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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 劉緒宗(Shiuh-Tzung Liu) | |
| dc.contributor.author | Ching-Fu Chang | en |
| dc.contributor.author | 張兢夫 | zh_TW |
| dc.date.accessioned | 2021-06-12T18:28:43Z | - |
| dc.date.available | 2012-08-28 | |
| dc.date.copyright | 2007-08-28 | |
| dc.date.issued | 2007 | |
| dc.date.submitted | 2007-08-06 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/27933 | - |
| dc.description.abstract | 高分子化合物在化學上有極大的應用，本篇論文用親水的乙二醇甲基醚(ethylene glycol methyl ether)的末端以醯胺鍵結(amide link)的方式將三級碳溴2-溴-2甲基丙醯溴(2-bromoisobutyryl bromide)做為巨起始劑，利用ATRP (atom radical transfer polymerization)的技術合成出疏水端為丙烯酸甲酯(methyl acrylate)的雙區塊聚合物。以此雙區塊聚合物來當作合成中孔洞性材料的模板，調控不同比例的乙二醇甲基醚和丙烯酸甲酯，可以觀察到有立方結構(cubic)和二維六角排列(hexagonal)的中孔洞性材料產生，擁有較一般中孔洞材料大的孔洞、高表面積並且有良好的熱穩定性。
為了使此種中孔洞材料帶有酸性，去做非勻相的酸性催化，本篇論文分別修飾鈦、鋁和鈷在中孔洞材料中。鈦和鋁會在水熱時進入矽與氧的骨架之中形成帶有路易士酸性的中孔洞矽氧材料，而鈷則是利用在疏水端(MA)上做3-疊氮丙胺 (3-azidopropyl amine) 官能基修飾，並進一步將疊氮還原成胺基使之和鈷配位變成錯合物，讓鈷能夠在形成中孔洞矽氧材料時，均勻的分布在孔洞表面，而不是隨機分布。隨著金屬的修飾，對此中孔洞材料的結構及性質造成巨大的影響，利用這些金屬氧化物表面缺乏電子所造成的酸性，將在Friedel Crafts反應、酮或醛的ammomaximaion和苯胺的氧化上有不錯的催化效果。 | zh_TW |
| dc.description.abstract | Modified ordered mesoporous silicas were synthesized by the use of amphiphilic di-block copolymers as templates. The hydrophilic end of the copolymers was polyethylene glycol, whereas the hydrophobic end was polymethyl acrylate. By fixing the length of polyethylene glycol, polyacrylate end was constructed through the atom transfer radical polymerization(ATRP). With the use of copolymers PEO-PMA, we have synthesized Al or Ti modified silica mesoporous silicas successfully. With the different ratio of PEO and PMA, the mesostructure of the mesoporous silicas are variable. Due to the modification of Al and Ti into the -Si-O-Si- framework, these porous materials have the Lewis acidity. Modification of amine groups on the polyacrylate end allows the coordination of cobalt ions, which are grafted onto the di-block copolymers. Upon sol-gel process, cobalt oxide nanoparticles was also grouped into the mesoporous silicas. All of these modified mesoporous silicas show good catalytic activity for Friedel Crafts reaction、ammoximaiton of ketones or aldehydes and oxidation of aniline. | en |
| dc.description.provenance | Made available in DSpace on 2021-06-12T18:28:43Z (GMT). No. of bitstreams: 1 ntu-96-R94223038-1.pdf: 3041785 bytes, checksum: 6589e270bd375b38999cf211ab21f2a3 (MD5) Previous issue date: 2007 | en |
