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Sol-gel法制備金屬摻雜的多孔硅、鋁氧化物復(fù)合材料

發(fā)布時間:2018-05-19 19:44

  本文選題:溶膠-凝膠法 + 介孔。 參考:《安徽大學(xué)》2011年碩士論文


【摘要】:介孔SiO2材料比表面積較大、孔道大小均勻、孔徑可在2nm至50nm范圍內(nèi)連續(xù)調(diào)節(jié)等特性,使其在分離提純、生物材料、催化、環(huán)境、能源、新型組裝材料(或作為納米反應(yīng)器制備具有特殊光、電、磁等性能的新型納米材料等)等領(lǐng)域具有多種潛在的用途,尤其是在生物醫(yī)學(xué)方面如蛋白質(zhì)固定分離、生物芯片、生物傳感器、藥物的包埋和控釋等具有廣闊的應(yīng)用前景。 本論文以高分子化合物為模板劑,采用了溶膠凝膠法(Sol-gel)和溶膠凝膠-水熱法合成介孔SiO_2及其金屬氧化物摻雜介孔SiO2復(fù)合材料,詳細(xì)研究了高分子模板、摻雜金屬、煅燒溫度等反應(yīng)條件對產(chǎn)物孔結(jié)構(gòu)的影響規(guī)律,初步探討了其在吸附去除有機(jī)染料方面的應(yīng)用,論文工作包括以下幾部分: 第一章運用高分子化合物聚乙二醇(PEG)作為模板劑,利用Sol-gel法合成出了介孔SiO2以及金屬氧化物摻雜的復(fù)合材料,主要考察了制備過程中PEG分子量長度、PEG質(zhì)量、金屬摻雜量、煅燒溫度等條件對材料孔結(jié)構(gòu)的影響。實驗結(jié)果表明:可根據(jù)PEG的分子量、濃度及鏈的長短進(jìn)行調(diào)節(jié)介孔材料的介相結(jié)構(gòu),一般來講PEG分子量對復(fù)合材料的孔結(jié)構(gòu)影響不大,材料的SABETa、Vtot數(shù)值隨著PEG質(zhì)量的增加而增加;SiO2中由于金屬氧化物的摻雜使得復(fù)合材料的比表面積孔容和孔徑減小,可能是氧化物占據(jù)了孔道,形成了Si-O-M化學(xué)鍵,從而提高了材料的熱穩(wěn)定和水熱穩(wěn)定性;另外考察了煅燒溫度的影響,溫度過低有機(jī)物去除不完全,溫度過高可能使得硅骨架坍塌,實驗證明550℃是最佳煅燒溫度。 第二章使用Sol-gel法直接合成了CuO/SiO2復(fù)合材料,采用X射線衍射(XRD),N2等溫吸附-脫附法,傅立葉變換紅外光譜(FT-IR),高分辨透射電鏡(HRTEM)等手段對合成的樣品進(jìn)行表征。實驗結(jié)果表明過渡金屬的摻雜引入基本沒有改變SiO2的骨架,一部分金屬離子進(jìn)入到Si02骨架中形成了M-O-Si鍵,形成的CuO晶相小顆粒占據(jù)了部分孔道,使得材料的比表面積有所下降。 第三章通過溶膠凝膠-水熱法制備了銅的氧化物復(fù)合材料,并研究了對有機(jī)染料亞甲基藍(lán)的吸附作用。實驗結(jié)果表明CuO/SiO2多孔復(fù)合材料對亞甲基藍(lán)有良好的吸附效果,在吸附劑(Cs-600-6-15-NaOH-11-12h-140)用量是0.015g,體系pH=9,攪拌時間為2h的條件下,對亞甲基藍(lán)的去除率高達(dá)97.17%。 實驗結(jié)果表明,以PEG為模板,通過溶膠凝膠法可以方便地制備出介孔二氧化硅及其金屬摻雜的復(fù)合材料,通過PEG分子量、添加質(zhì)量等反應(yīng)條件可以調(diào)節(jié)、控制復(fù)合材料的孔結(jié)構(gòu)特征,還可以有效地將無機(jī)金屬氧化物引入到Si02骨架中形成M-O-Si化學(xué)鍵,賦予介孔二氧化硅新的物理化學(xué)特性,制備出多功能的介孔復(fù)合材料,廣泛的應(yīng)用于吸附、催化等相關(guān)領(lǐng)域。
[Abstract]:Mesoporous SiO2 materials have large specific surface area, uniform pore size, continuous adjustment of pore size in the range of 2nm to 50nm and so on, which make them separate and purify, biomaterials, catalysis, environment, energy, etc. Novel assembly materials (or new nanomaterials with special optical, electrical, magnetic properties, etc.) have many potential applications, especially in biomedical fields such as protein fixation and separation, biochips, etc. Biosensors, drug encapsulation and controlled release have broad application prospects. In this paper, the mesoporous SiO_2 and its metal-oxide doped mesoporous SiO2 composites were synthesized by sol-gel method and sol-gel hydrothermal method with polymer compounds as template. The effect of calcination temperature on the pore structure of the product is discussed. The application of the product in adsorption and removal of organic dyes is discussed. The work of this paper includes the following parts: In the first chapter, the mesoporous SiO2 and metal oxide doped composites were synthesized by Sol-gel method using polyethylene glycol (PEG) as template. The molecular weight of PEG and the amount of metal doped were investigated. The influence of calcination temperature on the pore structure of the material. The experimental results show that the mesophase structure of mesoporous materials can be adjusted according to the molecular weight, concentration and chain length of PEG. Generally speaking, the molecular weight of PEG has little effect on the pore structure of composites. The Vtot value of SABETaI increases with the increase of PEG mass. The specific surface area pore volume and pore size decrease due to the doping of metal oxides in SiO2. It may be that the oxides occupy the pore channels and form the Si-O-M chemical bond. The thermal stability and hydrothermal stability of the materials were improved, and the effect of calcination temperature was investigated. The temperature was too low to remove organic matter completely, and the silicon skeleton might collapse when the temperature was too high. It was proved that 550 鈩,

本文編號:1911391

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