系統識別號 | U0002-2405202115384500 |
---|---|
DOI | 10.6846/TKU.2021.00631 |
論文名稱(中文) | 通過優化式非溶劑誘導及快速蒸汽誘導相分離法研究高性能分離膜的綠色製程 |
論文名稱(英文) | Study on the green production of high performance separation membranes by modified NIPS and FVIPS processes |
第三語言論文名稱 | |
校院名稱 | 淡江大學 |
系所名稱(中文) | 化學工程與材料工程學系博士班 |
系所名稱(英文) | Department of Chemical and Materials Engineering |
外國學位學校名稱 | |
外國學位學院名稱 | |
外國學位研究所名稱 | |
學年度 | 109 |
學期 | 2 |
出版年 | 110 |
研究生(中文) | 何兆全 |
研究生(英文) | Chao-Chuan Ho |
學號 | 807400022 |
學位類別 | 博士 |
語言別 | 繁體中文 |
第二語言別 | |
口試日期 | 2021-05-21 |
論文頁數 | 145頁 |
口試委員 |
指導教授
-
鄭廖平(lpcheng@mail.tku.edu.tw)
委員 - 莊曜宇(chuangey@ntu.edu.tw) 委員 - 童國倫(kltung@ntu.edu.tw) 委員 - 張朝欽(ccchang@mail.tku.edu.tw) 委員 - 賴偉淇(wclai@mail.tku.edu.tw) |
關鍵字(中) |
聚醚碸 聚乙烯吡咯烷酮 多孔型薄膜 濕式相轉換法 雙連續結構 聚偏二氟乙烯膜 膜蒸餾 快速蒸汽誘導相分離 |
關鍵字(英) |
Poly(ether sulfone) Polyvinylpyrrolidone Porous Membrane Wet phase inversion method Bi-continuous structure PVDF membrane Membrane distillation FVIPS |
第三語言關鍵字 | |
學科別分類 | |
中文摘要 |
本研究用濕式相轉換法由聚醚碸(PES)/聚乙烯吡咯烷酮(PVP)/γ-丁內酯(GBL)/水製備交穿型多孔薄膜,添加水的研究,膜皆非對稱結構,上表面為緊緻皮層,皮層下為雙連續層,孔隙由小而大,接著是巨孔結構; 隨著水的添加,上表面孔洞數量逐漸增加,膜之純水通量提升,結構中巨孔向下延伸至底部,添加水1.5 phr時,巨孔尺寸大幅縮小型態為孔洞互穿雙連續結構,孔隙度約為77~80 %;上表面接觸角不隨水添加而下降接近74~80。拉伸強度隨水添加量,呈先降後升趨勢。膜用BSA過濾時移除率在70~98%。 添加不同分子量PVP(K15及K30)研究,膜皆非對稱結構,K15比例提升,上表面孔洞的數量及尺寸先升後降,內部結構K5P8時胞孔結構出現,K0P13胞孔佔膜大部分區域,各膜孔隙度約為79%;上表面接觸角約為73%,拉伸強度隨K15提升呈先降後升。純水通量隨K15量增高通量先升後降。膜用Blue dextran過濾時移除率在97-99%範圍。 曝氣時間的研究,膜皆非對稱結構,曝氣時間的增加,上表面孔洞數量及尺寸逐漸增加,結構中巨孔呈縮小趨勢,膜孔隙度為77~78%,上表面接觸角在曝氣3/5/8秒時,介於70~74,過度曝氣表面會開出微米孔洞,接觸角為0。膜拉伸強度落在5.1~5.9 N/mm2。純水通量隨著曝氣時間增長呈上升趨勢。膜作Blue dextran過濾時移除率在97~98%範圍。 通過快速蒸汽誘導相分離(FVIPS)製備用於直接接觸式膜蒸餾(DCMD)脫鹽高度多孔聚偏二氟乙烯(PVDF)疏水對稱平板膜。製膜液由PVDF/磷酸三乙酯(TEP)/水及甘油成分組成,研究聚合物溶解溫度、沉澱槽溫度、甘油添加量及曝氣時間的影響。DCMD通過水循環通量和脫鹽實驗評估膜的滲透性和分離效能。不添加甘油時經過15秒的蒸汽誘導,膜的上表面從不曝氣的緻密光滑變為多孔和粗糙,膜橫截面均保持對稱的雙連續結構。更長蒸汽誘導時間的膜表現出更高的孔隙率,接觸角,厚度和純水通量,拉伸強度小幅度下降。孔徑大小與蒸汽誘導時間的增加無關。 添加甘油會減少開孔所需之曝氣時間及平均孔徑減小。孔隙率,接觸角,厚度隨著曝氣時間的增加而增加。拉伸強度相反。 使用去離子水和鹽水在DCMD測試各種製備疏水膜的性能。 3.5% 鹽水溶液,0.7 L/min循環流量和35 oC的溫差進行操作時,孔徑0.2/0.5/0.6 µm的膜其滲透通量分別為7.87/12.25/14.66 LMH。孔徑0.22和0.45 µm市售膜,通量分別為9.63和10.99 LMH。所有測試膜的脫鹽率均達到約100%。 長時間72小時測試,溫度差為35°C,鹽溶液3.5%,顯示截留率高達99.3%且滲透通量在5小時後達到平穩狀態,表明在進料過程中幾乎沒有潤濕現象。 |
英文摘要 |
