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Pengaruh Komposisi Bahan, Tekanan Jurnal Keramik dan Gelas Indonesia Vol.29 No.2 Desember 2020 : 82 - 91 SINTESIS DIKALSIUM FOSFAT ANHIDRAT UNTUK PREKURSOR BAHAN KERAMIK APATIT DARI BAHAN ALAM Synthesis of Anhydrous Dicalcium Phosphate for Precursor of Natural Ceramic Apatite Material M. Syaifun Nizar*, M. Syaifun Nizar*, Rizky Berliana W*, Kristanto Wahyudi* *) Kontributor Utama, **) Kontributor Anggota Balai Besar Keramik Jln. Jend Ahmad Yani No 392, Bandung, Indonesia Naskah masuk : 26 November 2020, Revisi: 30 Desember 2020, Diterima: 11 januari 2021 ABSTRAK ahan dikalsium fosfat merupakan salah satu bahan apatit yang digunakan untuk prekursor pembuatan bahan apatit lain seperti trikalsium B fosfat, tetrakalsium fosfat, dan hidroksiapatit. Bahan apatit tersebut memiliki kegunaan yang cukup luas di bidang medis dan industri farmasi. Penelitian ini bertujuan untuk menyiapkan bahan dikalsium fosfat dari bahan baku mineral kapur alam dengan metode yang mudah diterapkan untuk skala produksi industri. Dikalsium fosfat dibuat dengan cara presipitasi basah pencampuran asam fosfat dan slaked lime atau kalsium hidroksida dengan pengaturan suhu reaksi sekitar 60⁰C dan pH 3-4 dan pengeringan dilakukan pada suhu sekitar 180⁰C. Bahan yang dihasilkan diuji kandungan mineral dengan XRD dan EDX. Perhitungan semi kuantitatif bahan hasil sintesis mengandung lebih dari 90% dikalsium fosfat anhidrat, sisanya adalah mineral apatit lain. Bahan dikalsium fosfat ini sudah bisa digunakan sebagai prekursor pembuatan bahan apatit . Kata Kunci: kapur, asam fosfat, apatit, dikalsium fosfat anhidrat, prekursor ABSTRACT icalcium phosphate is one of the apatite materials used for precursors to synthesize other apatite D materials such as tricalcium phosphate, tetracalcium phosphate, and hydroxyapatite. Apatite materials are widely used in the medical field and pharmaceutical industry. This study aims to prepare dicalcium phosphate from natural limestone as a precursor for apatite with an easy-to-apply method for industrial scale. Wet precipitation process was performed to prepare dicalcium phosphate from phosphoric acid and slaked lime or calcium hydroxide with reaction temperature control at around 60⁰C and at pH of 3-4, then drying is carried out at about 180⁰C. The product is characterized for its mineral content by XRD and EDX. Semi-quantitative calculation of the synthesized material 82 Sintesis Dikalsium Fosfat Anhidrat..... M. Syaifun Nizar, dkk contains more than 90% dicalcium phosphate andhydrous, the rest is other apatite minerals. It can be used as a precursor for apatite production. Keywords: slaked lime, phosphoric acid ,apatite, dicalcium phosphate anhydrous, precursor. I. PENDAHULUAN menghasilkan nilai tambah yang tinggi Dikalsium fosfat anhidrat (DCPA) karena saat ini di Indonesia merupakan salah satu keluarga permintaan untuk bahan biomaterial senyawa apatit. Bahan apatit lainnya dan fine chemical untuk farmasi masih yaitu trikalsium fosfat, tetrakalsium ketergantungan dari bahan impor [5]. fosfat dan hidroksiapatit [1]. Bahan dikalsium fosfat digunakan Penggunaan bahan tersebut di dunia untuk industri pangan, kimia, medis medis dan farmasi saat