無氟超疏水高分子複合材料製備及其在高效能油水分離與乳化液分離之應用

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研究生：	Dula Daksa Ejeta Dula Daksa Ejeta
論文名稱：	無氟超疏水高分子複合材料製備及其在高效能油水分離與乳化液分離之應用 Preparation of Fluorine- and Nanoparticle-Free Superhydrophobic Polymer Composites for Oil/water Mixtures and Water-in-Oil Emulsions Separation
指導教授：	王志逢 Chih-Feng Wang 賴君義 Juin-Yih Lai
口試委員:	王志逢 Chih-Feng Wang 賴君義 Juin-Yih Lai 洪維松 Wei-Song Hung 胡蒨傑 Chien-Chieh Hu 王大銘 Da-Ming Wang 郭紹偉 Shiao-Wei Kuo 黃智峰 Chih-Feng Huang
學位類別：	博士 Doctor
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2022
畢業學年度：	110
語文別：	英文
論文頁數：	207
中文關鍵詞：	超疏水、超親油、聚（4-乙基苯酚）、聚氧代氮代苯并環己烷、熱固形高分子、油水分離、乳化液分離
外文關鍵詞：	superhydrophobicity, polymer composites, fluorine-free, nanoparticle-free, low surface energy polymers, oil/water separation, emulsion separation
相關次數：	點閱：382 下載：0
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在工業上以及我們的日常生活中常會產生許多含油廢水，這些含油廢水的排放以及海面上的漏油汙染皆會對自然環境造成嚴重的影響。此外，在石油化學工業中，油品中的少量水分也會對其造成許多問題，這些問題需耗費許多資源來解決。因此，開發具有高通量、低耗能、操作簡易、低成本、可量產之乳化劑穩定油包水乳化液處理材料是一個重要的課題。在本研究分為三個部分，我們製備三種具有不含氟、價格低廉之超疏水高分子複合材料。第一個研究中，我們利用聚（4-乙基苯酚）與1,3-phenylene bisoxazoline改質市售棉花，製備具有超疏水與超親油特性之高分子複合材料。此材料經壓縮後可應用於油包水乳化液分離，在重力過濾與加壓過濾下可分別展現10,400 L m-2 h-1 (gravity-driven) and 867,500 L m-2 h-1 bar-1 (0.1 bar)的高通量。在第二個研究中，我們以主練型聚氧代氮代苯并環己烷改質美耐皿海綿製備超疏水材料，此材料展現極佳的吸油特性(最多可吸附本身重量170倍之油汙)，壓縮後可應用於油包水乳化液分離，在重力過濾與加壓過濾下可分別展現13,900 L m-2 h-1 (gravity-driven) and 1,353,000 L m-2 h-1 bar-1 (0.025 bar)的高通量。最後一個研究中，我們利用酚醛樹脂與氧代氮代苯并環己烷改質市售棉花，製備超疏水高分子複合材料。此材料可應用於油水混和液分離，展現1.8x105 L m-2 h-1的高通量。壓縮後可應用於油包水乳化液分離，展現1.6x106 L m-2 h-1 bar-1 (0.025 bar)的高通量。以上的乳化液分離實驗中，濾液的油純度皆高於99.95 wt%，分離效果良好。我們的超疏水高分子複合材料因其高通量、高分離效率、低成本的製備方法皆說明它們在現實應用中具有巨大的潛力。

Nowadays, the discharge of large quantities of oily wastewater from our daily life and Industries, and the frequent oil spill accidents occurred all over the world have caused serious environmental problems. In addition, in transportation field, from production to refining petroleum and related products, a little amount of water in oil is common and causes operational problems, flow blockage, corrosion, inefficient separation, and consequently, adding high costs to the processing, transportation, and separation units. Therefore, an effective method or technology which can demonstrate the separation of surfactant-stabilized water-in-oil emulsions (SS-WOEs) in ultrahigh flux, excellent efficiency, easy operation, low energy consumption, good scalability, and recyclability is needed to resolve such issues. In this thesis work, stable superhydrophobic and superoleophilic (SHASO) materials were prepared from environmentally friendly, cost-effective, and nonfluorinated coating polymer and substrates composites via facile coating methods. In the first work, raw cotton-based SHASO material was prepared from poly(vinyl phenol)-1,3-phenylene bisoxazoline (PVPh-PBO) cross-linked polymer (PPCP) coating via facile immersion-curing method. The as-prepared material with water contact angle (WCA) of ~ 156o and oil CA (OCA) of ~ 0o, remarkably shows ultrahigh permeation fluxes of up to 10,400 L m-2 h-1 (gravity-driven) and 867,500 L m-2 h-1 bar-1 (0.1 bar) for SS-WOEs. In the second work, a melamine sponge-based superhydrophobic (WCA ~ 162.5°) and superoleophilic (OCA ~ 0o) material was prepared from Main-chain-type polybenzoxazine polymer coating via water-based nonsolvent-induced phase inversion method. The as-prepared material can remove oil/organic solvents from the surface of water, as well as underwater quickly with an outstanding absorption capacity (up to 170 times its weight) for chloroform, and most importantly, it extraordinarily displays ultrahigh permeation fluxes of up to 13,900 L m-2 h-1 (gravity-driven) and 1,353,000 L m-2 h-1 bar-1 (0.025 bar) for SS-WOEs. And in the third work, cotton-based SHASO materials were prepared from a cross-linked phenolic resin (PR) with bis(3-phenyl-3,4-dihydro-2H-1,3-benzoxazinyl)methane (BFA) as a coating chemical via similar method with the first work. The as-prepared materials possess in air WCA greater than 160o, and OCA ~ 0o, exhibiting remarkable separation performances for both simple oil/water mixtures and SS-WOEs with flux values of up to 1.8x105 L m-2 h-1 and 1.6x106 L m-2 h-1 bar-1, respectively. Generally, the as-prepared materials show an extraordinary separation performance of various SS-WOEs with ultrahigh flux and excellent minimum oil purity of 99.95 wt%. Essentially, most of coating polymer composites and all the substrates used in this study are commercially available, naturally abundant, cost-effective, eco-friendly and non-toxic. Furthermore, the coating methods and operation techniques applied herein are very simple, economical, effective, and easily scaled up for mass production and able to solve the problems associated with other methods that unable to generate large area substrates.