In this study, a wet phase inversion method was employed to prepare a highly porous membrane from PES/polyvinylpyrrolidone(PVP)/gamma-butyrolactone(GBL)/water dope solution. In the addition of water dosage, the results showed that the fabricated membranes had an asymmetric structure, with a dense skin layer on the top surface then a bi-continuous layer with orientations from small to large, followed by a macroporous structure. Pores number and size increased with increasing of water content, resulting pure water flux increased. The macropores in the structure was extended to the bottom. With 1.5 phr of water addition, the size of the macropores is reduced and converted into a bi-continuous structure, the porosity is about 77~80%. Upper surface contact angel close to 74~80 , tensile strength drop then up. On BSA filtration removal rate within the range of 70~98%. In the effect PVP (K15 and K30) experiments, the results show membrane had an asymmetric structure. As the ratio of K15 increases, the number and size of pore on the top surface first increase and then decrease. The internal structure at K5P8, the cell structure has appeared, at K0P13, the cells occupy most of the film area, the porosity of each membrane is about 79%, contact angle of the top surface is about 73%, tensile strength with increasing K15, which generally decreases first and increase thereafter , pure water flux as the addition of K15 in the dope solution increased, the flux first rose and then decreased. On Blue dextran filtration removal rate within the range of 97-99%. In the effect exposure time experiments, the results show membranes had an asymmetric structure. With the increase of exposure time, the number and size of pores on the top surface gradually increase. The macropores in the structure was extended to decrease with exposure time, porosity about 77~78%, contact angle of the top surface at 3/5/8 seconds of exposure time is between 70o~74o . Too long exposure time will caused pore size turn to micron size and structure collapses, contact angle close to 0o . The tensile strength falls within 5.1~5.9 N/mm2. The pure water flux increased with increase exposure time. On Blue dextran filtration removal rate within the range of 97~98% . The fast vapor-induced phase separation (FVIPS), a highly porous polyvinylidene fluoride (PVDF) hydrophobic symmetric flat membrane for direct contact membrane distillation desalination (DCMD) was successfully prepared. Tthe effects of polymer dissolution and water bath temperature, addition of glycerin as an additive and exposure time were explored. The DCMD process was used to evaluate the