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研究生： 古凡峰
ku fan feng
論文名稱： 石油工業廢觸媒對砂漿材料性質之影響
指導教授： 許貫中
Hsu, Kung-Chung
學位類別： 碩士
Master
系所名稱： 化學系
Department of Chemistry
論文出版年： 2000
畢業學年度： 88
語文別： 中文
中文關鍵詞： 廢觸媒 、波索蘭反應 、資源化
英文關鍵詞： spent catalyst, Pozzolanic reaction, take advantage
論文種類： 學術論文
相關次數： 點閱：154  下載：0 
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    • 摘要
    本研究是針對中油公司煉油過程中產生廢觸媒的資源化利用，因為每天中油廢觸媒卸出量為2公噸，且往常都用掩埋的方法處理，所以對環境而言是一大的負擔。
    資源化利用的方向是添加在混凝土裡，因為廢觸媒的主要成分為Al2O3和SiO2，而其成分比例和有波索蘭效果的高嶺土相似， 所以可以應用X光粉末繞射分析(XRD)和固態NMR儀器來探討廢觸媒是否有波索蘭反應，接著由水化熱和初、終凝的凝結時間、抗壓強度和壓汞測孔儀(MIP)的壓汞孔隙率來研究添得觸媒對水泥漿體的材料性質的影響。
    研究結果顯示觸媒在水泥漿體裡會進行波索蘭反應，且其效果比矽灰來得好，因為用XRD和固態NMR儀器實驗分析得知觸媒的波索蘭反應時間比矽灰快，故對水泥漿體的抗壓強度和緻密性有比較正面性的幫助。觸媒的顆粒小且反應活性大，所以當添加在砂漿時會消耗大量的水，造成砂漿流動性變差， 故要提高水膠比和強塑劑的量來增加砂漿的流動性。但因觸媒的添加，砂漿黏度會比較大，使得砂和水泥漿體不會有析離現象出現，故砂漿流動和分布會比較均勻。
    初、終凝的時間會因添加觸媒在水泥漿體而縮短，其原因是觸媒會加速水泥的水化反應，使得水泥漿體很快就由可塑性變成硬固性。因此，廢觸媒可以應用在因要早點拆模而需要凝結時間較短且抗壓強度較大的混凝土工程上。

    ABSTRACT
    This study is aimed at the way to take advantage of spent catalyst produced in the process of oil-refining in Chinese Petroleum Corp. Since the capacity of spent catalyst from Chinese Petroleum Corp is 2 metric tons every day, and that it used to be buried becomes an encumbrance to our environments.
    The way to take advantage of spent catalyst is to add spent catalyst to concrete. Because the main components of spent catalyst are Al2O3 and SiO2, and it is similar to the components and proportions of kaolin having Pozzolanic reaction, and then we can use powder X-ray (XRD) and solid NMR instruments to probe into if spent catalyst has Pozzolanic reaction. After that, we use hydration heat, the setting time of initial setting and final setting, compressive strength, and mercury intrusion porosimetry of MIP to analyze the effect of adding catalyst to cement pastes.
    The result of this study shows catalyst proceeds Pozzolanic reaction in cement paste, and the effect is better than silica fume. By using XRD and solid NMR instruments to analyze, we get the Pozzolanic reaction of catalyst is faster than the one of silica fume and is positive to compressive strength and density the microstructures of cement paste. Pellets of catalyst are small and have big active reaction, so it will waste much water when added to mortars, and that makes the fluid of mortars become worse.
    In order to raise the fluid of mortars, we add more W/B and SP. The viscosity of mortars increases by adding catalyst, that makes sands and cement paste have no segregation, and the fluid and distribution of mortars will be more even.
    The time of initial setting and final setting will be shorter by adding catalyst to cement paste because catalyst speeds up the hydration reaction of cement and makes cement paste hard from plasticity soon. So, spent catalyst can be applied in concrete that needs shorter setting time and larger compressive strength to remove forms earlier.

