臺灣博碩士論文加值系統

電化學群體感應抑制(electrochemical quorum quenching, eQQ)法為一種新型的群體感應抑制方式，已被證明能有效控制薄膜生物反應器(membrane bioreactor, MBR)的生物性阻塞，利用微生物分泌出的訊息分子AHLs (Acyl Homoserine Lactones)具有pH相依性的特性，透過電化學於陰極產生的電子與水做還原產生氫氧根離子，藉此提高生物膜週遭微環境或系統中局部之pH 值，使AHLs分子水解開環成acyl homoserine，喪失群體感應訊息分子的功能。本實驗室先前研究中，以鈦作為陽極能平均延緩一倍的濾膜阻塞時間，過程中發現以鐵作為陽極時會有混凝劑的釋出，造成較大顆粒污泥卡在電極網與濾膜之間，反而加速濾膜的阻塞。
　　因此本研究假設相較於將陰極配置在濾膜附近，在膜表面產生電化學反應生成氫氧根離子，可直接影響附著於濾膜上的生物膜發展，藉由氫氧根離子現地水解微生物所釋出的AHLs分子，進而干擾濾膜細菌的群體感應系統，得以延緩生物膜發展成較成熟、緊密的結構的時程，配合曝氣刮除的動力，應能減少濾膜阻塞的速率。本研究中將實驗分成兩大部分：(1)首先以不同參數、條件製作並優化兩種不同材質的導電膜，接著以電導率、通量、耐久測試評估導電膜的性能，(2)選定一種導電膜進行實驗室規模的連續流MBR試驗，探討在電化學群體感應抑制法中利用導電膜控制濾膜阻塞之成效，並觀察MBR的處理效能是否會受到影響。
　　本研究發現，PVDF中空纖維最佳化學鍍鎳法的導電膜條件為鍍鎳時間2分鐘，可使濾膜表面相距5公分處產生3.8×105 μS/cm電導率，清水通量為204.8 LMH，使用實驗室MBR出流水測試，在膜表面相距3公分處電導率至少為8031 μS/cm並可維持10天，並且鎳析出量極低(0.05 ppm/day)，不過運行於含活性污泥的MBR中，鎳層僅能維持3天，推測微生物可能對鎳層掉落具有一定程度的影響，而改良過後的環狀鍍鎳中空纖維導電膜，在膜表面距離5公分處電導率為2.2×105 μS/cm，並且可於活性污泥中運行15天。PES平板導電膜最佳的條件為添加8%碳黑(CB)及2%聚苯胺(PANI)在製膜溶液中，電導率與通量分別為1.9×104 μS/cm(相距5公分量測值)與219 LMH，其中通量相較於未添加任何導電材料的平板膜提升9.8倍。
本研究首次將PVDF中空纖維導電膜應用於電化學群體感應抑制法中，實驗結果觀察到在連續實驗第一輪和第二輪前半段中分別有94.4%及60.0%的延緩阻塞效率，在濾膜的膜阻抗分析中發現較鬆散的濾餅層為延緩阻塞主要貢獻的來源，且化學鍍鎳程序製成的導電膜及其應用在連續流MBR中，並未對所監測的MBR處理效能產生影響。根據上述結果可知具導電膜之MBR系統具有延緩濾膜阻塞的效果，若能進一步測試並尋求最佳電源供應、槽中濾膜曝氣等操作條件，預期未來將可實際應用於MBR中，以同時達到控制濾膜阻塞、節省能源及處理廢水與回收水資源之目的。

Electrochemical quorum quenching (eQQ) is a novel quorum quenching method, which has been demonstrated as an effective approach for biofouling control in the membrane bioreactor in our laboratory. Signal molecules AHLs (Acyl Homoserine Lactones) secreted by some microorganisms have pH-dependent properties. Hydroxide produced at the cathode through electrochemical approach can increase the pH value of the microenvironment around the biofilm or locally in a MBR system, so that AHLs can be hydrolyzed into acyl homoserine and its fuction in quorum sensing system is inactivated. In the previous research from our laboratory, the use of titanium anode was found to delay fouling of the filter membrane by one time on average. In contrast, it was found that when iron was used as the anode, Fe-coagulant released from anode can cause large sludge to accumulate between the electrode mesh and the filter membrane thus accelerated the fouling rate of the filtrati
on.