Table of Contents
Contents                                                                                                                                        Page
Acknowledgment    i
Abstract    ii
摘要 …    iv
Table of Contents    v
List of Figures    x
List of Schemes    xviii
Abbreviations    xxi
Chapter 1: General introduction    1
1    Background    1
2    Organization of the thesis    4
3    Motivation and objectives    5
3.1    Motivation    5
3.2    Objectives    6
Chapter 2: Review of related literatures    9
1    Fundamental understanding of wettability    9
1.1    Basic theories: Young’s equation    10
1.2    Wenzel model    12
1.3    CassieBaxter model    14
1.4    Surface wettability measurements    16
1.4.1    Static CA    16
1.4.2    Dynamic CAs    18
2    Classification of superwettable materials    20
3    Nature-inspired superwettable materials    21
4    Superhydrophobic surfaces and their fabrications    23
4.1    Superhydrophobic surfaces    23
4.2    Fabrication of superhydrophobic surfaces    25
5    Proposed methods to predict surface free energy of a solid material    32
6    The role of hydrogen bonding in determining surface free energy of polymer materials    36
7    Applications of superhydrophobic materials    44
8    Application of superhydrophobic materials for oil/water separation    46
8.1    Oils    46
8.2    The sources of oil contaminants in oily wastewater and their adverse effects    46
9    Research status on oil/water separation technologies    48
9.1    Oil/water mixtures    48
9.2    Oil/water separation technologies    50
10    Materials used for oil/water separations    55
11    SHASO materials: Fabrication and separation mechanisms    56
11.1    Fabrication    57
11.2    Separation mechanisms    59
12    Challenges    66
Chapter 3: Preparation of superhydrophobic and superoleophilic raw-cotton-based material for extremely high flux water-in-oil emulsion separation    68
1    Introduction    68
2    Experimental section    69
2.1    Materials    69
2.2    Methods    70
2.2.1    Preparation of polymer thin films    70
2.2.2    Preparation of cotton-based SHASO material    70
2.2.3    Preparation of SS-WOEs    71
2.2.4    Water-in-oil emulsions separation experiment    71
2.2.5    Quantitative evaluations    71
2.2.6    Material stability tests    72
2.2.7    Instruments and characterization    72
3    Results and discussions    73
3.1    Preparation  of PPCP thin films and PBC@RC    73
3.2    Surface wettability, morphology, and chemical composition characterizations    76
3.2.1    Surface wettability characterizations    76
3.2.2    Characterization of surface morphology and chemical compositions    79
3.3    Stability tests    82
3.4    Separation of water-in-oil emulsions    86
3.4.1    Separation of surfactant-free and SS-WOEs    86
3.4.2    Separation mechanisms    93
3.4.3    Antifouling property    95
4    Conclusions    96
Chapter 4: Preparation of a main-chain-type polybenzoxazine-modified melamine sponge via non-solvent-induced phase inversion for oil absorption and very-high-flux separation of water-in-oil emulsions    99
1    Introduction    99
2    Experimental section    101
2.1    Materials    101
2.2    Methods    101
2.2.1    Preparation procedures of HTPMS    102
2.2.2    Preparation of oil/water mixtures and water-in-oil emulsions    102
2.2.3    Oil/water mixtures separation experiments    102
3    Results and discussions    103
3.1    Preparation of HTPMS    103
3.2    Surface wettability characterizations    106
3.3    Morphology and chemical composition characterizations    108
3.4    Chemical and mechanical stabilities    111
3.5    Oil/water separation potential of HTPMS    116
3.5.1    Absorption capacity of HTPMS    116
3.5.2    Separation of SS-WOEs    120
3.5.3    Separation mechanisms    124
3.5.4    Antifouling property and recyclability of HTPMS    126
4    Conclusions    128
Chapter 5: Preparation of low cost cotton-based superhydrophobic and superoleophilic materials for successful separation of simple oil/water mixtures and water-in-oil emulsions with remarkable performance    129
1    Introduction    129
2    Experimental section    131
2.1    Materials    131
2.2    Methods    132
2.2.1    Preparation of PR thin films and superhydrophobic cotton-based substrates    132
2.2.2    Oil/water  mixtures separation experiment    132
3    Results and discussions    133
3.1    Preparation of PR80 films and PR80@CMs    133
3.2    Surface wettability, morphology, and chemical composition characterizations    140
3.2.1    Surface wettability characterizations    140
3.2.2    Surface morphology and chemical compositions characterizations    144
3.3    Stability of PR80@CMs under various conditions    146
3.4    Oil/water separation performance of PR80@CF and PR80@RC    148
3.4.1    Separation of simple oil/water mixtures    150
3.4.2    Separation of SS-WOEs    155
3.4.3    Recyclability    159
4    Conclusions    161
Chapter 6: Conclusions and future prospective    162
References    164
List of research papers, oral presentations, and other achievements    179

                                

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