臺灣博碩士論文加值系統

摘要
本研究藉由界面聚合程序製備高效能二氧化碳促進傳輸薄膜。並使用界面活性劑改質基材膜之表面親水性，最後藉由塗佈Pebax以填補聚合層之缺陷並改善複合膜之親水性與二氧化碳親和性。
本實驗使用ethylenediamine (EDA)、triethylenetetramine (TETA)以及 pentaethylenehexamine (PEHA)作為水相單體，trimesoyl chloride (TMC)作為有機相單體，並使用非對稱結構polysulfone (PSf)作為基材，再由Ethylenediamine tetrakis (propoxylate-B-ethoxylate)改善基材膜之親水性，製備改質PSf基材膜(mPSf)，藉由界面聚合方式製備固定載體式的二氧化碳促進傳輸超薄複合薄膜。再以旋轉塗佈方式將Pebax1657®塗佈於界面聚合層之上以改善薄膜分離效能。並探討界面聚合條件(水相及有機相濃度、水相浸泡時間、有機相反應時間以及水相單體結構變化)以及進料氣體壓力變化對於分離效能影響，進而探討水氣引入薄膜結構內對於促進傳輸機制之影響以及混和氣體操作下分離效能之變化。
本研究使用衰減式全反射(ATR-FTIR)傅立葉紅外光譜儀、場發射掃描式電子顯微鏡(FESEM)、水接觸角量測儀、可變單一能量慢速正電子束分析儀 (VMSPB)以及氣體吸附測試來瞭解薄膜結構特性以及表面親疏水性。
經由氣體分離效能實驗結果顯示，界面聚合條件變化主要影響聚合層厚度以及胺官能基含量，而在浸泡0.1M 水相單體1分鐘並與0.001M 有機相單體反應1分鐘時有最佳的氣體分離效能。在最佳的界面聚合條件下所製備之Pebax/EDA-TMC/mPSf複合薄膜於進料壓力為1bar操作溫度為50℃的濕潤環境下，有最佳二氧化碳透過係數為52.98GPU，而二氧化碳/氮氣選擇性為157.7；相較之下，使用含有六胺的PEHA製備複合薄膜，Pebax/PEHA-TMC/mPSf，並於相同操作條件下則具有二氧化碳透過係數為134.2GPU，而二氧化碳/氮氣選擇性為113.5。當進料壓力下降至0.1bar，並於50℃的濕潤環境下進行氣體分離測試，Pebax/PEHA-TMC/mPSf複合薄膜之二氧化碳透過係數可提升為728.9GPU，而二氧化碳/氮氣選擇性則會上升為273.2，其原因在於高壓操作下造成載體飽和而降低了二氧化碳分離效能。在混和氣體操作環境下，會因為競爭吸附而使分離效能明顯下降。

Abstract
In this study, the CO2-selective PA TFC membranes with fixed-site carrier were prepared via the interfacial polymerization of water-soluble amine monomers including ethylenediamine (EDA), triethylenetetramine (TETA) and pentaethylenehexamine (PEHA) with acyl chloride monomer trimesoyl chloride (TMC) on the surface of asymmetric modified polysulfone (mPSf) membranes. The mPSf is prepared by immersed PSf support membrane into the ethylenediamine tetrakis (propoxylate-B-ethoxylate) surfactant solution to enhanced the hydrophilicity and filled the small pore on the surface to form a smooth surface. And then the Pebax1657® a block copolymer composed of flexible polyether and rigid polyamide, was coated on the PA TFC membranes via the spin-coating method to improve the separation performance. These TFC membranes were applied to CO2/N2 separation process. The effects of monomer structure, concentration of aqueous and organic solutions, feed pressure and water content on the gas transport properties including CO2 permeability, N2 permeability and CO2/N2 selectivity were investigated.
Attentuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, Field-Emission scanning electron microscope (FESEM) observation, Variable monoenergy slow positron beam (VMSPB), Microbalance and water contact angle measurement were used to characterize the chemical structure, morphology and hydrophilicity of the TFC membrane.
From the results, the better interfacial polymerization condition is 0.1M aqueous solution immersion and 0.001M organic solution contact. In this interfacial polymerization condition, the Pebax/EDA-TMC/mPSf membrane was prepared by EDA and TMC, its CO2 permeance and CO2/N2 selectivity is 52.98GPU and 157.7, respectively. Compared with EDA monomer, PEHA is more appropriate for the TFC membrane preparation. Because the facilitated transport mechanism is increase linear as the amine group content. Thus Pebax/PEHA-TMC/mPSf membrane CO2 permeance and CO2/N2 selectivity is 134.2GPU and 113.5, respectively. Under the low feed pressure (0.1bar) test, the facilitated transport mechanism efficiency can be increase, and then enhanced the CO2 permeance to 728.9 GPU and CO2/N2 selectivity to 273.2 for Pebax/PEHA-TMC/mPSf membrane. Because the competitive adsorption, the separation performance is decrease significantly for 15%CO2/85%N2 mixing gas test.