    目錄 第一章 緒論----------------------------------------------1 1-1 研究動機------------------------------------------------------1 1-2 研究目的------------------------------------------------------1 1-3 研究方法------------------------------------------------------2 第二章 文獻回顧------------------------------------------3 2-1 沸石觸媒------------------------------------------------------3 2-2 水泥的組成與分類----------------------------------------------6 2-3 水泥的水化行為------------------------------------------------9 2-4 添加波索蘭材料對水泥水化行為之影響---------------------------12 2-5 強塑劑-------------------------------------------------------17 2-5-1 強塑劑的種類-------------------------------------------17 2-5-2 強塑劑的減水機理---------------------------------------18 2-5-3 強塑劑的坍度保持---------------------------------------18 2-6 水泥漿體之微觀結構-------------------------------------------20 2-6-1 水泥漿體之固相微觀結構---------------------------------21 2-6-2 水泥漿體中的非固相微觀結構-----------------------------24 2-7 核磁共振技術與在混凝土之應用---------------------------------27 第三章 實驗部分-----------------------------------------30 3-1 實驗材料-----------------------------------------------------30 3-2 實驗儀器-----------------------------------------------------33 3-3 實驗方法-----------------------------------------------------34 3-3-1 mini-slump cone擴散平均直徑之測試----------------------34 3-3-2 水泥漿抗壓試體之製備-----------------------------------34 3-3-3 NMR與XRD水泥漿試體製作--------------------------------35 第四章 實驗討論-----------------------------------------36 4-1 漿體新拌性質-------------------------------------------------36 4-1-1 迷你坍度流（Mini slump）-------------------------------36 4-1-2 實驗配比設計-------------------------------------------38 4-1-3 水化熱-------------------------------------------------43 4-1-4 水泥漿凝結時間-----------------------------------------45 4-2 漿體硬固性質-------------------------------------------------47 4-2-1 抗壓強度-----------------------------------------------47 4-2-2 MIP孔隙度分析------------------------------------------76 4-2-3 X光粉末繞射分析----------------------------------------78 4-2-4 NMR分析------------------------------------------------91 4-2-5 SEM觀測及分析-----------------------------------------102 第五章 結論--------------------------------------------107 第六章 參考資料----------------------------------------109 表目錄 表2-1 波特蘭水泥之主要成份及其性質------------------------------6 表2-2 波特蘭水泥之典型成份及性質--------------------------------7 表2-3 水泥熟料單礦物的水化特徵----------------------------------7 表2-4 各種成分對波特蘭水泥性質之影響 ---------------------------8 表2-5 波索蘭材料的成份和其在工程性上應用方向-------------------14 表2-6 水泥漿體之主要組成成份及其性質---------------------------21 表2-7 水泥漿體組成對漿體特性的影響-----------------------------22 表2-8 孔隙分類及其對混凝土性質之影響---------------------------25 表3-1 波特蘭第一型水泥化學成份分析-----------------------------30 表3-2 觸媒和矽灰成份-------------------------------------------31 表3-3 西螺砂之篩分析-------------------------------------------32 表4-1-1 不同觸媒或矽灰取代量的砂漿配比---------------------------38 表4-1-2 不同觸媒或矽灰取代量的砂漿配比---------------------------39 表4-1-3 不同觸媒或矽灰取代量的砂漿配比---------------------------39 表4-1-4 不同觸媒或矽灰取代量的砂漿配比---------------------------40 表4-1-5 不同觸媒或矽灰取代量的砂漿配比---------------------------40 表4-1-6 不同觸媒或矽灰取代量的砂漿配比---------------------------41 圖目錄 圖2-1 