臺灣博碩士論文加值系統

近五年來正滲透（Forward osmosis，FO）薄膜技術逐漸成熟，以半透膜區隔進流溶液（Feed solution，FS）與高濃度溶質的驅動溶液（Draw solution，DS），透過天然的濃度梯度產生滲透壓差，可在驅動溶液中獲取高品質的濾液。為了克服現有薄膜所面臨的主要問題：濾液通量低與反向溶質擴散現象，本研究旨在於優化複合式正滲透薄膜（Thin film composite FO membrane，TFC-FO）的製備條件，先針對聚碸（Polysulfone，PSf）支撐層的製備因子進行測試，以找出最佳的製備條件；接者針對表面聚醯胺（Polyamide，PA）活性層的製備進行優化，添加二氧化鈦（TiO2）奈米顆粒以提升薄膜的親水性，添加三乙胺（Triethylamine，TEA）與樟腦磺酸（Camphorsulfonic acid，CSA）以增強聚醯胺與聚碸的鍵結強度，提升薄膜的分離成效。接著，了解決正滲透常面臨的反向溶質擴散問題，研究自行開發多片式電正滲透系統，藉由外加電場以有效降低反向溶質擴散通量，同時有效控制膜面積垢，並可隨使用者的需求增家裝設的薄膜片數以提高系統過濾的有效面積。最後，為了瞭解製備薄膜的對微量污染物的分離成效與實際廢水回收效益，本研究應用所開發的薄膜與電滲透系統於個人與醫療保健用品（Pharmaceuticals personal care products，PPCPs）的去除與養殖廢水的回收，以評估製備薄膜與開發電正滲透系統之操作效益。
研究結果顯示，PSf薄膜的良好製備參數包含，環境濕度需控制在30 %，塗佈速度為9 cm/s，塗佈器高度為200 µm，最終至完完成的薄膜需浸泡於去離子水3天；PA層則為MPD（2 wt%）與PSf接觸時間為5分鐘，與TMC（0.15 w/v%）反應時間為1分鐘。以CSA與TEA進行化學改質的薄膜（命名為CT膜），具有最佳的薄膜選擇性（183.3 L/ mole）與良好的結構參數（384 μm）。將0.2 wt.%的105℃乾燥後TiO2（TiO2,d）加入CT膜中（製成的薄膜命名為CT-TiO2,d），能進一步提升水通量至8.1 L/m2h，並降低結構參數至188 μm。所製備的薄膜具有良好的聚醯胺結構，尤其是CT改質膜，對已解離的PPCPs（包含Virgin、TiO2,d、CT、及CT-TiO2,d）因靜電相斥作用，去除率均可高達96.4%以上，而對極高疏水性的Triclosan，通過反萃取實驗證實會其會吸附於薄膜表面而逐漸溶解貫穿導致去除率降低，對以分子態存在於水體當中的中性Carbamazepine，主要以篩分為去除機制，去除率也可高達95.3%。養殖廢水的回收實驗方面，CT-TiO2,d膜具有良好的親水性及抗垢性，在實驗初期表現出最高的水通量（5.07 L/m2 h），長時間測試下的最終累積產水量為361.1 L/m2。
電正滲透系統在陰離子交換膜（Anion exchange membrane，AEM）與陽離子交換膜（Cation exchange membrane，CEM）的組合模式下，外加電場可有效降低反向溶質的擴散通量，在外加1.5 V下也有最好的能源效益（0.108 kWh/m3），故以AEM-CEM組合搭配1.5 V下，使用CT膜對養殖廢水中PPCPs進行分離實驗，除了TRI以外，對其他PPCPs去除率均超過98 %以上，而TRI由於疏水性吸附於薄膜表面上會有溶解貫穿的現象，因此去除率僅有42.2 %。對養殖廢水的過濾實驗，在第1天時除了表現出非常高且穩定的水通量（5.67 L/m2 h），而實驗終止時FS的導電度為14.8 mS/cm，與FO系統（68.9 mS/cm）相差甚遠，這表示電正滲透系統對污染物攔截與反向溶質控制均展現優異的效能，能有效維持薄膜兩側的滲透壓差，穩定水通量，連續測試六天的累積產水量高達711.5 L/m2，能源效益為0.147 kWh/m3，為綠色節能且有效的創新水回收技術。