permeability and wettability of the membrane through water flux and desalination experiments. Without adding glycerin, after 15 seconds of steam induction time, the top surface of the membrane changed from dense to porous and rough, the cross-sections of membranes are symmetrical sponge-like structure. The membrane after longer exposure time showed higher porosity, contact angle, thickness and pure water flux, but the tensile strength dropped. The pore size has no big difference with increase exposure time. The addition of glycerin reduces the exposure time and also reduces poze size. The porosity, contact angle, thickness increased and tensile strength decreased with exposure time increases. The fabricated membranes and commercial membranes tested under the DCMD configuration using deionized water and brine. Using 3.5% NaCl, circulation flow of 0.7 L/min and temperature difference of 35 oC for the DCMD process, membranes with pore diameters of 0.2/0.5/0.6 µm, the permeation fluxes for fabricated membranes are 7.87/12.25/14.66 LMH. The commercial membranes with 0.22 and 0.45 um, fluxes were 9.63 and 10.99 LMH, respectively. The salt rejection rate with all membranes reached about 100%. The 72 hours long run test with 3.5% NaCl, temperature different of 35°C, high rejection rate 99.3% and permeate flux reached a plateau after 5 hours, showed that there was hardly any wetting during the DCMD process, and the membrane performs better in desalination than commercial membranes. |
第三語言摘要 | |
論文目次 |
Acknowledgements………………………………………..I 中文提要………………………………………………………..II Abstract…………………………………………………...IV 總目錄………………………………………...............VII 圖目錄…………………………………………..... XI 表目錄………………………………………….... XV 第一章 序論………………………………………… 1 1.1 以優化式非溶劑誘導相分離法製備非對稱型聚醚碸薄膜之配方開發與結構設計………………………………………… 1 1.2 使用快速蒸汽誘導相分離法製備用於膜蒸餾的高度多孔平板聚偏二氟乙烯 (PVDF)薄膜………………………………………… 2 第二章 背景………………………………………… 6 2.1 以優化式非溶劑誘導相分離法製備非對稱型聚醚碸薄膜之配方開發與結構設計………………………………………… 6 2.2 使用快速蒸汽誘導相分離法製備用於薄膜蒸餾的高度多孔平板聚偏二氟乙烯 (PVDF)薄膜………………………………………… 10 2.2.1 直接接觸式薄膜蒸餾 (DCMD)………………………………………… 10 2.2.1.1 質量傳送………………………………………… 11 2.2.1.2 熱傳………………………………………… 12 2.2.1.3 溫度極化係數 (TPC)………………………………………… 13 2.2.1.4 濃度極化對MD性能的影響………………………………………… 13 2.2.2 MD薄膜的要求………………………………………… 14 2.2.3 蒸汽誘導法製作MD薄膜………………………………………… 16 2.2.3.1 溶劑的影響………………………………………… 16 2.2.3.2 添加劑在製膜液中的作用………………………………………… 16 2.2.3.3 曝氣時間的影響………………………………………… 17 2.2.3.4 相對濕度的影響………………………………………… 18 2.2.3.5 