This study hypothesizes that the electrochemical reaction conducted on the membrane surface can generate hydroxides and affect the development of the biofilm directly. In situ hydrolysis of AHLs can delay the development of biofilms into a more mature and compact structure. Combined this approach with the scouring from aeration should reduce the rate of membrane fouling. The main objectives of this study are: (1) to fabricate and optimize two types of conductive membranes from different materials. To evaluate different parameters and conditions of manufacturing conductive membranes by measuring its conductivity, flux, and durability, (2) applying one type of the conductive membrane to a laboratory-scale continuous flow MBR, and evaluate the effect of the conductive membrane on biofouling mititgation. Besides, the performance of the MBR will also be monitored to see if the applied process has any adverse affects on the system.
Results showed that the optimum conditions for electroless nickel plating on PVDF hollow fiber are as follows: the nickel plating time is 2 minutes, which can produce 3.8×105 μS/cm conductivity at a distance of 5 cm from the surface of the filter membrane, and the pure water flux is 204.8 LMH. The conductivity at a distance of 3 cm from the membrane surface can last for 10 days with very low nickel release (0.05 ppm/day) in the effluent. However, the nickel layer can only be maintained for 3 days in the activated sludge, it is speculated that microorganisms may have influence on the durability of the nickel layer. The nickel-plating on hollow fiber membrane was further modified into ring-shaped and it can produce 2.2×105 μS/cm conductivity at a distance of 5 cm from the surface of the filter. This type of membrane can be operated in activated sludge for 15 days. The optimum conditions for the conductive flat sheet PES membrane are as follows: 8% carbon black (CB) and 2% polya