ini sudah dan farmasi, akan tetapi aplikasi yang cukup luas, misalnya untuk bahan menunjukkan peningkatan nilai semen tulang, scaffold tulang, tambah yang signifikan adalah untuk pembuatan tulang buatan, obat, dan keperluan medis dan farmasi. Maka juga drug carrier [2]. Beberapa semen dari itu perlu dikembangkan teknologi gigi dan scaffold menggunakan bahan yang sesuai untuk mengembangkan dikalsium fosfat sebagai salah satu industri medis dan farmasi berbasis komponennya bersamaan dengan kapur yang menghasilkan bahan- komponen apatit lain karena memiliki bahan dengan taraf sesuai standar karakteristik bio-resorbable yang tinggi medis dan farmasi. sehingga bersifat bio-kompatibel dan Senyawa dikalsium fosfat memiliki juga osteo-kompatibel [3][4]. Di perbandingan Ca/P 1:1, sehingga industri farmasi, bahan dikalsium bahan ini dapat digunakan sebagai fosfat digunakan sebagai perekat dan prekursor senyawa apatit lain dengan pengisi pada tablet dan kapsul. cara menambahkan kadar kalsium Batu kapur yang melimpah di agar memiliki perbandingan molar Indonesia berpotensi sebagai bahan lebih tinggi dari Ca/P 1:1 yang sesuai baku untuk sintesis material yang dengan senyawa apatit yang digunakan pada industri biomaterial diinginkan [6]. Teknologi pembuatan dan farmasi. Pengolahannya produk apatit sebelumnya 83 Jurnal Keramik dan Gelas Indonesia Vol.29 No.2 Desember 2020 : 82 - 91 menggunakan umpan bahan baku ke menyiapkan teknologi pembuatan dalam reaktor yang berbeda-beda prekursor DCPA sebagai bahan dasar untuk setiap produk apatit, sedangkan untuk pembuatan bahan apatit lain dengan menerapkan teknologi pada dengan penyederhanaan teknologi tulisan ini umpan bahan baku biasa sintesis yang sudah ada, dimana dibuat sederhana atau hanya satu teknologi sebelumnya bahan baku macam saja akan tetapi keluaran apatit dapat berbeda-beda garam produk apatit bisa bervariasi, untuk kalsium dan sumber fosfatnya untuk membuat produk apatit dibuat dengan tiap produk apatit yang berbeda, yaitu satu alur jalur produksi yang unik penyederhanaan sumber bahan baku untuk setiap produk. Teknologi ini untuk membuat prekursor yang bisa tidak hanya menghasilkan satu jenis diolah untuk sintesis produk apatit lain bahan, akan tetapi mendorong sehingga line produksi pembuatan terciptanya industri bahan-bahan apatit dapat dibuat paralel untuk dapat medis dan farmasi yang lain [7]. membuat berbagai macam produk Bahan dikalsium fosfat merupakan apatit berbeda dengan teknologi saat salah satu bahan dasar yang dapat ini dengan line produksi satu produk dijadikan prekursor untuk bahan fine apatit satu line produksi. chemical berbasis kapur atau bahan II. METODOLOGI PENELITIAN apatit. Dengan mengatur proses produksi yang dimodifikasi sesuai Bahan yang digunakan untuk dengan kebutuhan, teknologi pembuatan dikalsium fosfat adalah pembuatan dikalsium fosfat ini dapat slaked lime dari kapur alam yang dijadikan landasan untuk pembuatan berasal dari Cirebon dan Padalarang bahan apatit lain [7]. Masing-masing dengan kemurnian diatas 68% kadar bahan apatit tersebut memiliki fungsi berat, dan asam fosfat teknis dengan dan karakterstik yang berbeda-beda kadar 85% berat. Bahan slaked lime yang dapat digunakan sesuai dengan diukur kadar air untuk