Enhancing Downstream Recovery Efficiency in Poly(ethylene 2,5-furandicarboxylate) (PEF) Recycling through pH-Controlled Crystallization of 2,5-Furandicarboxylic Acid (FDCA)

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Title:	Enhancing Downstream Recovery Efficiency in Poly(ethylene 2,5-furandicarboxylate) (PEF) Recycling through pH-Controlled Crystallization of 2,5-Furandicarboxylic Acid (FDCA)
Authors:	李欣珉;Lee, Hsin-Ming
Contributors:	化學工程與材料工程學系
Keywords:	聚(乙烯-2,5-呋喃二甲酸酯);結晶;2,5-呋喃二甲酸;Poly(ethylene 2,5-furandicarboxylate);Crystallization;2,5-Furandicarboxylic Acid
Date:	2025-07-23
Issue Date:	2025-10-17 11:25:50 (UTC+8)
Publisher:	國立中央大學
Abstract:	聚(乙烯-2,5-呋喃二甲酸酯)（ PEF）是一種源自可再生資源的生質聚酯，因其優異的阻隔性能及環境友善特性，被視為可取代石化來源的聚對苯二甲酸乙二酯 PET）的潛力材料。儘管已有許多研究專注於透過水解、醇解或催化程序對PEF 進行化學解聚以回收單體2,5-呋喃二甲酸 FDCA），但對於解聚後的下游處理步驟如結晶、過濾與乾燥的研究仍相對稀少。這些步驟對於提升 PEF 回收製程的能效與可擴展性具有關鍵影響。本研究的目標為透過放大 FDCA 晶體尺寸來提升下游回收效率。實驗中開發了一項控制結晶的方法，於25 °C條件下緩慢滴加硫酸，使結晶過程維持於亞穩定區中，避免快速進入成核區，藉此促進晶體生長並抑制過度成核，進而獲得更大且更易處理的晶體。小規模實驗結果顯示，將滴定頻率由1 ml/min降至每20分鐘1 ml（，可將晶體尺寸由 10 μm提升至60 μm（，整體滴定過程耗時8小時。大規模實驗的規模為小規模的五倍，使用200 ml的 0.6 M NaOH 水溶液、120 ml 的0.6 M H₂SO₄以及 10 g 的PEF。實驗中FDCA的產率達84.6（±（2%（，就是是 10（g的PEF可產生 7.08（g的FDCA（，且其度度為 96（±（2（wt%。放大的晶體顯著提升了下游處理效率，過濾速率提高了2.75倍，而乾燥所需時間則縮短了 1.5 倍（。本方法為優化下游回收條件、降能能耗及提升生質聚合物回收製程的可行性提供了實用策略。整體而言，本研究結果凸顯了整合下游製程設計於PEF回收研究中的重要性，以促進其永續產業化應用。;Poly(ethylene 2,5-furandicarboxylate) (PEF), a bio-based polyester derived from renewable resources, has emerged as a promising alternative to petroleum-based polyethylene terephthalate (PET) due to its superior barrier properties and environmental benefits. While numerous studies have focused on the chemical depolymerization of PEF using hydrolysis, glycolysis, or catalytic processes to recover the monomer 2,5-furandicarboxylic acid (FDCA), limited attention has been given to the downstream processes that follow depolymerization, including crystallization, filtration, and drying. These steps are critical for enabling energy-efficient and scalable recycling of PEF materials. In this study, we aimed to improve downstream recovery efficiency by increasing the size of the crystallized FDCA particles. A controlled crystallization method was developed by slowly titrating sulfuric acid into the system under 25 °C, keeping the crystallization process within the metastable zone rather than rapidly entering the nucleation zone. This approach favors crystal growth over excessive nucleation, resulting in larger and more manageable particles. Experimental results from small-scale crystallization study demonstrated that reducing the titration frequency from 1 ml/min to 1 ml for every 20 min increased the crystal size from approximately 10 μm to 60 μm. The entire process with the addition rate of 1 II ml for every 20 min takes 8 h to complete. The large-scale experiment was conducted at a scale five times greater than that of the small-scale setup. 200 ml of 0.6 M NaOH(aq), 120 ml of 0.6 M H2SO4(aq) and 10 g of PEF was used in the process. In the large-scale experiment, the FDCA yield reached 84.6 ± 2%, indicating that 10 g of PEF produced approximately 7.08 g of FDCA, and the purity of FDCA was 96 ± 2 wt%. The enlarged crystals significantly enhanced downstream processing efficiency, with the filtration rate increased by 2.75 times and the drying time reduced by a factor of 1.5. This method provides a practical strategy to optimize downstream recovery conditions, reduce energy consumption, and improve the scalability of bio-based polymer recycling processes. Overall, the findings highlight the importance of integrating downstream process design into PEF recycling research to support its sustainable industrial application.
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