傳統電解水的陽極析氧反應（OER）因為動力學較慢且過電位高，加上產物氧氣缺乏經濟價值，限制了整體的電能轉換效率。若改用 5-羥甲基糠醛（HMF）的電催化氧化反應（HMFOR）來取代 OER，能有效降低反應電位，並在陽極得到高附加價值的樹脂前驅物 2，5-呋喃二甲酸（FDCA）。不過，常見的 H 型電解槽屬於批次反應，溶液沒有流動導致質傳效果較差，無法在高電流密度下操作，為了解決批次系統的限制，本研究改採用流動式反應器進行反應。 本研究製備出 NiCoP@CoFeLDH 複合電極。製備步驟先將泡沫鎳基材進行滾壓，接著利用水熱法與高溫磷化程序在泡沫鎳表面成核 NiCoP，最後在表面電鍍一層 CoFe LDH，形成 n-n 型異質接面。結構上結合導電性佳的 NiCoP 基底與具備層狀結構的 CoFe LDH，這種異質結構不僅能防止奈米片層相互堆疊，增加活性位點的暴露面積，也能降低電荷傳遞阻抗，更快速的傳輸電子。 在流動槽系統中通電至 120 C 時，NiCoP@CoFeLDH 的 HMF 轉化率與 FDCA 產率分別為 92% 與 75.6%，表現優於純 NiCoP、Pre-NiCoP 與 CoFeLDH。主要是觸媒藉由NiCoP與 CoFeLDH的相互作來降低活化能，改善反應初期的表面結構轉換，並加快最後一步醛基轉變為羧基的反應速度，讓中間產物能連續氧化。另外，陰離子交換膜的選擇也會影響催化表現，相較於具補強網格的 F-75 膜，改用具親水通道的 A-80 均相膜，使 HMF 轉化率與 FDCA 產率分別提升了 30.1% 與 34.2%，並能降低系統阻抗與減少 HMF 熱降解等副反應。 本研究透過觸媒的設計與流動式反應器的搭配，改善了系統的反應速率與質傳限制。在參數調整方面，本研究藉由調降 pH 值有效抑制腐殖質生成以提升碳平衡，並配合進料濃度與流速的調整改善質傳限制，以提升法拉第效率。;The anode oxygen evolution reaction (OER) in traditional water electrolysis suffers from sluggish kinetics， high overpotentials， and low-value products， which limit overall energy conversion efficiency. Replacing OER with 5-hydroxymethylfurfural oxidation (HMFOR) effectively reduces the reaction potential while producing a high-value resin precursor， 2，5-furandicarboxylic acid (FDCA)， at the anode. However， conventional H-type electrolytic cells suffer from poor mass transfer due to their batch reaction nature， restricting high-current-density operations. To overcome these limitations， this study utilizes a flow-cell reactor. In this study， a NiCoP@CoFeLDH composite electrode was fabricated. The preparation involved rolling a nickel foam substrate， nucleating NiCoP via hydrothermal and high-temperature phosphorization processes， and finally electrodepositing a layer of CoFe layered double hydroxide (LDH) to form an n-n heterojunction. This heterostructure effectively combines the highly conductive NiCoP substrate with the layered CoFe LDH. It not only prevents nanosheet restacking and increases the exposed area of active sites， but also reduces charge transfer resistance for faster electron transport. In the flow-cell system， passing a charge of 120 C through the NiCoP@CoFeLDH electrode achieved an HMF conversion of 92% and an FDCA yield of 75.6%， outperforming pure NiCoP， Pre-NiCoP， and CoFeLDH. This excellent performance is mainly attributed to the synergistic interaction between NiCoP and CoFeLDH. This synergy lowers the activation energy， facilitates surface structural transformation at the initial reaction stage， and accelerates the final oxidation step from an aldehyde group to a carboxyl group， enabling the continuous oxidation of intermediates. Furthermore， the choice of anion exchange membrane significantly impacted catalytic performance. Compared to the mesh-reinforced F-75 membrane， using the A-80 homogeneous membrane with hydrophilic channels increased HMF conversion and FDCA yield by 30.1% and 34.2%， respectively. It also lowered system resistance and reduced side reactions like HMF thermal degradation. Overall， combining the rationally designed catalyst with the flow-cell reactor successfully improved the reaction rate and mitigated mass transfer limits. Through parameter optimization， decreasing the pH effectively suppressed humin formation to enhance the carbon balance， while adjusting the feed concentration and flow rate further overcame mass transfer limitations to boost Faradaic efficiency.
