具磷酸官能基之中孔洞材料的合成鑑定暨於鑭系金屬及毒物之吸附應用

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余亞芸(Ya-yun Yu) 查詢紙本館藏

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化學學系

論文名稱

具磷酸官能基之中孔洞材料的合成鑑定暨於鑭系金屬及毒物之吸附應用

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摘要(中)

本篇論文主要合成兩種磷酸官能基化的中孔洞材料，並分別探討磷酸官能基化之中孔洞材料對於吸附鑭系金屬中的鉺金屬以及除草劑巴拉刈的吸附效果。
合成方面分為兩大部分，第一部分是以非離子型界面活性劑Brij-76當作模板，以1,4-bis(trithoxysilyl)benzene (BTEB) 和3-(Trihydroxysilyl)propyl methylphosphonate (SPMP) 當作共同矽源，在低酸量的條件下以直接共聚合成法合成出雙官能基的中孔洞材料BS-x，第二部分同樣是以Brij-76當作模板，利用SPMP和Tetraethyl orthosilicate (TEOS) 為共同矽源，合成出含有磷酸官能基的TS-x材料，兩者的磷酸官能基含量皆可高達到40 %。並利用X-ray 粉末繞射、固態核磁共振光譜、等溫氮氣吸脫附、熱重分析儀、穿透式電子顯微鏡及掃描式電子顯微鏡等儀器鑑定材料的結構，同時也鑑定官能基含量對孔洞性質的影響。
應用方面，首先探討鑭系金屬中鉺金屬的吸附，並比較兩種磷酸官能基材料的吸附能力，由結果可得知，若材料中磷酸官能基含量越多，越利於提升金屬的吸附效果，且吸附的最佳條件為pH = 3.5。比較於其他鑭系金屬，含有磷酸的材料對於鉺金屬有較佳的吸附能力，在經過四次重複利用後仍然保有99 %以上的重複使用能力。
在吸附除草劑巴拉刈的實驗部分，發現若修飾上的磷酸官能基越多可能會使孔洞阻塞而不利於巴拉刈的吸附，由於巴拉刈為具有芳香環的分子，利用含有苯環的BS系列材料，藉由 π-π 分子間的吸引力讓巴拉刈更容易進入到孔洞內部和官能基鍵結，進而提升吸附效果。

摘要(英)

Here we report synthesis of two kinds of materials functionalized with tunable content of phosphonic acid groups, to adsorb Erbium ions and Paraquat.
One is bifunctional materials, synthesized by co-condensation of two different organosilane precursors, that is, 1,4-bis(triethoxysilyl)benzene (BTEB) and sodium 3-(trihydroxysilyl)propyl methyl phosphate (SPMP), under acidic condition using nonionic surfactant Brij-76 as template. These materials were periodic mesoporous organosilicas (PMOs) with benzene bridging groups in the silica wall, and denoted as BS-x, where x is the mole ratio of phosphonic acid groups.
The other is synthesized by co-condensation of tetraethyl orthosilicate (TEOS) and SPMP under same condiction like BS-x, and is called TS-x.
Materials were characterized by powder X-ray diffraction (XRD), nitrogen sorption measurements, solid-state 13C and 29Si MAS NMR spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM).
In adsorption experiment, first, we used BS-x and TS-x to adsorb erbium ions.
The adsorption process was carefully studied with differernt factors.The results reveal that the adsorption of erbium ion on mesoporous silica is strongly dependent on the content of phosphonic acid (PA) groups, and increases with the PA content increases.Theses materials retained more than 99 % metal removal efficiency after use for four consecutive cycles.
The second adsorption experiment suggested that there is a benefit for the use of aromatic groups as the enhanced π-π interaction between the aromatic groups of the BS-x materials and paraquat increase the adsorption in comparison to TS-x.The synthesized materials are promising for adsorption of herbicides.

關鍵字(中)

★ 中孔洞材料
★ 苯環
★ 磷酸
★ 巴拉刈
★ 鉺金屬

關鍵字(英)