niline (PANI) in casting solution. The obtained conductivity and flux are 1.9×104 μS/cm (measured at a distance of 5 cm) and 219 LMH, respectively. The flux is 9.8 times higher than the flat sheet membrane without adding any conductive materials.
This is the first study to use electroless nickel plating on PVDF hollow fiber to study electrochemical quorum quenching in MBR systems. Results in this study showed that there were 94.4% and 60.0% fouling delayed efficiency in the first round and the first half of the second round of experiments, respectively. When analyzed resistance of the fouled membrane, majority of resistance came from loose cake layer. Moreover, the electroless nickel plating conductive membrane did not affect the MBR treatment efficiency. Overall, applying conductive membrane in MBRs should delaying the fouling rate of the membrane. Further testing of operating conditions including both electrical and aerational parameters will be required before this method is practically applied into MBR system in the future to control membrane fouling, save energy, achieve wastewater treatment and reclaim water simultaneously.

第一章 序論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 薄膜生物反應器3
2.1.1 薄膜生物反應器之原理3
2.1.2 薄膜之阻塞與控制3
2.2 群體感應(quorum sensing, QS)系統4
2.2.1 群體感應之原理4
2.2.2 Acyl-homoserine Lactones　5
2.2.3 AHLs 的 pH 相依性5
2.3 群體感應抑制6
2.3.1 群體感應抑制法6
2.3.2 電化學群體感應抑制法7
2.4 導電膜7
2.4.1 導電膜種類與應用7
2.4.2 導電膜的製作方式9
第三章 實驗方法與材料10
3.1 PVDF中空纖維導電膜10
3.1.1 鍍鎳中空纖維導電膜製作10
3.1.2 PVDF中空纖維膜鍍鎳之耐久測試12
3.2 PES平板導電膜12
3.2.1 PES平板導電膜製作12
3.2.2 氧化石墨烯( Graphene oxide, GO)之製備15
3.2.3 粒狀活性碳(Granular activated carbon, GAC)之製備15
3.2.4 粒狀活性炭電極之製備16
3.2.5 聚苯胺(Polyaniline, PANI)之製備16
3.3 導電膜之性能分析法16
3.3.1 電導率16
3.3.2 純水通量17
3.3.3 掃描式電子顯微鏡(Scanning Electron Microscope, SEM)、能量色散X射線譜(Energy-Dispersive X-ray spectroscopy, EDX)17
3.3.4 膜孔隙度17
3.3.5 平均孔洞直徑18
3.4 薄膜生物反應器連續試驗18
3.4.1 濾膜製備18
3.4.2 人工廢水(Synthetic Wastewater)19
3.4.3 薄膜生物反應器19
3.5 實驗分析方法21
3.5.1 水中懸浮固體物(MLSS)21
3.5.2 化學需氧量(COD)21
3.5.3 氨氮、硝酸鹽氮、亞硝酸鹽氮21
3.5.4 膜阻抗分析22
3.6 實驗藥品23
第四章 實驗結果25
4.1 PVDF中空纖維膜鍍鎳之方法測試25
4.1.1 鈀還原方式差異之電導率效果試驗25
4.1.2 評估重複使用氯化鈀溶液對鍍膜效果之影響29