沸石之二級構成單元--------------------------------------4 圖2-2 方鈉石群晶體--------------------------------------------5 圖2-3（a） 沸石A之結構--------------------------------------------5 圖2-3（b） 沸石X及Y之結構----------------------------------------5 圖2-4 水泥水化過程放熱速率及水泥顆粒之水化過程---------------11 圖2-5（a） 矽酸三鈣和波索蘭物質水化反應過程-----------------------16 圖2-5（b） 鋁酸三鈣和波索蘭物質水化反應過程-----------------------16 圖2-6 強塑劑SNF分散和保持坍度的作用圖-----------------------19 圖2-7 波特蘭水泥漿體微觀結構之示意圖-------------------------20 圖2-8 添加15﹪矽灰水化七天後之29Si NMR光譜圖（W/C+S=0.7）----29 圖3-1（a） 水泥放大1000倍----------------------------------------30 圖3-1（b） 水泥放大6000倍----------------------------------------30 圖3-2（a） 觸媒放大1000倍----------------------------------------31 圖3-2（b） 觸媒放大6000倍----------------------------------------31 圖3-3（a） 矽灰放大35倍------------------------------------------31 圖3-3（b） 矽灰放大8500倍----------------------------------------31 圖3-4 磺酸化奈甲醛縮合物(SNF)分子結構------------------------32 圖3-5 迷你坍度錐---------------------------------------------33 圖4-1-1 不同配比的漿體隨SNF劑量改變流度-----------------------37 圖4-1-2 觸媒、矽灰取代水泥對砂漿中SNF劑量的變化---------------42 圖4-1-3 水泥漿的溫度隨著水化時間變化---------------------------43 圖4-1-4 水泥漿的溫度隨著水化時間變化---------------------------44 圖4-1-5 水泥漿的溫度隨著水化時間變化---------------------------44 圖4-1-6 觸媒取代量不同的水泥漿初終凝變化-----------------------45 圖4-1-7 觸媒取代量不同的水泥漿初終凝變化-----------------------46 圖4-1-8 觸媒取代量不同的水泥漿初終凝變-------------------------46 圖4-2-1 不同SNF劑量流動值-------------------------------------48 圖4-2-2 不同SNF劑量下砂漿抗壓強度變化-------------------------48 圖4-2-3 不同SNF劑量下觸媒取代水泥之砂漿流動值-----------------49 圖4-2-4 不同SNF劑量下觸媒取代水泥之砂漿抗壓強度變化-----------49 圖4-2-5 不同SNF劑量矽灰取代水泥之砂漿流動值-------------------50 圖4-2-6 不同SNF劑量下矽灰取代水泥之砂漿抗壓強度變化-----------50 圖4-2-7 不同水膠比純水泥砂漿抗壓強度變化-----------------------52 圖4-2-8 同樣的工作度的條件下用觸媒和矽灰取代水泥沙漿抗壓強度值的 變化------------------------------------------------54 圖4-2-9 同樣的工作度的條件下用觸媒和矽灰取代水泥沙漿抗壓強度值的 變化------------------------------------------------54 圖4-2-10 同樣的工作度的條件下用觸媒和矽灰取代水泥沙漿抗壓強度值的 變化------------------------------------------------55 圖4-2-11 不同觸媒取代量所造成水泥漿體強度變化------------------56 圖4-2-12（a） 不同觸媒取代量之砂漿抗壓強度比值--------------------57 圖4-2-12（b） 不同觸媒取代量之砂漿抗壓強度------------------------57 圖4-2-13（a） 不同觸媒取代量之砂漿抗壓強度比值--------------------58 圖4-2-13（b） 不同觸媒取代量之砂漿抗壓強度------------------------59 圖4-2-14（a） 不同觸媒取代量之砂漿抗壓強度比值--------------------59 圖4-2-14（b） 不同觸媒取代量之砂漿抗壓強度------------------------60 圖4-2-15（a） 不同矽灰取代量之砂漿抗壓強度比值--------------------62 圖4-2-15（b） 不同矽灰取代量之砂漿抗壓強度------------------------62 圖4-2-16（a） 不同矽灰取代量之砂漿抗壓強度比值--------------------63 圖4-2-16（b） 不同矽灰取代量之砂漿抗壓強度------------------------63 圖4-2-17（a） 不同矽灰取代量之砂漿抗壓強度比值--------------------64 圖4-2-17（b） 不同矽灰取代量之砂漿抗壓強度------------------------64 圖4-2-18 用不同觸媒和矽灰的量取代水泥，造成砂漿抗壓強度的差異--65 圖4-2-19 用不同觸媒和矽灰的量取代水泥，造成砂漿抗壓強度的差異--66 圖4-2-20 用不同觸媒和矽灰的量取代水泥，造成抗壓強度的差異------66 圖4-2-21 用不同觸媒的量取代水泥，造成砂漿抗壓強度比值(SNF0.5%)-67 圖4-2-22 用不同觸媒的量取代水泥，造成砂漿抗壓強度比值(SNF0.8%)-68 圖4-2-23 用不同觸媒的量取代水泥，造成砂漿抗壓強度比值(SNF1.1%)-69 圖4-2-24 含不同劑量SNF的5%觸媒取代量砂漿抗壓強度比值----------70 圖4-2-25 含不同SNF的劑量的砂漿流度值---------------------------70 圖4-2-26 含不同劑量SNF造成10%觸媒取代量砂漿抗壓強度比值-------71 圖4-2-27 含不同SNF的劑量的砂漿流度值--------------------------72 圖4-2-28 不同矽灰取代量的砂漿抗壓強度比值(SNF0.5%)-------------73 