HUDA, IHSANUL (2020) SINTESIS KALSIUM PIROFOSPAT DARI CANGKANG TELUR MENGGUNAKAN METODE SOLVOTHERMAL DAN KESTABILANNYA PADA SUHU TINGGI. S2 thesis, Universitas Mercu Buana Jakarta.
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Abstract
Calcium pyrophosphate (CPP) has been successfully synthesized using the solvothermal method. The basic ingredients used are chicken and duck eggshell waste. Chicken and duck eggshells are cleaned and crushed, then calcined at 1000 °C for 2 hours to obtain powder with a CaO phase. CaO powder is then mixed with H3PO4 and put into a solvothermal vessel. The solvothermal process is carried out at 130 °C for 16 hours. The single phase CaHPO4 is obtained after the solvothermal process. CaHPO4 powder was calcined in muffle furnaces with a temperature of 800 °C for 2 hours and normal atmospheric conditions. The results of the phase analysis show the formation of the CPP single phase in the absence of other impurities. These results indicate the ratio of Ca and P is 1. Improving the mechanical properties of CPP can be done by adding zirconia (Zr) material. The composition of CPP and zirconia was 95 or 90 and 5 or 10 wt.%, respectively. The mixing of these powder was carried out using High Energy Milling (HEM) with ball to powder ratio (BPR) was 5 for 30 minutes. After that, the mixed powder was heated at 1000 ℃ for 60 minutes. The results of characterization using X-ray Diffraction showed that heating treatment decomposes CPP, which indicated by the formation of CaZrO3. Moreover, the particle size of CPP with the addition of Zr increased significantly. The SEM results show the CPP microstructure size of chicken eggshell (TA) which was originally 590 ± 43 nm to CPP TAZ5 1.212 ± 268 nm and CPP TAZ10 1.324 ± 384 nm. Where as for CPP from duck eggshell (TB), which was originally 455 ± 32 nm to TBZ5 CPP 1.112 ± 546 nm and TBZ10 CPP 1.123 ± 392 nm. Further studies are needed to obtain the optimum conditions of the solvothermal process of eggshell waste and heating accordingly so as not to change the chemical composition of CPP so that modification of CPP- can be achieved. Keywords: Calcium Pirofospat, Solvothermal, Zirconia, High Energy Milling Kalsium pirofospat (CPP) telah berhasil disintesis dengan menggunakan metode solvothermal. Bahan dasar yang digunakan adalah limbah cangkang telur ayam dan bebek. Cangkang telur ayam dan bebek dibersihkan dan digerus, kemudian dikalsinasi pada temperatur 1000°C selama 2 jam untuk mendapatkan serbuk dengan fasa CaO. Serbuk CaO kemudian dicampurkan dengan H3PO4 dan dimasukkan ke dalam bejana solvothermal. Proses solvothermal dilakukan pada temperatur 130°C selama 16 jam. Fasa tunggal CaHPO4 diperoleh setelah proses solvothermal. Pemanasan serbuk CaHPO4 dilakukan pada tungku muffle dengan temperatur 800°C selama 2 jam dan kondisi atmosfir biasa. Hasil analisa fasa menunjukkan terbentuknya fasa tunggal CPP tanpa adanya fasa pengotor lainnya. Hasil ini menunjukkan perbandingan Ca dan P adalah 1. Peningkatan sifat mekanik CPP dapat dilakukan dengan menambahkan material zirkonia (Z). Komposisi zirkonia yang ditambahkan sebesar 5% dan 10% (w/w). Pencampuran CPP dilakukan menggunakan High Energy Milling (HEM) dengan Ball Powder Ratio (BPR) sebesar 5:1 selama 30 menit. Campuran selanjutnya dipanaskan pada temperatur 1000 selama 60 menit. Hasil karakterisasi menggunakan X-ray Diffraction menunjukkan bahwa perlakuan pemanasan dapat mendekomposisi CPP dan terbentuknya CaZrO3. Pemanasan juga menyebabkan ukuran partikel semakin besar. Hasil SEM menunjukkan ukuran mikrostruktur CPP dari cangkang telur ayam (TA) yang semula 590±43 nm menjadi CPP TAZ5 1.212±268 nm dan CPP TAZ10 1.324±384 nm. Sedangkan untuk CPP dari cangkang telur bebek (TB) yang semula 455±32 nm menjadi CPP TBZ5 1.112±546 nm dan CPP TBZ10 1.123±392 nm. Studi lebih lanjut diperlukan untuk mendapatkan kondisi optimum dari proses solvothermal limbah cangkang telur dan pemanasan yang sesuai supaya tidak merubah komposisi kimia pada CPP agar dalam memodifikasi CPP- bisa tercapai. Kata kunci: Kalsium Pirofospat, Solvothermal, Zirkonia, High Energy Milling
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