| dc.description.tableofcontents | 目錄
目錄 ……………………………………………………………………………………I 圖目錄 ……………………………………………………………………………… III 表目錄 ………………………………………………………………………………VI 摘要 …………………………………………………………………………………VIII 第一章 緒論 …………………………………………………………………………1 1-1中孔洞材料簡介 ………………………………………………………………1 1-2 中孔洞材料的修飾 ………………………………………………………… 2 1-3含路易士酸的孔洞材料在催化上的應用 ……………………………………9 1-4 本篇論文研究方向 ……………………………………………………………14 第二章 兩性雙區塊共聚物的合成與修飾…………………………………………16 2-1 聚乙二醇甲基醚(polyethylene glycol methyl ether)修飾醯胺化反應……… 16 2-2 聚乙二醇甲基醚-聚丙烯酸甲酯雙區塊共聚物(Polymethyl acrylate-b-polyethylene glycol methyl ether) …………………………………17 2-3 聚乙二醇甲基醚-聚丙烯酸甲酯雙區塊共聚合物的修飾(modification of polymethyl acrylate-b-polyethylene glycol methyl ether) ……………………19 第三章 中孔洞材料的製備與鑑定…………………………………………………26 3-1 含鋁的中孔洞材料…………………………………………………………… 26 3-1-1結構與物理性質之鑑定……………………………………………………26 3-1-2 熱重分析(TGA) ………………………………………………………… 30 3-1-3 鋁金屬含量及存在方式之鑑定 …………………………………………32 3-1-4酸性鑑定 ………………………………………………………………… 34 3-1-5 與常見之含鋁矽氧中孔洞材料之比較 …………………………………35 3-2 含鈦的中孔洞材料…………………………………………………………… 37 3-2-1 結構與物理性質鑑定 ……………………………………………………37 3-2-2 熱重分析(TGA) …………………………………………………………41 3-2-3鈦金屬含量及存在方式之鑑定 ………………………………………… 42 3-2-4 酸性鑑定………………………………………………………………… 45 3-2-5 與常見之含矽氧中孔洞材料之比較 ……………………………………46 3-3 合成含鈷的中孔洞材料 ………………………………………………………47 3-3-1結構與物理性質之鑑定……………………………………………………47 3-3-2 熱重分析(TGA) …………………………………………………………49 3-3-3 鈷金屬含量及存在方式之鑑定 …………………………………………50 3-3-4酸性鑑定……………………………………………………………………51 第四章 含鋁、鈦和鈷之矽氧孔洞材料在催化上的應用 ………………………… 53 4-1 含鋁金屬修飾的矽氧孔洞材料在催化上的探討 ……………………………53 4-2 含鈦金屬修飾的矽氧孔洞材料在催化上的探討 ……………………………57 4-2-1 環己烯的催化 …………………………………………………………57 4-2-2 催化酮或醛之衍生物生成oxime ……………………………………… 58 4-3 含鈷金屬修飾的矽氧孔洞材料在催化上的探討…………………………… 65 第五章 結論 ………………………………………………………………………73 第六章 實驗部分 ……………………………………………………………………75 6-1 測試儀器……………………………………………………………………… 75 6-2 化學試劑、溶劑與試劑的純化……………………………………………… 80 6-3 實驗過程 ………………………………………………………………………84 參考文獻 ……………………………………………………………………………94 附圖 ………………………………………………………………………………101 圖目錄 圖1-1中孔洞材料在各方面的應用 …………………………………………………2 圖1-2 ZSM-5的孔道結構示意圖 ……………………………………………………3 圖1-3 含鎢或鈀修飾的兩性雙區塊金屬錯合物 …………………………………… 5 圖1-4 (sulfos)Rh(cod)利用氫鍵吸附在二氧化矽的表面上 …………………………6 圖1-5 兩種不同的途徑去讓有機金屬分子固定在孔洞材料的表面 ………………7 圖1-6 以中孔碳材CMK-3合成中孔洞氧化銅 ……………………………………8 圖1-7週期性中孔有機材料……………………………………………………………9 圖1-8固體酸酸基的兩種形式 ………………………………………………………10 圖1-9將甲基三氧化錸修飾在沸石中……………………………………………… 11 圖1-10鈦對烯類的環氧化反應之反應機構 ………………………………………12 圖1-11 2,4-di-tert-butyl alcohol和phenol的Friedel-Crafts反應……………………14 圖2-1 以ATRP的方式合成聚乙二醇甲基醚-聚丙烯酸甲酯共聚物之1H NMR光 譜 …………………………………………………………………………… 19 圖2-2 