溶解溫度的影響………………………………………… 19 2.2.3.6 沉澱槽種類與溫度的影響………………………………………… 19 第三章 實驗方法………………………………………… 20 3.1 化學藥品和材料………………………………………… 20 3.2 薄膜製作………………………………………… 20 3.2.1以優化式非溶劑誘導相分離法製備非對稱型聚醚碸薄膜之配方開發與結構設計………………………………………… 20 3.2.2 使用快速蒸汽誘導相分離法製備用於膜蒸餾的高度多孔平板聚偏二氟乙烯(PVDF)薄膜………………………………………… 22 3.3 薄膜性能………………………………………… 24 3.3.1 聚醚碸薄膜的純水通量及抗垢測試………………………………………… 24 3.3.2 聚偏二氟乙烯薄膜DCMD設置和操作方法………………………………………… 26 3.4 薄膜鑑定 …………………………………………28 第四章 結果與討論………………………………………… 31 4.1 以優化式非溶劑誘導相分離法製備非對稱型聚醚碸薄膜之配方開發與結構設計………………………………………… 31 4.1.1製膜液添加水量之效應………………………………………… 31 4.1.1.1薄膜之孔隙結構………………………………………… 31 4.1.1.2薄膜之物性分析………………………………………… 38 4.1.1.3薄膜中成孔劑PVP之殘留分析………………………………………… 38 4.1.1.4薄膜之拉伸測試………………………………………… 47 4.1.1.5純水通量測試………………………………………… 48 4.1.1.6薄膜之BSA抗垢能力測試………………………………………… 54 4.1.2 PVP分子量效應之探討………………………………………… 57 4.1.2.1薄膜之製備與物性分析………………………………………… 57 4.1.2.2薄膜之Blue dextran 過濾能力測試………………………………………… 79 4.1.3曝氣時間之效應………………………………………… 81 4.1.3.1薄膜之製備與物性分析………………………………………… 81 4.1.3.2薄膜之Blue dextran 過濾能力測試………………………………………… 99 4.2 使用快速蒸汽誘導相分離法製備用於膜蒸餾的高度多孔平板聚偏二氟乙烯(PVDF)薄膜………………………………………… 101 4.2.1 薄膜形態………………………………………… 101 4.2.1.1 聚合物溶解和沉澱槽溫度的影響………………………………………… 101 4.2.1.2 甘油添加的影響………………………………………… 107 4.2.2 薄膜的孔隙率,接觸角度,厚度和機械性能 …………………………………………110 4.2.2.1 聚合物溶解溫度和沉澱槽溫度的影響………………………………………… 110 4.2.2.2 甘油添加的影響………………………………………… 115 4.2.3 DCMD應用中的薄膜性能………………………………………… 118 4.2.3.1 循環流量的影響………………………………………… 118 4.2.3.2 上下游溫差的影響………………………………………… 120 4.2.3.3 NaCl濃度的影響………………………………………… 122 4.2.3.4 長時間操作對淡化期間DCMD性能的影響………………………………………… 124 第五章 結論………………………………………… 126 5.1 以優化式非溶劑誘導相分離法製備非對稱型聚醚碸薄膜之配方開發與結構設計………………………………………… 126 5.2 使用快速蒸汽誘導相分離法製備用於膜蒸餾的高度多孔平板聚偏二氟乙烯(PVDF)薄膜………………………………………… 127 參考文獻………………………………………… 129 圖目錄 圖 1. DCMD裝置中的熱傳和質傳[63]………………………………………… 11 圖 2. 製備PES薄膜之流程………………………………………… 21 圖 3. 不同濃度牛血清白蛋白(BSA)之UV吸收度檢量線.………………………………………… 25 圖 4. 不同濃度藍色葡聚醣(Blue dextran)之UV吸收度檢量線………………………………………… 26 圖 5. DCMD裝置示意圖………………………………………… 28 圖6. PES薄膜上表面之SEM影像圖. (a) K13H0, (b) K13H0.5, (c) K13H1, (d) K13H1.5, (e) K13H1.7 ((a-1)~(e-1)為Image J 分析圖)………………………………………… 34 圖 7. PES薄膜截面之SEM影像圖 (a) K13H0, (b) K13H0.5, (c) K13H1, (d) K13H1.5, (e) K13H1.7………………………………………… 35 圖 8. PES薄膜截面之SEM放大影像圖(a) K13H0, (b) K13H0.5, (c) K13H1, (d) K13H1.5, (e) K13H1.7………………………………………… 36 圖 9. PES薄膜截面之下表面SEM放大影像圖. (a) K13H0, (b) K13H0.5, (c) K13H1, (d) K13H1.5, (e) K13H1.7………………………………………… 37 圖 10. (a)聚醚碸PES與 (b)聚乙烯吡咯烷酮PVP之H-NMR光譜圖 40 圖 11. PES薄膜之H-NMR光譜圖. (a) K13H0, (b) K13H0.5, (c) K13H1, (d) K13H1.5, (e) K13H1.7………………………………………… 43 圖12. PES薄膜之FTIR-ATR光譜圖. (a) K13H0, (b) K13H0.5, (c)K13H1, (d) K13H1.5, (e) K13H1.7………………………………… 46 圖 13. 