本文選題：MCM-41　切入點：溶膠-凝膠法　出處：《廣西師范大學(xué)》2017年碩士論文

【摘要】：MCM-41分子篩介孔材料具有較高的比表面積、均勻的和可連續(xù)調(diào)控的孔徑、一維的孔道結(jié)構(gòu),且具有可調(diào)控的形貌如球狀、膜片及纖維狀等許多優(yōu)點,使得它們在工業(yè)催化、生物醫(yī)藥、吸附分離、納米材料器件的制備以及環(huán)境保護等領(lǐng)域體現(xiàn)出巨大的應(yīng)用前景。但由于MCM-41的水熱穩(wěn)定性低、反應(yīng)活性低、無磁性、具有中性的骨架結(jié)構(gòu)等性質(zhì)又限制了 MCM-41在各方面的應(yīng)用,因此吸引大量學(xué)者對其進行研究。本文主要研究Y/MCM-41復(fù)合材料的制備和性能。主要研究內(nèi)容如下:1.采用溶膠-凝膠法合成MCM-41分子篩,通過改變制備過程中TEOS的加入量、氨水的加入量、攪拌時間和攪拌速度的工藝條件,合成出系列樣品,并對樣品進行表征。XRD表征說明TEOS=2.0ml、氨水=32.8ml、攪拌時間=4h時所制備MCM-41分子篩的結(jié)晶度最好;FT-IR表征說明所制備的所有樣品都含有SiO2成分,且都不含有模板劑CTAB,說明此時的溫度條件(550℃、6h、1℃/min)可以很好的去除模板劑,杜絕了模板劑對樣品表征的影響:SEM分析說明TEOS=2.0ml、氨水=32.8ml、攪拌時間=4h時所制備MCM-41分子篩的顆粒性最好;BET分析所得樣品具有較高的比表面積(742～1123m2/g),孔徑均勻(2.5nm左右),因此可知所制備樣品屬于介孔材料;TEM表征說明TEOS=2.0ml、氨水=32.8ml、攪拌時間=4h時所制備MCM-41分子篩具有較為良好的長程有序六方孔道結(jié)構(gòu)。2.以熱溶劑法制備了 Fe3O4粒子,用XRD對其表征發(fā)現(xiàn)制備出來的Fe3O4粒子純度較高,用SEM對其表征發(fā)現(xiàn)樣呈現(xiàn)出很規(guī)則球形,樣品大小基本一致,無團聚現(xiàn)象。另外以溶膠-凝膠法制備出Fe3O4/MCM-41復(fù)合材料,并改變了 Fe3O4、TEOS、氨水的加入量制備出一系列不同的Fe3O4/MCM-41復(fù)合材料,并對其進行表征。XRD表明Fe3O4=0.037g、TEOS=2.0ml、氨水=32.8ml時所制備Fe3O4/MCM-41復(fù)合材料具有相對較好的結(jié)晶度,且含有Fe3O4和MCM-41組分。FT-IR表明所制備的Fe3O4/MCM-41復(fù)合材料中MCM-41可能包覆在Fe3O4的表面。SEM表明Fe3O4=0.037g、TEOS=2.0ml、氨水=32.8ml時所制備Fe3O4/MCM-41復(fù)合材料具有相對較好的顆粒性和有序性。TEM表面Fe3O4=0.037g、TEOS=2.0ml、氨水=32.8ml時所制備Fe3O4/MCM-41復(fù)合材料具有更為良好的長程有序六方結(jié)構(gòu),且MCM-41成功包覆在Fe3O4的表面,證實了 FT-IR的可能性。BET分析表明所制備的復(fù)合材料具有良好的比表面積平均可達784m2/g,孔徑基本維持在2.2～2.7nm之間,歸屬于介孔材料。因此我們成功制備出結(jié)晶度較高、比表面積較高且孔道結(jié)構(gòu)規(guī)整的Fe3O4/MCM-41介孔復(fù)合材料。
[Abstract]:MCM-41 molecular sieve mesoporous materials have high specific surface area, uniform and continuously adjustable pore size, one-dimensional pore structure, and have many advantages such as ball shape, membrane and fiber, which make them catalyze in industry.Biomedicine, adsorption and separation, preparation of nanomaterials and environmental protection show great application prospects.However, because of its low hydrothermal stability, low reaction activity, non-magnetic properties and neutral skeleton structure, MCM-41 has limited its applications in various fields, so it has attracted a large number of scholars to study it.The preparation and properties of Y/MCM-41 composites are studied in this paper.The main research contents are as follows: 1.MCM-41 molecular sieve was synthesized by sol-gel method. A series of samples were synthesized by changing the amount of TEOS, the amount of ammonia, stirring time and stirring speed.The samples were characterized by XRD, 2.0 ml, 32.8 ml ammonia, and the crystallinity of MCM-41 molecular sieve was the best when stirring time was 4 h. All the samples were characterized by FT-IR, and all the samples contained SiO2.And no template agent CTAB was found, which indicated that the temperature of 550 鈩，

本文編號：1707808