將3-疊氮丙胺修飾上聚乙二醇甲基醚-聚丙烯酸甲酯之1H NMR光譜 … 21 圖2-3 將3-疊氮丙胺修飾上聚乙二醇甲基醚-聚丙烯酸甲酯之IR光譜 …………22 圖2-4 將修飾上聚乙二醇甲基醚-聚丙烯酸甲酯聚合物的疊氮還原成胺基(EO45MAn-NH2) ……………………………………………………… 23 圖2-5 將聚乙二醇甲基醚-聚丙烯酸甲酯聚合物上架接丙胺(EO45MAn-NH2)之 IR光譜…………………………………………………………………23 圖2-6 二氯化鈷與含胺基的聚乙二醇甲基醚-聚丙烯酸甲酯的在水溶液下的吸收光譜………………………………………………………………………25 圖3-1以EO45MA27 做為模板合成含鋁中孔洞材料Al-27的XRD圖與BET圖…27 圖3-2以EO45MA27為模板合成含鋁中孔洞材料Al-27的TEM圖 ………………27 圖3-3以EO45MA60 做為模板合成含鋁中孔洞材料Al-60的XRD圖與BET圖… 28 圖3-4以EO45MA60為模板合成含鋁中孔洞材料Al-60的TEM圖 ……………… 28 圖3-5以EO45MA100 做為模板合成含鋁中孔洞材料Al-100的XRD圖與BET圖29 圖3-6以EO45MA100為模板合成含鋁中孔洞材料Al-100的TEM圖……………… 29 圖3-7未鍛燒之含鋁中孔洞材料熱重分析圖(TGA/DTG) ………………………31 圖3-8鍛燒後之含鋁中孔洞材料IR吸收光譜 ……………………………………32 圖3-9 以EO45MA60 做為模板合成含鋁及不含鋁的中孔洞材料Al-60及Si-60之 XRD圖 ……………………………………………………………………… 33 圖3-10以EO45MAn 做為模板合成含鋁中孔洞材料的27Al-MAN-NMR光譜……34 圖3-11以EO45MAn 做為模板合成含鋁中孔洞材料的NH3-TPD圖 ……………35 圖3-12以EO45MA27為模板合成含鈦中孔洞材料Ti-27的XRD圖與BET圖 …37 圖3-13以EO45MA27為模板合成含鈦中孔洞材料Ti-27的TEM圖 ………………38 圖3-14以EO45MA60做為模板合成含鈦中孔洞材料Ti-60的XRD圖與BET圖… 39 圖3-15以EO45MA60為模板合成含鈦中孔洞材料Ti-60的TEM圖……………… 39 圖3-16 以EO45MA100為模板合成含鈦中孔洞材料Ti-100的XRD圖與BET圖… 40 圖3-17以EO45MA100 做為模板合成含鈦中孔洞材料Ti-100的TEM圖 ………40 圖3-18 未鍛燒之含鈦中孔洞材料熱重分析圖(TGA/DTG) ………………………42 圖3-19 含鈦之中孔洞材料之固態UV吸收光譜圖 ………………………………43 圖3-20含鈦中孔洞材料Ti-27、Ti-60、Ti-100和3-Ti-60的高角度XRD圖 ……44 圖3-21鍛燒後之含鈦中孔洞材料IR及Raman吸收光譜 …………………………45 圖3-22以EO45MAn 做為模板合成含鈦中孔洞材料的NH3-TPD圖 ……………46 圖3-23以EO45MA100做為模板合成含鈷中孔洞材料Co-40的XRD圖與BET圖48 圖3-24以EO45MA100做為模板合成含鈦中孔洞材料Co-40的TEM圖與SEM圖 49 圖3-25未鍛燒之含鈷中孔洞材料Co-40熱重分析圖(TGA/DTG) ……………… 49 圖3-26含鈷中孔洞材料Co-40之X光光電子電子能譜(XPS) ……………………50 圖3-27含鈷中孔洞材料Co-40之反射式UV-vis吸收光譜 ………………………51 圖3-28以EO45MA40-NH2做為模板合成含鈷中孔洞材料的NH3-TPD圖 ………51 圖4-1 環己酮經TS-1催化作ammoximation的反應機制 ………………………59 圖4-2 回收催化劑在苯胺氧化反應上的利用 ……………………………………72 圖6-1 ASAP 2010 Micrometrics 孔徑分析儀示意圖 ………………………………78 | |
| dc.language.iso | zh-TW | |
| dc.title | 合成含金屬修飾之中孔洞材料及其在催化上的應用 | zh_TW |
| dc.title | Synthesis of Metal Modified Mesoporous Silicas
and their Applications on Catalysis | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 95-2 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 鄭淑芬(Soo-fin Cheng),林英智(Ying-Chih Lin) | |
| dc.subject.keyword | 中孔洞材料,鋁,鈦,鈷,聚乙二醇,聚丙烯酸甲酯, | zh_TW |
| dc.subject.keyword | mesoporous,aluminum,coblat,titanium,PEO,PMA, | en |
| dc.relation.page | 107 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2007-08-07 | |
| dc.contributor.author-college | 理學院 | zh_TW |
| dc.contributor.author-dept | 化學研究所 | zh_TW |
| 顯示於系所單位： | 化學系 | |
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