Zahra, Nikmatuz (2025) Pengembangan Green Process Sintesa Poly Lactic Acid (PLA) Melalui Jalur Ring Opening Polimerisasi (ROP) dengan Bantuan Gelombang Ultrasonic. Doctoral thesis, Institut Teknologi Sepuluh Nopember.
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Abstract
Sintesa Poly Lactic Acid (PLA) umumnya dilakukan melalui metode Ring Opening Polimerisasi (ROP) yang terdiri dari beberapa tahapan yakni dehidrasi, polikondensasi, depolimerisasi, dan polimerisasi. Metode ini membutuhkan kondisi reaksi ekstrem, seperti suhu tinggi, waktu reaksi lama, dan tekanan rendah. Selain itu, proses ini sering kali menggunakan katalis logam seperti tin (II) 2 ethylhexanoate (Sn(Oct)₂), yang berpotensi meninggalkan residu berbahaya. Oleh karena itu, penelitian ini menawarkan pendekatan green process dengan mengombinasikan energi alternatif berupa iradiasi ultrasonik dan penggunaan biokatalis creatinine sebagai alternatif katalis logam. Meskipun kinerja biokatalis belum sebaik katalis logam dalam hal berat molekul akhir, penggunaannya memberikan nilai tambah dari aspek keberlanjutan dan keamanan lingkungan. Penelitian ini bertujuan untuk mendapatkan kondisi optimum pada tahap dehidrasi dan polimerisasi dengan iradiasi gelombang ultrasonik menggunakan pendekatan statistik Response Surface Methodology (RSM), membandingkan efisiensi proses sintesis PLA antara metode konvensional dan metode berbasis ultrasonik termasuk konsumsi energinya, mempelajari karakteristik PLA yang disintesis menggunakan biokatalis creatinine, mengevaluasi pengaruh penambahan co-inisiator terhadap hasil akhir PLA, serta memperbaiki sifat mekanik PLA melalui modifikasi material. Optimasi proses dilakukan menggunakan RSM dengan Central Composite Design (CCD). Tahap dehidrasi menghasilkan kondisi optimum pada waktu 98,852 menit dan daya 109,6 watt, menghasilkan asam laktat dengan kadar air rendah sebesar 1,9858%. Proses ROP menggunakan katalis logam Sn(Oct)₂ dengan bantuan ultrasonik menunjukkan kondisi optimum pada waktu 3,66 jam dan daya 99,29 watt, menghasilkan PLA dengan berat molekul hingga 88.184,32 g/mol, kristalinitas 44,76%, dan suhu leleh (Tm) 165,64°C. Sementara itu, penggunaan creatinine sebagai biokatalis (2%) selama 5 jam menghasilkan PLA dengan yield 90,24%, berat molekul 30.855,12 g/mol, kristalinitas 27,68%, dan suhu leleh 126,67°C. Penambahan metanol sebagai co-inisiator dalam rasio 1,5:100 meningkatkan hasil menjadi yield optimum 92,03%, berat molekul 50.472,20 g/mol, suhu leleh 148,64°C, dan kristalinitas 38,4%. Hasil penelitian ini menunjukkan bahwa integrasi iradiasi ultrasonik, biokatalis, dan co-initiator tidak hanya meningkatkan efisiensi sintesis PLA, tetapi juga mendukung arah pengembangan proses yang lebih hijau dan berkelanjutan.
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The synthesis of Poly Lactic Acid (PLA) is commonly carried out through the Ring Opening Polymerization (ROP) method, which involves several stages, namely dehydration, polycondensation, depolymerization, and polymerization. This method requires extreme reaction conditions, such as high temperatures, long reaction times, and low pressure. In addition, it often employs metal catalysts such as tin(II) 2-ethylhexanoate (Sn(Oct)₂), which may leave hazardous residues. Therefore, this study proposes a green process approach by combining alternative energy through ultrasonic wave irradiation and the use of creatinine biocatalyst as an alternative to metal catalysts. Although the performance of the biocatalyst is not yet as effective as that of metal catalysts in terms of final molecular weight, its use offers added value from the perspective of sustainability and environmental safety. This research aims to determine the optimum conditions in the dehydration and polymerization stages using ultrasonic irradiation based on a statistical approach, the Response Surface Methodology (RSM); to compare the synthesis efficiency between conventional and ultrasound-assisted methods, including energy consumption; to investigate the characteristics of PLA synthesized using creatinine biocatalyst; to evaluate the effect of co-initiator addition on the final PLA product; and to improve PLA’s mechanical properties through material modification. Process optimization was conducted using RSM with a Central Composite Design (CCD). The dehydration stage yielded optimum conditions at 98.852 minutes and 109.6 watts, resulting in lactic acid with a low moisture content of 1.9858%. The ROP process using the metal catalyst Sn(Oct)₂ under ultrasonic assistance showed optimum conditions at 3.66 hours and 99.29 watts, producing PLA with a molecular weight of up to 88,184.32 g/mol, crystallinity of 44.76%, and melting temperature (Tm) of 165.64°C. Meanwhile, the use of creatinine as a 2% biocatalyst for 5 hours yielded PLA with a yield of 90.24%, molecular weight of 30,855.12 g/mol, crystallinity of 27.68%, and melting temperature of 126.67°C. The addition of methanol as a co-initiator at a 1.5:100 ratio increased the yield to 92.03%, with a molecular weight of 50,472.20 g/mol, melting temperature of 148.64°C, and crystallinity of 38.4%. These findings indicate that the integration of ultrasonic irradiation, biocatalysts, and co-initiators not only improves the efficiency of PLA synthesis but also supports the development of a greener and more sustainable process.
| Item Type: | Thesis (Doctoral) |
|---|---|
| Uncontrolled Keywords: | Biokatalis Creatinine, Biokomposit film, Irradiasi Ultrasonik, Poly Lactic Acid, Ring Opening Polimerization. Creatinine Biocatalyst, Film Biocomposite, Ultrasonic Irradiation, Poly Lactic Acid, Ring Opening Polymerization. |
| Subjects: | T Technology > TP Chemical technology > TP1140 Polymers T Technology > TP Chemical technology > TP155.7 Chemical processes. T Technology > TP Chemical technology > TP248.3 Biochemical engineering. Bioprocess engineering |
| Divisions: | Faculty of Industrial Technology and Systems Engineering (INDSYS) > Chemical Engineering > 24001-(S3) PhD Thesis |
| Depositing User: | Nikmatuz Zahra |
| Date Deposited: | 05 Aug 2025 03:21 |
| Last Modified: | 05 Aug 2025 03:21 |
| URI: | http://repository.its.ac.id/id/eprint/126388 |
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