4.1.3 不同薄膜清潔方式之鍍膜效果試驗31
4.1.4 PVDF中空纖維膜鍍鎳之批次實驗36
4.1.5 PVDF中空纖維膜鍍鎳之耐久測試45
4.1.6 PVDF中空纖維膜鍍鎳之優化48
4.2 PES平板導電膜之批次實驗56
4.2.1 氧化石墨烯(GO)參雜之平板導電膜56
4.2.2 活性碳(GAC)電極參雜之平板導電膜60
4.2.3 碳黑(CB)參雜之平板導電膜：63
4.2.4 碳黑(CB)、聚苯胺(PANI)參雜之平板導電膜66
4.3 鍍鎳中空纖維導電膜之連續式實驗74
4.3.1 鍍鎳中空纖維導電膜連續實驗75
4.3.2 處理效能比較82
第五章 結論與建議88
5.1 結論88
5.2 建議89
參考文獻90

圖 2 1 Homeserine lactone訊息分子的不同結構。5
圖 2 2 AHLs的水解變化。6
圖 2 3 C4-HSL的內脂環(lactone ring)的「開環」與「閉環」途徑。菱形為pH值上升的路徑，正方形為pH值下降時的路徑(Yates et al., 2002)。6
圖 3 1 以壓克力管固定之導電膜濾膜模組。18
圖 3 2 薄膜生物反應器系統配置圖。20
圖 4 1 鍍鎳方法一：膜依序浸泡氯化鈀溶液和硼氫化鈉溶液的電導率結果，兩溶液之浸泡時間均為1分鐘或2分鐘。26
圖 4 2 鍍鎳方法二：添加還原劑至氯化鈀溶液中的電導率結果，兩溶液之浸泡時間均為1分鐘或2兩分鐘。26
圖 4 3 圖片中左邊即為氯化鈀溶液，中間為薄膜浸入氯化鈀溶液取出後，再浸泡後之硼氫化鈉溶液(左、中溶液用於方法一)，而右邊為薄膜在浸泡氯化鈀溶液後不取出，直接將硼氫化鈉還原劑添加進氯化鈀溶液的混和液(方法二)。28
圖 4 4 左圖為未使用過的濾膜，中間為經過方法一鈀還原後的濾膜，右邊為鍍鎳後的濾膜。28
圖 4 5 氯化鈀溶液連續使用三次於中空纖維膜鍍鎳的電導率結果，實驗共進行三重複(PdCl2 1-3)，使用之次數以括符內之數字表示。30
圖 4 6 不同的薄膜清潔方式的鍍鎳膜電導率結果。32
圖 4 7 不同的薄膜清潔方式處理後的鍍鎳中空纖維膜之通量結果，通量數據為測試設定在1 bar之透膜壓力下之結果，Original為未鍍鎳的原始乾淨濾膜。33
圖 4 8 僅清潔濾膜表面的鍍鎳導電膜外觀。左圖為使用次氯酸、檸檬酸及中性脫脂溶液清潔，右圖為使用中性脫脂溶液清潔。34
圖 4 9 清潔濾膜表面及內側的鍍鎳導電膜外觀。左圖為使用次氯酸、檸檬酸及中性脫脂溶液清潔，右圖為使用中性脫脂溶液清潔。34
圖 4 10 濾膜經過三個不同氯化鈀溶液浸泡時間(10s、35s、60s)，再搭配三個不同鍍鎳溶液浸泡時間(10s、35s、60s)之條件下的清水膜通量結果，通量數值為透膜壓力設定在1 bar下之結果，Original為未鍍鎳的原始乾淨濾膜。38
圖 4 11 濾膜經過三個不同氯化鈀溶液浸泡時間(10s、35s、60s)，再搭配三個不同鍍鎳溶液浸泡時間(10s、35s、60s)之條件下所完成鍍鎳膜的外觀。39
圖 4 12 濾膜經過三個不同鍍鎳溶液浸泡時間(1 min、2 min、3 min)之條件下的鍍鎳膜電導率結果。41
圖 4 13 濾膜經過三個不同鍍鎳溶液浸泡時間(1 min、2 min、3 min)之條件下的鍍鎳膜通量結果，通量數值為透膜壓力設定在1 bar下之結果，Original為未鍍鎳的原始乾淨濾膜。42
圖 4 14 不同鍍鎳時間之鍍鎳導電膜膜表面及截面之SEM影像圖，(a) blank (b) 鍍鎳1分鐘 (c) 鍍鎳2分鐘 (d) 鍍鎳3分鐘。43
圖 4 15 濾膜經過三個不同鍍鎳溶液浸泡時間(1 min、2 min、3 min)之條件下所完成鍍鎳膜的外觀。44
圖 4 16 鍍鎳膜耐久實驗電導率及陰極分配電壓變化圖。46
圖 4 17 鍍鎳膜耐久實驗鎳含量及占鎳層百分比變化圖。47
圖 4 18 不同鍍鎳時間之鍍鎳導電膜在清水下通量及上升膜壓關係圖(第一輪)。48
圖 4 19 不同鍍鎳時間之鍍鎳導電膜在清水下通量及上升膜壓關係圖(第二輪)。49
圖 4 20 鍍鎳45秒導電膜於反應槽運行之膜壓圖。50
圖 4 21 鍍鎳45秒導電膜於反應槽運行13天後之膜外觀。50
圖 4 22 內掛式小槽及放入反應槽中之外觀。將鍍鎳膜放入內掛式小槽中，底部加裝斜隔板防止曝氣直接影響到濾膜表面，頂部開口使活性污泥溢流進入再從斜隔板底部開口處流出，保持活性污泥的流動。51
圖 4 23 不同鍍鎳時間的導電膜於反應槽中過濾三天前後之膜外觀，(a) 45秒 (b) 1分鐘 (c) 2分鐘 (d) 3分鐘。53
圖 4 24 左圖為改良後的鍍鎳導電膜外觀，右圖為施加1.8V電壓於導電膜10分鐘後，加入酚鈦指示劑的出流水，顏色呈粉紅色。54