製膜液中水含量對薄膜拉伸強度作圖………………………………………… 48 圖 14. PES薄膜之純水通量 …………………………………………50 圖 15.PES薄膜之PMI孔徑分佈圖. (a) K13H0, (b) K13H0.5,(c) K13H1, (d) K13H1.5, (e) K13H1.7…………………………………….54 圖 16. PES薄膜過濾BSA之通量隨時間變化圖 ……………………………57 圖 17. PES薄膜上表面之SEM影像圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13 ((a-1)~(e-1)為Image J 分析圖)…………………………61 圖 18. PES薄膜截面之SEM影像圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13………………………………………… 61 圖 19. PES薄膜截面孔洞SEM放大影像圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13…………………………………………62 圖 20. PES薄膜截面之SEM放大影像圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13………………………………………… 63 圖 21. PES薄膜下表面之SEM影像圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13………………………………………… 64 圖 22. PES薄膜之H-NMR光譜圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13………………………………………… 69 圖 23. PES薄膜之FTIR-ATR光譜圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13…..………………………………………… 72 圖 24. 製膜液中K15含量對薄膜拉伸強度作圖……………………………… 74 圖 25. PES薄膜之純水通量………………………………………… 75 圖 26. PES薄膜之PMI孔徑分佈圖. (a) K13P0, (b) K10P3, (c) K8P5, (d) K5P8, (e) K0P13...........………………………………………… 78 圖 27. PES薄膜過濾Blue dextran之通量隨時間變化圖………………………………………… 81 圖 28. PES薄膜上表面之SEM影像圖. (a) K13H0, (b) K13T5, (c) K13T8, (d) K13T11 ((a-1)~(c-1)為Image J 分析圖)…………………………………… 84 圖 29. PES薄膜截面之SEM影像圖. (a) K13H0, (b) K13T5, (c) K13T8, (d) K13T11……………………………………………………………………………….85 圖 30. PES薄膜截面孔洞SEM放大影像圖. (a) K13H0, (b) K13T5, (c) K13T8, (d) K13T11………………………………………… 86 圖 31. PES薄膜截面之SEM放大影像圖. (a) K13H0, (b) K13T5, (c) K13T8, (d) K13T11………………………………………… 87 圖 32. PES薄膜下表面之SEM影像圖. (a) K13H0, (b) K13T5, (c) K13T8, (d) K13T11………………………………………… 88 圖 33. PES薄膜之H-NMR光譜圖. (a) K13T5, (b) K13T8, (c) K13T11………………………………………… 91 圖 34. PES薄膜之FTIR-ATR光譜圖. (a) K13H0, (b) K13T5, (c) K13T8, (d) K13T11 ………………………………………………………………………………94 圖 35. 曝氣時間對薄膜拉伸強度作圖………………………………………… 95 圖 36. PES薄膜之薄膜純水通量………………………………………… 96 圖 37. PES薄膜之PMI孔徑分佈圖. (a) K13T5, (b) K13T8, (c) K13T11………………………………………… 99 圖 38. PES薄膜過濾Blue dextran之通量隨時間變化圖………………………………………… 101 圖 39. 薄膜上表面形態對PVDF/TEP製膜液曝氣時間的依賴性. 放大倍數:10 s = 10k×,15, 25, 及35 s = 2k………………………………………… 103 圖 40. 薄膜下表面形態對PVDF/TEP製膜液曝氣時間的依賴性. 放大倍數 = 2k………………………………………… 104 圖 41. 在70%相對濕度和60 oC下,曝氣不同時間所獲得PVDF膜的SEM圖像(橫截面放大0.5k,插圖放大5k,比例尺顯示實際尺寸) 106 圖 42. PVDF / TEP/甘油系統中,曝氣時間對薄膜上表面形態的影響。