臺灣博碩士論文加值系統

本研究以水熱法合成高比表面積之規則中孔洞碳材（OMC），以硝酸氧化修飾中孔洞碳材（OMCA），增加含氧之官能基，之後以迴流嫁接法接合不同胺基批覆量（5、10及20 wt%）及不同種類之胺基分子（四乙烯戊胺，Tetraethylenepentamine，TEPA；三（2-胺基乙基）胺，Tris（2-aminoethyl）amine，TAEA；聚乙烯亞胺，Polyethylenimine，PEI）進行胺基修飾。利用X光粉末繞射儀（XRD）、氮氣等溫吸附-脫附儀（BET）、場發射式掃描電子顯微鏡（FESEM）及穿透式電子顯微鏡（TEM）鑑定所製備的中孔洞碳材之結構及外觀形貌，以傅立葉轉換紅外光譜儀（FTIR）及元素分析儀（EA）探討材料之表面官能基及元素含量，並鑑定胺基修飾材料之表面接合胺基量及孔徑大小差異。在二氧化碳吸附測定方面，利用重量法及體積法評估材料的二氧化碳吸附量，並計算出胺基之氮原子利用效率（CO2/N ratio）。最後利用原位紅外光譜儀（In-situ FTIR）判斷二氧化碳吸附後之產物，以解釋反應機制。
實驗結果顯示，在TEPA及TAEA方面，10 wt%為最適批覆量，而OMCA-
TEPA-10有最高之吸附量，多於OMCA-TAEA-10及OMCA-PEI-10。體積法之結果顯示，OMCA-TEPA-10有最高之化學吸附量，13.23 μg/m2，多於OMCA-TAEA-10之12.96 μg/m2，及OMCA-PEI-10之7.03 μg/m2。然而在氮原子利用效率上，OMCA-TEPA-10卻為最低值0.027，低於OMCA-TAEA-10之0.037及OMCA-PEI-10之0.031，此因TEPA之長直鏈分子的立體障礙所導致。在原位紅外光譜儀的結果，則發現三種胺基有carbamic acid及carbamate的共同吸附產物，且吸附產物在不同溫度下的訊號強弱變化趨勢與化學吸附量之變化趨勢相同。1

In this study, the ordered mesoporous carbon (OMC) with high surface areas and high pore volume was prepared by hydrothermal method, and then modified by nitric acid solution, which was named OMCA. OMCA materials were modified by grafting different amine separately, which were tetraethylenepentamine (TEPA) , tris（2-aminoethyl）amine (TAEA) and polyethylenimine (PEI), and loaded with varied amounts (5, 10 and 20 wt%). The textual, structural properties, and surface morphology of all prepared materials were characterized by powder X-ray diffraction (XRD), N2 sorption isotherms, transmission electron microscopy(TEM) and Fourier transform infrared (FTIR) spectroscopy. Carbon dioxide capture capacity of amine-modified mesoporous carbon was obtained by thermogravimetric analysis (TGA) and volumetric adsorption analyzer (BET); the latter was also used to investigate the adsorption performance on CO2/N ratio. The reaction mechanisms of CO2 adsorption on amine-grafted OMCA were confirmed by infrared spectroscopy.
The experimental results indicated that the optimal amine loaded amount is 10 wt% for OMCA-TEPA and OMCA-TAEA material. OMCA-TEPA-10 has highest adsorption amount. The results of the volumetric method showed that OMCA-
TEPA-10 also had the highest chemical adsorption amounts, 13.23 μg/m2,which was more than OMCA-TAEA-10, 12.96 μg/m2 and OMCA-PEI-10, 7.03 μg/m2. The CO2/N molar ratio were 0.027、0.037 and 0.031, respectively. OMCA-TEPA-10 had highest chemical adsorption amounts but lowest CO2/N ratio due to the steric hindrance. By in-situ FTIR spectroscopy, we showed that the amine groups reacted with CO2 and formed carbamic acids and carbamate under dry conditions. The intensities of ammonium carbamate, carbamic acids and carbamate changed with temperature, and the chemical adsorption intensities had the same trends.

摘要 I
Abstract II
目錄 IV
圖目錄 VI
表目錄 XI
第一章 緒論 1
1.1 研究背景 1
1.2 研究目的與內容 2
第二章 文獻回顧 4
2.1 二氧化碳之性質與來源 4
2.2二氧化碳的捕捉與分離技術 5
2.3 中孔洞碳材簡介 7
2.3.1 中孔洞矽材 7
2.3.2 中孔洞碳材 9
2.4 碳材表面修飾 13
2.4.1 氧化修飾 13
2.4.2 微孔處理 15
2.4.3 胺基修飾 17
2.5 胺基與二氧化碳之作用 21
第三章 實驗設備及方法 26
3.1 研究架構與內容 26
3.2 吸附材製備 28
3.2.1 中孔洞碳材製備 28
3.2.2 氧化修飾中孔洞碳材 28
3.2.3 迴流嫁接法製備胺基改質中孔洞碳材 29
3.3 材料表面特性分析 30
3.3.1 X光粉末繞射（X-ray Diffraction，XRD） 30
3.3.2 穿透式電子顯微鏡（Transmission Electron Microscopy，TEM） 31
3.3.3 場發射掃描式電子顯微鏡 （Field-emission Scanning Electron Microscopy，FESEM） 32
3.3.4 氮氣等溫吸附–脫附曲線（N2 Adsorption / Desorption，BET） 32
3.3.5 傅立葉紅外線光譜 （Fourier Transform Infrared Spectroscopy，FTIR） 39
3.3.6 元素分析（Elemental Analysis，EA） 40
3.3.7 羧酸含量判定 40
3.4 二氧化碳吸附量測定 41
3.4.1 重量法 41
3.4.2 體積法 41
3.4.3 原位紅外光譜吸附測試 42
第四章 結果與討論 43
4.1 規則中孔洞碳材 43
4.1.1 特性分析結果 43
4.1.2 二氧化碳吸附結果 49
4.2 氧化修飾中孔洞碳材 52
4.2.1 特性分析結果 52
4.2.2 二氧化碳吸附結果 61
4.3 胺基修飾中孔洞碳材 64
4.3.1 特性分析結果 64
4.3.2 二氧化碳吸附結果 73
4.3.3 等量吸附熱結果與探討 101
4.4 反應機制探討 104
第五章 結論與建議 111
5.1 結論 111
5.2 建議 112
參考文獻 113
附錄 實驗數據 124

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