論文目次

中文摘要 I
Abstract II
目錄 III
圖目錄 VIII
表目錄 XII
第一章緒論 1
1-1中孔洞二氧化矽分子篩 1
1-1-1中孔洞材料簡介 1
1-1-2官能基化之中孔洞材料 4
1-2界面活性劑之簡介 8
1-2-1分子結構種與種類介紹 8
1-2-2共聚高分子 (Block copolymer) 10
1-2-3界面活性劑分子的排列與微胞的形成 11
1-2-4界面活性劑與矽氧化物的交互作用 15
1-3中孔洞材料之應用 19
1-3-1吸附鑭系金屬 19
1-3-2吸附巴拉刈 21
1-4相關文獻回顧 23
1-4-1表面修飾磷酸官能基之中孔洞材料 23
1-4-2含苯環官能基之中孔洞材料 26
1-5研究動機與目的 29
第二章實驗部分 30
2-1實驗藥品 30
2-2實驗步驟 31
2-2-1合成具苯環以及磷酸官能基之BS-x 31
2-2-2合成具磷酸官能基之TS-x 31
2-2-2-1以不同矽源加入延遲時間合成具磷酸官能基之TS-x 31
2-2-3以硫酸裂解中孔洞材料之模板 32
2-2-4鉺金屬吸附實驗 32
2-2-4-1不同初始濃度下吸附鉺金屬實驗 32
2-2-4-2不同反應時間下吸附鉺金屬實驗 32
2-2-4-3不同pH下吸附鉺金屬實驗 33
2-2-5鉺金屬之檢量線製作 33
2-2-6材料的重複利用性 33
2-2-7巴拉刈吸附實驗 34
2-2-7-1不同初始濃度下吸附巴拉刈實驗 34
2-2-7-2不同反應時間下吸附巴拉刈實驗 34
2-2-7-2不同pH下吸附巴拉刈實驗 35
2-2-8巴拉刈檢量線之製作 35
2-3 實驗設備 36
2-3-1實驗合成設備 36
2-3-2 實驗鑑定儀器 36
2-4 鑑定方法 38
2-4-1 同步輻射光束線 (NSRRC Beam Line) 38
2-4-2 X射線粉末繞射 (Powder X-Ray Diffractometer) 39
2-4-3 氮氣吸脫附等溫曲線、表面積與孔洞特性之鑑定 40
2-4-4傅立葉紅外線吸收光譜儀 (Fourier Transform Infrared Spectrometer；FTIR) 45
2-4-5 熱重分析儀 (Thermogravimetric Analyzer；TGA) 46
2-4-6低真空掃描式電子顯微鏡 (Scanning Electron Microscope；SEM) 48
2-4-7穿透式電子顯微鏡 (Transmission Electron Microscope；TEM) 49
2-4-8 固態核磁共振儀 (Solid State Nuclear Magnetic Resonance；Solid State NMR) 51
2-4-9紫外光-可見光光譜儀 (UV / Vis Spectrometer) 59
第三章結果與討論 61
3-1合成不同矽源比例之中孔洞材料 61
3-1-1 XRD鑑定 61
3-1-2 13C CP/MAS NMR鑑定 64
3-1-3等溫氮氣吸脫附鑑定 67
3-1-4 29Si MAS NMR鑑定 71
3-1-5 TGA 熱重分析 75
3-1-6 SEM影像 76
3-1-7 TEM影像 78
3-2 中孔洞材料吸附鉺金屬之吸附實驗 81
3-2-1 鉺金屬之UV光譜以及檢量線 81
3-2-2 不同初始濃度吸附鉺金屬之效果 82
3-2-3 在不同反應時間吸附鉺金屬之討論 84
3-2-4 不同pH吸附鉺金屬之探討 85
3-2-5中孔洞材料吸附鉺金屬後的FT-IR 87
3-2-6 材料的重複利用性 88
3-2-7 吸附等溫模式 89
3-3-8動力學吸附探討 93
3-2-9不同鑭系金屬之吸附探討 97
3-3 中孔洞材料吸附巴拉刈之吸附實驗 98
3-3-2 在不同反應時間吸附巴拉刈之討論 98
3-3-1 不同濃度吸附巴拉刈之討論 99
3-3-3 不同pH吸附巴拉刈之探討 100
3-3-4 表面電位 104
3-3-5 吸附等溫模式 106
3-3-6動力學吸附探討 108
第四章結論 110
參考文獻 111
附錄一 122
第五章緒論 122
5-1 類沸石咪唑骨架材料 123
5-2有機金屬骨架材料吸附金屬的應用與發展 122
第六章實驗部分 125
6-1實驗藥品 125
6-2實驗步驟 126
6-2-1純水相系統合成類沸石咪唑骨架材料 (ZIF-90) 126
6-2-2醇水混和系統合成類沸石咪唑骨架材料 (ZIF-90) 126
6-2-3含銀奈米顆粒之類沸石咪唑骨架材料的合成 126
6-2-4還原對硝基苯酚 (4-nitrophenol) 實驗 127
第七章結果與討論 128
7-1 ZIF-90系列X射線粉末繞射儀 (XRD) 128
7-2 ZIF-90系列之穿隧式電子顯微鏡 (SEM) 影像 129
7-3 ZIF-90之13C CP/MAS NMR 130
7-4 Ag@ZIF-90系列之 (XRD) 131
7-5 Ag@ZIF-90催化實驗 133
7-6化學還原法合成含銀奈米顆粒之類沸石咪唑骨架材料 135
7-7 TEM影像 137
附錄二 138
8-1銅金屬之吸附實驗 138

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指導教授

高憲明

審核日期

2015-7-30

推文