (dengan 26,4wt% senyawa hidrokarbon) dan 61,7wt% (dengan 39,0wt% senyawa hidrokarbon).

Synthesis of NiPd-NH2/Lapindo Mud catalyst for the hydrotreatment process of used cooking oil into biofuel had been carried out. The aim of this research was to synthesize a catalyst with the highest activity and selectivity in producing liquid fraction consisted of high percentage of hydrocarbon compounds (biofuel). The Ni, Pd, and NiPd was loaded onto the mud through wet-impregnation method followed by calcination using N2 gas at 450 �°C for 3 h and reduction under the flow of H2 gas at at 500 �°C for 3 h. This step produced LL, Ni/LL, Pd/LL, NiPd/LL catalysts. The addition of amine-functionalized group onto the catalyst was performed by grafting method using 3-Aminopropyl Trimethoxy Silane (3-APTMS) in 20 mL toluene. This step produced NH2/LL, Ni-NH2/LL, Pd-NH2/LL, and NiPd-NH2/LL catalysts. The obtained catalysts were then characterized using X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Fourier Transform Infrared Spectrometry (FTIR), Surface Area Analyzer (SAA), Scanning Electron Microscopy-Enegry Dispersive X-Ray (SEM-EDX), Transmission Electron Microscopy (TEM), and acidity test using gravimetric method. The catalyst was then used in hydrotreatment of used cooking oil in a stainless-steel semi-batch reactor system under H2 stream for 2 h. The hydrotreatment of catalyst with the best performance was carried out with variation of temperatures (450, 500, and 550 �°C) and catalyst/feed weight ratios (1/50, 1/100, and 1/200). The usability of catalyst with the best performance was carried out in second followed by third hydrotreatment run. The composition of liquid product was analyzed by Gas Chromatography-Mass Spectrometry (GC-MS). The NiPd-NH2/LL catalyst with the pore volume and total acidity of 0.03 cc g-1, and 0.07 mmol g-1 was the best performed catalyst that produced the highest liquid fraction of 78.9wt% which consisted of hydrocarbon compounds (biofuel) of 66.1wt% at 550 �°C and catalyst/feed weight ratio of 1/100. The firsts, second, and third run of the hydrotreatment using NiPd-NH2/LL catalyst produced liquid fraction of 71.5wt% (hydrocarbon compounds of 48.9wt%), 37 wt% (hydrocarbon compounds of 26.4wt%) and 61.7wt% (hydrocarbon compounds of 39.0wt%).

Kata Kunci : lapindo mud, hydrotreatment, biofuel, bimetal catalyst

  1. S1-2021-398534-abstract.pdf  
  2. S1-2021-398534-bibliography.pdf  
  3. S1-2021-398534-tableofcontent.pdf  
  4. S1-2021-398534-title.pdf