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姓名 陳鏡全( Jing-Quan Chen)  查詢紙本館藏   畢業系所 化學工程與材料工程學系
論文名稱 MFI沸石超微粒子之製作
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摘要(中) 本研究的主要的目的在於製作奈米級MFI沸石粒子,再利用界面活性劑聚集這些沸石粒子。期望產物有微孔-中孔的層次結構,以增進產物的利用價值。
在實驗合成的步驟上,我們利用Kirschhock於1999年發表的文獻為基礎,從透明的MFI precursor製備至奈米沸石粒子。接下來直接在沸石懸浮溶液中加入界面活性劑,希望溶液中的沸石粒子間可以聚集出具有中孔結構之二次粒子。我們發現只有一次的水熱程序的溶液中,會生成奈米沸石粒子與subcolloid particle的共存情形。因此我們使用二次水熱程序的方式,使溶液中的subcolloid particle完全轉換成奈米沸石粒子,使溶液中幾乎只存在奈米沸石粒子。
我們發現使用二次水熱程序下所獲得之奈米沸石粒子團聚物,在XRD測量是非晶態,但是經過1300C 24 hr之蒸氣處理後,會得到MFI的吸收峰。由氮氣恆溫吸附的結果發現,吸附量會因蒸氣處理的溫度及時間的增加而有較高微孔的吸附量。用TEM 觀察發現溶液中幾乎全為10 nm左右的奈米沸石粒子。用SEM觀察產物之表面也只看到約20 nm的沸石粒子。
摘要(英) The objective of this study is to prepare nano zeolite particles, and then, use surfactant to aggregate these nano particles. We wish to produce the aggregation of nanoparticles, with intercrystalline mesoporousity.
We follow approach of Kirshhock et al. to prepare precursor of MFI-nano zeolitic particles. We have used the method of addition of surfactant into the zeolitic solution to aggregate nano particles. Particles show meso -pores between them. We discover that, when we use only one heating step to make particles, we find nano zeolite particles and subcolloidal particles coexisting. So,we have changed our process to double heating process. If we use this process, we find subcolloidal particles almost become nano particles.
When we use double heating process to prepare nano zeolitic particles, we need higher steaming temperature and longer steam time. We can see the XRD diffraction peaks and value of microporous adsorption also in-creases. We have used SEM and TEM to observe the nano zeolitic particles.
We believe that, this process can be used to make the assembly of MFI nano zeolitic structure,with intercrystalline mesoporousity.
關鍵字(中) ★ 奈米粒子
★ 沸石
關鍵字(英)
論文目次 中文摘要i
英文摘要ii
目錄iii
圖目錄v
表目錄vi
第一章緒論1
1.1沸石的簡介1
1.1.1沸石的結構2
1.2 MFI沸石的簡介3
第二章文獻回顧5
2.1沸石的形成與成長5
2.2奈米沸石懸浮液的製備7
2.2.1 奈米沸石懸浮液的製備研究7
2.2.2懸浮粒子的分離8
2.3研究方向9
第三章 奈米沸石的製備10
3.1奈米沸石的製備10
3.2樣品性質的分析14
3.2.1 XRD分析14
3.2.2氮氣恆溫吸附分析17
3.2.3熱重分析22
3.2.4 TEM分析23
3.2.5 SEM分析23
3.3 結果與討論25
第四章 奈米沸石製備的改質29
4.1實驗方法30
4.2樣品性質的分析34
4.2.1 XRD分析34
4.2.2 氮氣恆溫吸附分析38
4.2.3 TEM分析41
4.2.4 SEM分析42
4.3 結果與討論43
第五章 結論
5.1XRD與氮氣恆溫吸附討論46
5.2實驗上其它觀點49
5.3檢討與建議49
參考文獻52
附錄1實驗所使用的儀器與藥品54
附錄2熱重分析計算55
附錄3.實驗程序解釋與實驗XRD與t-plot及孔洞分析圖56
參考文獻 1.趙桂蓉”,”沸石觸媒,”化工,1991,第38卷第6期,50-55
2. Lesley Smart and Elaine Moore,1st ed.1992,chap5
3. Sandra L. Burkett and Mark E. Davis,”Mechanisms of Structure Dir ection in the Synthesis of Pure-Silica Zeolites. 1. Synthesis of TPA/Si-ZSM-5,”Chem. Mater., 1995,7,920-928
4. Brian J. Schoeman and Oren Regev,”A study of the initial stage in the crystallization of TPA-silicalite-1,” Zeolite, 1996, 17, 447-456
5. Brian J. Schoeman , ”Analysis of the nucleation and growth of TPA-silicalite-1 at elevated temperatures with the emphasis on colloidal ”, Microporous and Mesoporous Material, 1998, 22, 9-22
6.Raman Ravishankar, Christine Kirschhock, Brian J. Schoeman, Peter Vanoppen, Piet J.Grobet,Sebastian Storck, Wilhelm F. Maier,Johan.A. Martens, Frans C.De Schryver and Pierre A. Jacobs,”Physicochemical Characterization of Silicalite-1 Nanophase Material”,J.Phys. Chem. B,1998,102,2633-2639
7.Raman Ravishankar, Christine E.A.Kirschhock, Peter-Paul Knops-Gerrits, Eddy J.P.Feijen, Piet J.Grobet, Peter Vanoppen, Frans C.DeSchryver, Gerhard Miehe, Hartmut Fuess, Brian J.Scheoman, Pierre A.Jacobs and Johan.A. Martens,”Characterization of Naonsized Material Extracted from Clear Suspensions for MFI Zeolite Synthesis, ”J.PhysChem.B,1999,103,4960-4964.