摘要 I
Abstract III
致謝 V
目錄 VII
圖目錄 X
表目錄 XIII
第一章 緒論 1
1.1 前言 1
1.2 薄膜的定義 3
1.3 薄膜分離程序 5
1.4 薄膜結構型態 7
1.4.1多孔性薄膜 (Porous Membrane) 7
1.4.2緻密性薄膜 (Dense Membrane) 7
1.4.3 無機薄膜 (Inorganic Membrane) 8
1.4.4 有機/無機混成薄膜 (Organic/Inorganic Hybrid Membrane) 8
1.5 氣體分離膜 10
1.6 複合膜之製備 12
1.6.1 基材膜之製備 13
1.6.2 緻密層之製備 14
1.7　界面聚合法 15
1.7.1　基材膜性質 17
1.7.2　聚合反應條件 19
1.7.3　新型單體運用 23
1.7.4　添加劑影響 26
1.8　旋轉塗佈技術 29
1.9　促進傳輸機制 31
1.10　文獻回顧 35
1.11　動機與目的 42
第二章 實驗 43
2.1 實驗藥品 43
2.2 實驗儀器 45
2.3 薄膜製備 46
2.3.1 聚醯胺複合膜之製備 46
2.3.2 旋轉塗佈層之製備 49
2.4 薄膜鑑定 50
2.4.1全反射式傅立葉轉換紅外線光譜儀(Attenuated Total Reflectance Fourier Transform Infrared spectroscopy, ATR-FTIR) 50
2.4.2 場發射掃描式電子顯微鏡 (Field-Emission Scanning Electron Microscope, FE-SEM) 51
2.4.3 薄膜表面親水性測試 51
2.4.4　X射線光電子能譜儀 (X-ray Photoelectron spectroscopy, XPS) 52
2.4.5　可變單一能量慢速正電子束分析儀 (Variable monoenergy slow positron beam, VMSPB) 52
2.4.6 氣體分離測試 57
2.4.7 氣體吸附測試 59
2.5 實驗流程 61
第三章 結果與討論 62
3.1 前言 62
3.2 界面活性劑對界面聚合層之製備的影響 63
3.2.1 界面活性劑對基材膜表面改質之影響 63
3.2.2 界面活性劑改質對氣體分離效能之影響 68
3.3 Pebax旋轉塗佈層對氣體分離效能之影響 70
3.4 界面聚合條件對氣體分離效能之影響 77
3.4.1 水相單體溶液浸泡時間之影響 77
3.4.2 有機相單體溶液接觸時間之影響 82
3.4.3 水相單體濃度之影響 86
3.4.4 有機相單體濃度之影響 91
3.5 操作條件對氣體分離之影響 103
3.5.1 進料壓力對氣體分離效能之影響 103
3.5.2 混和氣體分離效能測試 105
第四章 結論 107
第五章 參考文獻 109