放大倍率: M4 與M5 (0,5 s) 為10k, M5 (10,15 s) 與 M6為2k………………………………………… 108 圖 43. PVDF / TEP/甘油系統中,曝氣時間對薄膜下表面形態的影響。放大倍率為2k………………………………………… 109 圖 44. 在70%相對濕度和60 oC下,曝氣不同時間後,所獲得PVDF膜的SEM圖像(橫截面放大0.5k,插圖放大5k,比例尺顯示實際尺寸) …………………………………………110 圖 45. 在各種聚合物溶解和沉澱槽溫度下,曝氣時間對薄膜孔隙率的影響………………………………………… 111 圖 46. 在各種聚合物溶解和沉澱槽溫度下,曝氣時間對薄膜上表面接觸角度的影響………………………………………… 112 圖 47. 在各種聚合物溶解和沉澱槽溫度下,曝氣時間對膜孔隙率的影響………………………………………… 115 圖 48. 在各種聚合物溶解和沉澱槽溫度下,曝氣時間對薄膜上表面接觸角的影響………………………………………… 116 圖 49. 在各種循環流量下,PVDF薄膜之DCMD滲透通量與阻隔率。(A)通量,(B) NaCl阻隔率。實驗參數:進料的氯化鈉溶液= 3.5%,ΔT = 35 oC,滲透測循環流量 = 0.3 L/min………………………………………… 119 圖 50. 在不同的ΔT下,各PVDF薄膜之DCMD滲透通量與阻隔率。 (A)通量 (B)氯化鈉阻隔率。實驗參數:進料的氯化鈉溶液 = 3.5%. 進料側循環流量 = 0.7 L/min. 滲透側循環流量 = 0.3 L/min………………………………………… 121 圖 51. 在各種NaCl濃度下,各PVDF薄膜之DCMD滲透通量與阻隔率。 (A) 通量 (B) 氯化鈉阻隔率。 實驗參數: ΔT = 35℃。進料側循環流量 = 0.7 L/min. 滲透側循環流量 = 0.3 L/min………………………………………… 123 圖 52. PVDF薄膜之DCMD穩定性測試(A)通量(B)NaCl阻隔率 ;實驗參數:ΔT= 35 oC。 進料側循環流量 = 0.7 L/min. 滲透側循環流量 = 0.3 L/min………………………………………… 125 表目錄 表 1. 影響薄膜MD滲透性能之關鍵參數………………………………………… 14 表 2. 製備PES薄膜之製膜液組成………………………………………… 21 表 3. 製備聚偏二氟乙烯(PVDF)薄膜的製膜液條件………………………………………… 23 表 4. PES薄膜之厚度、接觸角、孔隙度、孔洞尺寸及製膜液黏度………………………………………… 32 表 5. 由H-NMR計算所得PVP之殘留率及移除率………………………………………… 39 表 6. PES薄膜之FTIR/ATR上下表面分析………………………………………… 44 表 7. PES薄膜之拉伸強度與伸長率………………………………………… 47 表 8. PES薄膜之純水通量 (LMH)………………………………………… 51 表 9. 不同方式計算所製薄膜表面平均孔徑dma………………………………………… 51 表 10. PES薄膜之BSA過濾測試 …………………………………………55 表 11. PES薄膜過濾BSA之阻力 …………………………………………56 表 12. PES薄膜之厚度、接觸角、孔隙度、孔洞尺寸及製膜液黏度………………………………………… 59 表 13. 由H-NMR計算所得PVP之殘留及移除率………………………………………… 66 表 14. PES薄膜之FTIR/ATR上下表面分析………………………………………… 70 表 15. PES薄膜之拉伸強度與伸長率 …………………………………………73 表 16. PES薄膜之純水通量 (LMH)………………………………………… 75 表 17. 不同方式計算所製薄膜表面平均孔徑dma………………………………………… 76 表 18. PES薄膜之Blue dextran過濾測試 …………………………………………80 表 19. PES薄膜過濾Blue dextran之阻力………………………………………… 80 表 20. PES薄膜之厚度、接觸角、孔隙度、孔洞尺寸及製膜液黏度………………………………………… 83 表 21. 由H-NMR計算所得PVP之殘留率及移除率 …………………………………………89 表 22. PES薄膜之FTIR/ATR上下表面分析…………………………………………92 表 23. PES薄膜之拉伸強度與伸長率………………………………………… 95 表 24. PES薄膜之純水通量 (LMH)………………………………………… 97 表 25. 不同方式計算所製薄膜表面平均孔徑dma.………………………………………… 97 表 26. PES薄膜之Blue dextran過濾測試………………………………………… 100 表 27. PES薄膜過濾Blue dextran之阻力………………………………………… 100 表 28. 通過FVIPS製備的PVDF薄膜的厚度,下表面接觸角,拉伸強度,平均流量孔徑和純水通量………………………………………… 114 表 29. 通過FVIPS加甘油製備的PVDF薄膜的厚度,下表面接觸角,拉伸強度,平均流量孔徑和純水通量………………………………………… 117 |
參考文獻 |
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