menentukan kebutuhan aplikasi yang akan jumlah perbandingan mol jumlah asam diterapkan akan tetapi proses dasar fosfat yang akan dicampurkan. Rata- pembuatannya secara garis besar rata pengukuran kadar air slaked lime dapat dihimpun dan dikelompokan berkisar antara 68-77% menjadi dasar sesuai dengan keperluan. Tujuan dari perhitungan jumlah asam fosfat yang penelitian ini adalah untuk akan dipakai. Asam fosfat yang dipakai 84 Sintesis Dikalsium Fosfat Anhidrat..... M. Syaifun Nizar, dkk memiliki kadar 85% berat yang Setelah kering bahan tersebut diayak diencerkan dengan akuades menjadi 4 sampai dengan 200 mesh. kali volume. Jumlah mol kalsium dan Reaksi kimia pada saat titrasi fosfat dihitung dengan perbandingan adalah sebagai berikut : Ca/P 1:1. Kalsium hidroksida H3PO4 + Ca(OH)2 → CaHPO4↓+ 2H2O [10] dicampurkan dengan asam fosfat Produk reaksi tersebut dikarakterisasi dengan cara titrasi asam fosfat dengan menggunakan X-ray diffraction untuk kecepatan yang lambat, reaksi titrasi melihat fasa mineral dan menghitung ini terjadi proses presipitasi basah secara semi kuantitatif kadar dikalsium pada suhu 60oC-80oC [8] pH 3-4 dan fosfat. Uji Energy Dispersive X-ray 10-11 [9] dengan pengadukan selama dilakukan untuk mengetahui 6 jam. Setelah diaduk, campuran perbandingan Ca/P bahan dikalsium tersebut diendapkan selama 12 jam fosfat hasil sintesis. Sampel bahan lalu dikeringkan pada suhu 180oC. DCPA komersial diuji juga sebagai perbandingan. Gambar 1. Diagram alur proses pembuatan dikalsium fosfat pada temperatur 180oC tanpa III. HASIL DAN PEMBAHASAN dicampur dengan asam fosfat sebagai Sampel nomor 1 adalah sampel sampel kontrol, untuk melihat kalsium hidroksida yang dikeringkan perubahan kandungan bahan kalsium 85 Jurnal Keramik dan Gelas Indonesia Vol.29 No.2 Desember 2020 : 82 - 91 yang dipanaskan dan juga melihat menggunakan pendekatan semi perubahan kalsium hidroksida yang kuantitatif metode Rietvield dari berubah menjadi CaCO3. Pada Tabel difraktogram XRD. 1 dihitung kandungan mineralnya Tabel 1. Hasil perhitungan semi-kuantitatif XRD. Kuantitas Fasa Mineral (% berat) No Sampel CaCO3 CaOH2 DCPD DCPA CaO 1 63,05 35,34 0,75 0,55 0,3 2 60,00 38,00 1,00 1,00 - 3 45,61 52,10 1,86 0,49 - 4 - 0,16 1,41 98,23 - Sampel no 1 mengandung fasa hidrat 2H2O yang akan hilang karena kalsit 63,05% karena bahan kalsium pemanasan menjadi dikalsium fosfat hidroksida kehilangan air sehingga anhidrat. Struktur kristal keduanya berubah menjadi kalsit. Fasa kalsium berbeda, dikalsium fosfat dihidrat hidroksida masih tersisa sebanyak berstruktur kristal monoklinik 35,34%. Proses pengeringan dapat sedangkan dikalsium fosfat anhidrat mengurangi kadar air cukup signifikan. berstruktur triklinik. Oleh karena itu, Analisis sampel kontrol ini untuk keduanya memiliki difraktogram XRD melihat perbandingan apakah ada yang berbeda. kalsium hidroksida yang tersisa pada Sampel No.3 merupakan hasil sampel yang dicampur dengan asam sintesis dari campuran perbandingan fosfat. mol sesuai stoikiometri Ca/P 1:1, pH Sampel nomor 2 merupakan yang terukur pada akhir reaksi sekitar sampel komersial dikalsium fosfat. 10-11 atau bersifat basa. Pada Tabel 1 Sampel ini diuji untuk melihat
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