圖4-2-29 不同矽灰取代量的砂漿抗壓強度比值(SNF0.8%)-------------73 圖4-2-30 不同矽灰取代量的砂漿抗壓強度比值(SNF1.1%)-------------74 圖4-2-31 含不同劑量SNF的5%矽灰取代量砂漿抗壓強度比值----------75 圖4-2-32 含不同劑量SNF的5%矽灰取代量砂漿抗壓強度比值----------75 圖4-2-33 水泥砂漿孔隙體積和抗壓強度比較------------------------77 圖4-2-34 由一個晶格所生的繞射--------------------------------78 圖4-2-35（a） 矽灰和純CH反應0天---------------------------------80 圖4-2-35（b） 矽灰和純CH反應7天---------------------------------80 圖4-2-35（c） 矽灰和純CH反應28天--------------------------------81 圖4-2-36（a） 觸媒和純CH反應0天---------------------------------82 圖4-2-36（b） 觸媒和純CH反應7天---------------------------------82 圖4-2-36（c） 觸媒和純CH反應28天--------------------------------83 圖4-2-37（a） 水泥水化反應3天------------------------------------83 圖4-2-37（b） 水泥水化反應28天-----------------------------------84 圖4-2-38（a） 觸媒取代量30%水泥水化反應3天-----------------------85 圖4-2-38（b） 觸媒取代量30%水泥水化反應7天-----------------------85 圖4-2-38（c） 觸媒取代量30%水泥水化反應28天----------------------86 圖4-2-39（a） 觸媒取代量60%水泥水化反應1天-----------------------87 圖4-2-39（b） 觸媒取代量60%水泥水化反應3天-----------------------87 圖4-2-39（c） 觸媒取代量60%水泥水化反應7天-----------------------88 圖4-2-39（d） 觸媒取代量60%水泥水化反應28天----------------------88 圖4-2-40（a） 矽灰取代量30%水泥水化反應3天-----------------------89 圖4-2-40（b） 矽灰取代量30%水泥水化反應7天-----------------------90 圖4-2-40（c） 矽灰取代量30%水泥水化反應28天----------------------90 圖4-2-41 觸媒未反應的NMR圖-----------------------------------91 圖4-2-42 觸媒和氫氧化鈣混合物--------------------------------92 圖4-2-43 觸媒和氫氧化鈣反應7天圖----------------------------93 圖4-2-44(a)(b)(c) 鋁在矽聚合物的相對位置圖-----------------------94 圖4-2-45 鋁在矽聚合物的相對位置圖----------------------------95 圖4-2-46 觸媒和氫氧化鈣反應28天圖---------------------------95 圖4-2-47 未反應的矽灰NMR圖----------------------------------96 圖4-2-48 矽灰和氫氧化鈣反應7天時的NMR圖--------------------97 圖4-2-49 矽灰和氫氧化鈣反應28天時的NMR圖-------------------98 圖4-2-50 水泥未反應的NMR圖----------------------------------98 圖4-2-51 水泥試體水化反應28天的NMR圖-----------------------99 圖4-2-52 觸媒取代30%水泥試體水化反應28天的NMR圖-----------100 圖4-2-53 30%矽灰取代水泥試體水化反應28天的NMR圖------------101 CH：矽灰=0.3：0.7-------------------------------------------------102 圖4-2-54（a） 7天1000倍、4500倍---------------------------------102 圖4-2-54（b） 28天1000倍、4500倍--------------------------------102 CH：觸媒=0.3：0.7-------------------------------------------------103 圖4-2-55（a） 7天1000倍、6000倍---------------------------------103 圖4-2-55（b） 28天1000倍、6000倍--------------------------------103 觸媒：水泥=0.3：0.7-----------------------------------------------104 圖4-2-56（a） 3天1000倍、6000倍---------------------------------104 圖4-2-56（b） 7天1000倍、6000倍---------------------------------104 圖4-2-56（c） 28天1000倍、6000倍--------------------------------104 矽灰：水泥=0.3：0.7-----------------------------------------------105 圖4-2-57（a） 3天1000倍、6000倍---------------------------------105 圖4-2-57（b） 7天1000倍、6000倍---------------------------------105 圖4-2-57（c） 28天1000倍、6000倍--------------------------------105 水泥：觸媒=1：0---------------------------------------------------106 圖4-2-58（a） 3天1000倍、6000倍----------------------------------106 圖4-2-58（b） 7天1000倍、6000倍----------------------------------106 圖4-2-58（c） 28天1000倍、6000倍---------------------------------106

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