PREPARATION OF POROUS CARBON MATERIAL BY PYROLYSIS OF PHENOL AND P-TERT-BUTYLPHENOL WITH FORMALDEHYDE :
Operating Condition Influence of Pyrolysis to Internal Surface Area and Mean pore diameter
Endro Wahyono
Magister Teknik Pengendalian Pencemaran Lingkungan,
Jurusan Teknik Kimia, Fakultas Teknik UGM
Abstract
Porous carbon material is carbon type which has internal surface area as specific characteristic. One way to produce this material is by pyrolisis using nature or synthetic substance as precursor. Pyrolisis process as describe above, will cause non-carbon atom as composer of polymer substance will disperse and evaporate, this process will left carbon charcoal as residue with specific atom frame structure atom carbon matching with chain structure precursor polymer and building coordinated pore network. Purpose of this research is to get optimum operational condition of pyrolisis process including temperature, remp rate and thermal soak time.
Production process of porous carbon material start by making precursor in the form of phenolic resin by reacting phenol (C6H5OH) and p-tert-butylphenol (C10H14O) with formaldehyde (CH2O) using acid as catalyst. Controlled process parameter in making chain network phenolic resin is catalyst, and type of reactant used in polymeration reaction. By controlling certain parameters as mention above, network of polymer chain formed can be directed as we please. Phenolic resin precursor then pirolised by optimizing operation condition in retort, at temperature about 400-900oC, ramp rate 1,67-10oC/minute, thermal soak time 15-150 minute and activating process using phosphate acid (H3PO4). To know the characteristic of porous carbon material formed, done by undergo adsorption test with nitrogen gas at temperature of 77K (-196oC), Scanning Electron Microscope (SEM) test and iodine number test. From this characterization process, we can see internal surface area, pore size distribution, average pore diameter, strength of liquid adsorption, and visualization of porous carbon material.
Based on result of this research, the optimum temperature for this operation is at 900oC with activation process using phosphate acid, where obtained internal surface area is 2.828 m2/g. The optimum ramp rate is 1,67oC/minute with internal surface area 973 m2/g. From iodine number test is bigger correspond to internal surface area.
Keyword: Porous carbon material, Phenolic resin, Pyrolisis
Intisari
Material karbon berpori adalah tipe karbon yang mempunyai ciri khas adanya luas permukaan internal. Salah satu cara untuk menghasilkan material tersebut, dapat dengan cara melakukan pirolisis menggunakan bahan alam maupun sintetis sebagai prekursor. Proses pirolisis ini akan menyebabkan atom non-karbon penyusun bahan polimer terurai dan menguap sehingga hanya menyisakan arang karbon dengan struktur kerangka atom karbon yang spesifik sesuai dengan struktur rantai polimer prekursor dan membentuk jaringan pori secara teratur. Penelitian ini bertujuan untuk mendapatkan kondisi operasi proses pirolisis yang optimum meliputi suhu, laju kenaikan suhu pemanasan (ramp rate) dan waktu (thermal soak time).
Proses pembuatan material karbon berpori diawali dengan membuat prekursor berupa phenolic resin dengan cara mereaksikan antara fenol (C6H5OH) dan para-tersierbutilfenol (C10H14O) dengan formaldehyde (CH2O) menggunakan katalis asam. Parameter proses yang dikontrol dalam rangka pembentukan jaringan rantai polimer phenolic resin adalah katalis, dan jenis reaktan yang dipergunakan dalam reaksi polimerisasi. Dengan mengendalikan beberapa parameter tersebut, jaringan rantai polimer yang terbentuk dapat diarahkan sesuai dengan yang diinginkan. Prekursor berupa phenolic resin tersebut kemudian dipirolisis dengan melakukan optimasi kondisi operasi dalam retort, pada kisaran suhu 400-900oC, laju kenaikan suhu pemanasan 1,67-10 oC/menit, dan waktu selama 15-150 menit serta melakukan proses aktivasi menggunakan asam fosfat (H3PO4). Untuk mengetahui karakteristik material karbon berpori yang dihasilkan, dilakukan uji adsorpsi dengan gas nitrogen pada suhu 77 K (-196oC), uji Scanning Electron Microscope (SEM) dan uji iodine number. Dari proses karakterisasi ini dapat dilihat luas permukaan internal, distribusi ukuran pori, diameter pori rata-rata, daya serap dalam cairan dan visualisasi material kabon berpori tersebut.
Berdasarkan hasil penelitian suhu operasi yang optimum pada 900oC dengan proses aktifasi menggunakan asam fosfat, dimana diperoleh internal surface area sebesar 2.828 m2/g. Untuk pengaruh laju kenaikan suhu pemanasan dihasilkan kondisi optimum pada 1,67oC/menit dengan internal surface area 973 m2/g. Sedangkan untuk waktu (thermal soak time) diperoleh kondisi operasi optimum pada waktu 90 menit dengan internal surface area 1.196 m2/g. Dari uji iodine number diperoleh hasil semakin besar sesuai internal surface area.
Keywords: Material karbon berpori, Phenolic resin, Pirolisis
Kesimpulan
1. Pada proses optimasi perubahan suhu pirolisis terhadap internal surface area, didapatkan kesimpulan semakin tinggi suhu pirolisis maka internal surface area yang dihasilkan akan semakin besar. Sedangkan diameter
2. Pengaruh laju kenaikan suhu pemanasan (ramp rate) pirolisis terhadap internal surface area adalah dimana semakin lambat laju pemanasan, akan diperoleh internal surface area semakin besar. Hasil penelitian menunjukkan dengan ramp rate paling lambat internal surface area yang dihasilkan adalah 973 m2/g pada 1,67oC/menit. Sedangkan untuk distribusi ukuran
3. Penelitian waktu proses pirolisis (thermal soak time) diperoleh internal surface area terbesar pada thermal soak time 90 menit yaitu sebesar 1.196 m2/g, pada proses ini terlihat kenaikkan internal surface area pada waktu 15-90 menit, selanjutnya mengalami penurunan pada 120 menit dan meningkat lagi pada 150 menit, akan tetapi semakin lama waktu thermal soak time fenomena hysteresis juga tidak terjadi. Jadi semakin lama waktu thermal soak time akan mempengaruhi pembentukan
4. Berdasarkan uji iodine number diperoleh hasil pada suhu 550oC dengan bilangan iodine sebesar 252 mg/g, suhu 650oC (650 mg/g) dan suhu 700oC (839 mg/g). Berdasarkan hasil penelitian terlihat semakin besar internal surface area juga semakin besar pula bilangan iodinenya. Dari hasil uji pada kondisi operasi minimal 650oC sudah dapat digunakan untuk aplikasi pada fase cair dilihat hasil bilangan iodine yang diperoleh diatas 500 mg/g.
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