8.Christine E.A.Kirschhock, Raman Ravishankar, Frederik Verspeurt, Piet J.Grobet,Pierre A.Jacobs and Martens,”Identification of Precursor Species in the Formation of MFI Zeolite in the TPAOH TEOS H2O System,” J.Phys. Chem.B, 1999,103,4965-4971
9.Christine E.A.Kirschhock, Raman Ravishankar,L. Van Looveren, P.A.Jacobs and J.A.Martens,”Martens,”Mechanism of Transformation of Precursors into Nanoslabs in the Early Stages of MFI and MEL Zeolite Foramtion from TPAOH-TEOS-H2O and TBAOH-TEOS-H2O Mixtures,”J.Phy.Chem.B,1999,103,4972-4978
10.Christine E.A.Kirschhock, Raman Ravishankar,L. Van Looveren, P.A.Jacobs and J.A.Martens,”Aggregation Mechanism of Nanoslabs with Zeolite MFI-Type Structure,”J.Phys.Chem.B,1999,103,11021-11027
11.Peter-Paul E.A. de Moor, Theo P.M.Beelen,and Rutger A.van Santen,”In situ Observation of Nucleation and Crystal Growth in Zeolite Synthesis. A Small-Angle X-ray Scattering Investigation on Si-TPA-MFI,”J.Phys.Chem.B,1999,103,1639-1650
12.A.E.Persson,B.J.Schoeman, J.Sterte andJ.-E. Otterstedt,”The Synthe sis of Discrete Colloid Particles of TPA-silicate-1,” Zeolites, 1994, 14, 557-567
13. Brian J.Schoeman,”A Spectroscopic Study of the Initial Stage in the Crystallization of TPA-silicalite from Clear Solutions,”Progress in Zeolites and Microporous Materials,1997,105,647-654
14.C.S.Tsay and A.S.T.Chiang,”The Synthesis of Colloidal Zeolite TPA-silicalite-1,” Microporous and Mesoporous Materials,1998,26,89-99
15.Limin Huang,Zhengbao Wang,Jinyu Sun,Lei Miao,Quanzhi Li,Yushan Yan, and Dongyuan Zhao,”Fabrication of Ordered Porous Structures by Self-Assembly of Zeolite Nano crystals, ”J.Am. Chem. Soc., 2000, 122, 3530-3531
16.程珊珊”沸石晶核的製備與排列”,中央大學化工所碩士論文,2000
17.Michal Kruk and Mietek Jaroniec,”Characterization of Highly Order-ed MCM-41 Silicas Using X-ray Diffraction and Nitrogen Adsorption ,” Langmuir,1999,15,5279-5284
18.Mietek Jaroniec and Michal Kruk,”Standard Nitrogen Adsorption Data for Characterization of Nanoporous Silicas ,” Langmuir, 1999, 15, 5410-5413
19.陳力俊等,”材料電子顯微鏡學,”第四章電子繞射圖形之幾何性質,p75-78,國科會精儀中心,83年11月修定版
指導教授 蔣孝澈(A.S.T. Chiang) 審核日期 2001-7-13
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