 
圖目錄
Figure 1-1 Schematic representation of various membrane cross-sectional morphologies. 4
Figure 1-2 Model of gas separation with a polymer membrane. 11
Figure 1-3 Schematic diagram of thin-film composite membrane [2]. 12
Figure 1-4 Diagrams of polymer film growth at liquid interfaces [20]. 15
Figure 1-5 Schematic of spin coating process [74]. 30
Figure 1-6 Facilitated transport mechanism. 31
Figure 1-7 Schematic mechanism of facilitated transport of CO2 by monoprotonated ethylendiamine used as carrier [84]. 38
Figure 2-1 Schematic representation of interfacial polymerization procedure. 48
Figure 2-2 Schematic diagram of chemical reaction and structures for synthesized polyamide. 48
Figure 2-3 Variable monoenergy slow positron beam spectroscopy. (A) 50 Ci 22Na positron source, (B) W-mesh moderator, (C) magnetic field (70G) coils, (D) ExB filter, (E) positron accelerator, (F) correcting magnets, (G) gas inlet, (H) positron lifetime detector (MCP) for PAL, (I) turbo molecular pump, (J) samples, (K) sample manipulator, (L) ion pump, (M) Ge solid state detector, (N) lifetime detector (BaF2). 55
Figure 2-4 Doppler broadening energy spectrum and definitions of S, W, and R (3γ/2γ ratio) parameters from DBES [94]. 56
Figure 2-5 Schematic representation of gas permeation apparatus. 58
Figure 2-6 Apparatus of gas sorption. 60
Figure 3-1 ATR-FTIR spectra of (a) PSf support and (b) EDA-TMC/PSf membrane. 64
Figure 3-2 SEM images of PSf support membrane (a, b) and EDA-TMC/PSf membrane (c, d). 64
Figure 3-3 SEM images of PSf membrane (a, b) and mPSf membrane (c, d). 67
Figure 3-4 SEM images of mPSf support membrane (a, b) and EDA-TMC/mPSf membrane (c, d). 69
Figure 3-5 SEM images of EDA-TMC/mPSf membrane (a, b), PEBAX/mPSf membrane (c, d), Pebax/EDA-TMC/mPSf membrane (e, f). 72
Figure 3-6 S parameters as a function of positron incident energy for mPSf, EDA-TMC/mPSf, Pebax/mPSf, and Pebax/EDA-TMC/mPSf membranes. 73
Figure 3-7 ATR-FTIR spectra of (a) mPSf support, (b) EDA-TMC/mPSf and (c) Pebax/EDA-TMC/mPSf membrane. 73
Figure 3-8 Cross-sectional SEM images of polyamide TFC membranes prepared with different immersion time of aqueous EDA solution, (a) 0.5, (b) 1.0, (c) 1.5, (d) 2.0, (e) 3.0 min. (Polyamide layer was prepared as follow: mPSf was immersed into 0.1M EDA for various time then contacted with 0.01M TMC for 1min.) 80
Figure 3-9 The effect of immersion time of aqueous EDA solution on (a) permeance and (b) CO2/N2 selectivity at 50 ℃ and 1 bar. (Polyamide layer was prepared as follow: mPSf was immersed into 0.1M EDA for various time then contacted with 0.01M TMC for 1min.) 81
Figure 3-10 Cross-sectional SEM images of polyamide TFC membranes prepared with different contact time of organic TMC solution, (a) 0.5, (b) 1.0, (c) 1.5, (d) 2.0, (e) 3.0 min. (Polyamide layer was prepared as follow: mPSf was immersed into 0.1M EDA for 1 time then contacted with 0.01M TMC for various min.) 84
Figure 3-11 The effect of contact time of organic TMC solution on (a) permeance and (b) CO2/N2 selectivity at 50 oC and 1 bar. (Polyamide layer was prepared as follow: mPSf was immersed into 0.1M EDA for 1 time then contacted with 0.01M TMC for various min.) 85
Figure 3-12 Cross-sectional SEM images of polyamide TFC membranes prepared with different concentration of aqueous EDA solution, (a) 0.05, (b) 0.07, (c) 0.10, (d) 0.15, (e) 0.20 M. 88
Figure 3-13 The effect of concentration of aqueous EDA solution on (a) permeance and (b) CO2/N2 selectivity at 50 oC and 1 bar. (Polyamide layer was prepared as follow: mPSf was immersed in EDA solution of various concentration for 1 min then contacted with 0.01M TMC for 1 min.) 90
Figure 3-14 Cross-sectional SEM images of polyamide TFC membranes prepared with different concentration of organic TMC solution, (a) 0.0005, (b) 0.001, (c) 0.005, (d) 0.01, (e) 0.02 , (f) 0.03 , (g) 0.05 M. 94
Figure 3-15 The effect of concentration of organic TMC solution on (a) permeance and (b) CO2/N2 selectivity at 50 oC and 1 bar. (Polyamide layer was prepared as follow: mPSf was immersed in 0.1M EDA for 1 min then contacted with TMC solution of various concentration for 1 min.) 96
Figure 3-16 SEM images of polyamide TFC membranes prepared with different amine monomers, (a, b) EDA, (c, d) TETA, (e, f) PEHA. 100
Figure 3-17 S parameter as a function of positron incident energy for polyamide TFC membranes prepared with different amine monomers. 101
Figure 3-18 The effect of feed pressure on (a) gas permeance and (b) CO2/N2 selectivity at 50oC. 104

 
表目錄
Table 1-1 Develop of (technical) membrane processes [1]. 5
Table 1-2 Driving force and the two-phase systems separated by membranes for different membrane process[1] 6
Table 3-1 Gas separation performance of PSf support and polyamide TFC membranes under dry and wet conditions. 66
Table 3-2 The water contact angle values of PSf and mPSf support membranes. 67
Table 3-3 Gas separation performance of mPSf support and polyamide TFC membranes under dry and wet conditions. 69
Table 3-4 The water contact angle values of mPSf support, EDA-TMC/mPSf and Pebax/EDA-TMC/mPSf membranes. 76
Table 3-5 Gas separation performance of polyamide, Pebax, and Pebax/ polyamide TFC membranes under dry and wet conditions. 76
Table 3-6 Surface atomic carbon composition from C1s x-ray photoelectron spectra for polyamide TFC membranes with different EDA concentration. 89
Table 3-7 Surface atomic carbon composition from C1s x-ray photoelectron spectra for polyamide TFC membranes prepared with different TMC concentration. 95
Table 3-8 Surface atomic carbon composition from C1s x-ray photoelectron spectra for polyamide TFC membranes prepared with different amine monomers. 101
Table 3-9 Gas separation performance of Pebax/polyamide TFC membranes prepared with various amine monomers under dry and wet conditions. 102
Table 3-10 Mixing gas separation performance of Pebax/polyamide TFC membranes prepared with 0.1M PEHA for immersion time of 1min and 0.001M TMC for contact time of 1min. 106
Table 3-11 Gas adsorption capacity of PEHA-TMC layer at 50 oC and 1 bar. 106

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