Forward osmosis (FO) membrane technology has been gradually developed and applied, which uses a semi-permeable membrane to separate the feed solution (FS) and the draw solution (DS) with high concentration of solutes to provide the driving force of concentration gradient. However, the major challenges of applying FO technology are low permeate flux and the occurrence of reverse solute flux. Therefore, we evaluated the key parameters of synthesizing the polysulfone (PSf) support layer and polyamide (PA), respectively, to optimize the performance of thin-film composite FO membranes (TFC-FO). Then ,the TFC-FO were further modified using titanium dioxide (TiO2) to improve surface hydrophilicity, triethylamine (TEA) and camphorsulfonic acid (CSA) to enhance the structural strength of PA and the separation performance. In order to mitigate reverse solute diffusion from DS and membrane fouling, we developed an electric FO module (e-FO) with flexible number of membranes to increase effective membrane area. Finally, the synthesized membrnaes and e-FO system were applied for the removal of pharmaceutical and personal care products (PPCPs) and the recovery of aquaculture wasrewater (AWW) to evaluate membrane separation performance, water recovery rate, and energy efficienty.
After the confirmation of good combination of parameters for preparing PSf and PA layers, respectively, the PA further modified using CSA and TEA (named CT) exhibited the highest membrane selectivity of 183.3 L/mole and favorable structural parameter of 384 μm. Addition of 0.2 wt.% dried TiO2 at 105°C (named TiO2,d) into the CT membrane (named CT-TiO2,d) can further increase the permeate flux to 8.1 L/m2 h and reduce the structural parameter to 188 μm. The PA layers were well formed on each membrane, especially CT, which exhibited very high rejection (> 96.4%) of ionized PPCPs (including Virgin、TiO2,d、CT and CT-TiO2,d) because of electrostatic repulsion, high rejection of neutral carbamazepine because of size exclusion, and low rejection of highly hydrophobic tricolson because of adsorption and penetration through membranes. CT-TiO2,d exhibited the highest hydrophilicity and anti-fouling charactersitics during AWW recovery experiments with the highest permeate flux (5.07 L/m2 h) and water recovery of 361.1 L/m2.
The combination of anion exchange membrane (AEM) and cation exchange membrane (CEM) with applied voltage of 1.5 V can significantly reduce the reverse solute flux in the e-FO system and also had the best energy efficiency (0.108 kWh/m3) among the tested combination of membranes and applied voltages. Applying CT and 1.5 V in the e-FO system with AEM-CEM mode can considerably enhance the rejection of PPCPs to over 98% (except for TRI of 42.2%), exhibited high and stable permeate flux (5.67 L/m2 h) and significantly reduce reverse solute flux during the recovery of AWW compared to the experimental results without the application of external voltage. In the AWW recovery tests continuously operated for 6 days, the water production rate was 711.5 L/m2 with the energy efficiency of 0.147 kW h/m3. Therefore, the e-FO system exhibited excellent rejection of trace pollutants, significant mitigation of reverse solute flux, and is a green, energy-saving, effective, and novel water recovery technology.

摘要 I
Abstract III
致謝 V
目錄 VI
圖目錄 IX
表目錄 XII
符號表 XIII
第一章 緒論 1
1.1研究緣起 1
1.2研究目的 2
第二章 文獻回顧 3
2.1正滲透的原理及應用 3
2.1.1 滲透的原理及應用 3
2.1.2 正滲透的原理與操作方式 5
2.1.3 正滲透技術的應用 7
2.2影響正滲透操作成效的關鍵因子 12
2.2.1 薄膜特性 12
2.2.2 驅動溶液組成 13
2.2.3 濃度極化 16
2.2.4 水質特性 17
2.3 正滲透膜的製備與改質技術 20
2.3.1 相轉換 20
2.3.2 界面聚合（Interfacial polymerization，IP） 24
2.3.3 奈米複合式薄膜(Thin film nanocomposite，TFN) 26
2.4 正滲透膜的分離機制與模式 28
2.4.1 薄膜的分離機制 28
2.4.2 質傳係數與滲透壓計算 29
2.4.3 滲透傳輸預測公式 32
2.5 電解輔助滲透或電正滲透 34
2.5.1 電滲透作用 34
2.5.2 模組開發 36
第三章 研究方法及步驟 39
3.1研究方法 39
3.2實驗材料 40
3.2.1 TFC-FO 製膜材料 40
3.2.2 改質材料 41
3.2.3 污染物篩選 42
3.3實驗設計與步驟 46
3.3.1 PSf支撐層製備 46
3.3.2 PA活性層製備 47
3.3.3 FO模組及操作參數 48
3.3.4 電正滲透操作參數及型號 50
3.4薄膜操作效能與特性分析 51
3.4.1 水通量、反向溶直通量及薄膜選擇性計算 51
3.4.2 水滲透係數、鹽滲透係數計算 52
3.4.3 結構參數計算 53
3.4.4 電正滲透系統之能源消耗（Energy consumption）計算 54
3.4.5 PPCPs去除率及膜面吸附量 55
3.4.6 薄膜特性分析 56
第四章 結果與討論 60
4.1製膜參數優化 60
4.1.1 TFC薄膜孔隙浸潤性對水通量及反向溶質通量之影響 60
4.1.2 不同濕度下配製PSf對水通量及反向溶質通量之影響 61
4.1.3 製備PSf塗佈速度對水通量及反向溶質通量之影響 63
4.1.4 支撐層塗佈器高度對水通量及反向溶質通量之影響 64
4.1.5 PSf相轉換反應時間對水通量及反向溶質通量之影響 65
4.1.6 優化製膜參數小結 66
4.2正滲透薄膜改質 67
4.2.1 添加不同特性之TiO2改質PA活性層 67
4.2.2 添加CSA&TEA改質PA活性層 74
4.2.3 水合處理（Hydration） 83
4.2.4 正滲透薄膜改質小結 84
4.3結構參數與薄膜選擇性 85
4.3.1 結構參數與薄膜選擇性評估薄膜優異性 85
4.3.2 結構參數與薄膜選擇性小結 88
4.4外加電場提升正滲透分離成效 89
4.4.1 BP離子交換膜設置對多片式電正滲透系統之效能影響 89
4.4.2 AEM-CEM離子交換膜設置對多片式電正滲透系統之效能影響 92
4.4.3 電正滲透分離機制確認 95
4.4.4 外加電場提升正滲透分離成效小結 100
4.5實場應用 101
4.5.1 製備薄膜對PPCPs的去除成效 101
4.5.2 製備薄膜對養殖廢水之分離成效 104
4.5.3 電正滲透系統對養殖廢水及PPCPs之分離成效 109
4.5.4 實場應用小結 114
第五章 結論與建議 115
5.1結論 115
5.2建議 117
附錄一 導電度檢量線 118
附錄二 離子層析儀檢量線 119
參考文獻 120

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