圖 4 25 環狀鍍鎳導電膜於反應槽運行15天前後之膜外觀。左圖為運行前、右圖為運行15天後。55
圖 4 26 參雜不同比例的氧化石墨烯(GO)導電膜之外觀，參雜量由左至右分別為0.05、0.01、1%。57
圖 4 27 參雜不同比例的氧化石墨烯(GO)導電膜之電導率結果。58
圖 4 28 參雜不同比例的氧化石墨烯(GO)導電膜之通量結果。59
圖 4 29 參雜活性碳(GAC)電極導電膜之外觀，左圖為orginal活性碳電極，右圖為twice活性碳電極。61
圖 4 30 參雜不同比例的活性碳(GAC)電極導電膜之電導率結果。62
圖 4 31 參雜不同比例的碳黑(CB)導電膜之外觀，由左至右分別為1、5.5、10%。63
圖 4 32 參雜不同比例的碳黑(CB)導電膜之電導率結果。64
圖 4 33 參雜不同比例的碳黑(CB)導電膜之通量結果。65
圖 4 34 參雜不同比例的碳黑(CB)及PANI(聚苯胺導電膜之外觀，(a) CBPblank (b) 2CBP (c) 4CBP (d) 6CBP (e) 8CBP (f) 10CBP (g) 12CBP。68
圖 4 35 參雜不同比例的碳黑(CB)及PANI(聚苯胺)導電膜之電導率及通量結果。69
圖 4 36 參雜不同比例的碳黑(CB)及PANI(聚苯胺)導電膜上表面及截面之SEM影像圖，(a) CBPblank (b) 2CBP (c) 4CBP (d) 6CBP (e) 8CBP (f) 10CBP (g) 12CBP。72
圖 4 37 鍍鎳中空纖維導電膜第一階段連續實驗之透膜壓力變化圖。75
圖 4 38 鍍鎳導電膜連續實驗第二輪之膜外觀。上圖為實驗前、下圖為實驗結束後。78
圖 4 39 連續實驗三輪結束後污泥性質。左圖為團聚、較濃稠的塊狀污泥、中間為污泥沉降比(SV30)、右圖為大量塊狀污泥沉積在反應槽底部。78
圖 4 40 鍍鎳導電膜連續實驗第三輪實驗結束後之膜外觀。左圖為eQQ導電膜、右圖為control導電膜。79
圖 4 41 鍍鎳導電膜連續實驗第一輪之膜阻抗分析圖。80
圖 4 42 鍍鎳導電膜連續實驗第三輪之膜阻抗分析圖。81
圖 4 43 鍍鎳導電膜連續實驗中，eQQ、control、main membrane、anode及MBR的pH值盒鬚圖。**代表p-value < 0.01，存在高度顯著性差異。82
圖 4 44 連續流MBR實驗中陰極槽MLSS濃度變化圖。83
圖 4 45 連續流MBR實驗中人工廢水COD濃度及去除率。83
圖 4 46 連續流MBR實驗中人工廢水及出流水氨氮濃度。84
圖 4 47 連續流MBR實驗中出流水亞硝酸鹽氮濃度。85
圖 4 48 連續流MBR實驗中出流水硝酸鹽氮濃度。85
圖 4 49 連續流MBR實驗中氨氮去除率。86
圖 4 50 連續流MBR實驗中總氮去除率。86

表 3 1 實驗中更改之鈀還原及膜清潔方式整理表。11
表 3 2 實驗中浸泡溶液及鍍鎳時間整理表。12
表 3 3 導電平板膜製膜過程更改處整理表。13
表 3 4 導電平板膜製膜液及電極配方整理表。13
表 3 5 人工廢水成份(Weerasekara et al., 2014)。19
表 3 6 薄膜反應器之操作參數。20
表 3 7 藥品中英文名稱、化學式、廠商及純度對照表。23
表 4 1 不同膜清潔方式的鍍膜導電膜電導率及通量整理。35
表 4 2 濾膜經過三個不同氯化鈀溶液浸泡時間(10s、35s、60s)，再搭配三個不同鍍鎳溶液浸泡時間(10s、35s、60s)之條件下的鍍鎳膜電導率(μS/cm) ( ND：not detected)。37
表 4 3 不同鍍鎳時間之鍍鎳導電膜EDX元素分析結果( ND：not detected)。44
表 4 4 不同鍍鎳時間之鍍鎳導電膜孔徑大小。44
表 4 5 氧化石墨烯(GO)參雜製膜液配方。57
表 4 6 不同比例的氧化石墨烯(GO)參雜之導電膜膜厚度及孔隙度結果。60
表 4 7 活性炭(GAC)電極配方。60
表 4 8 活性炭(GAC)電極製膜液配方。61
表 4 9 碳黑(CB)製膜液配方。63
表 4 10 不同比例的碳黑(CB)參雜之導電膜膜厚度及孔隙度結果。65
表 4 11 碳黑(CB)及聚苯胺(PANI)製膜液配方67
表 4 12 參雜不同比例的碳黑(CB)及PANI(聚苯胺)導電膜之膜厚度、孔隙度及孔徑大小結果。73
表 4 13 鍍鎳中空纖維導電膜第一階段連續實驗之透膜壓力累積率及延緩阻塞百分比。76
表 4 14 連續實驗第一輪膜阻抗分析中透膜壓力原始數值表。80
表 4 15 連續實驗第三輪膜阻抗分析中透膜壓力原始數值表。81

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