本文關(guān)鍵詞： MCM-22 分子篩 微波 合成　出處：《華東師范大學(xué)》2010年碩士論文　論文類型：學(xué)位論文

【摘要】： MCM-22分子篩是MWW拓?fù)浣Y(jié)構(gòu)的代表,其傳統(tǒng)合成方法主要采用水熱合成法,合成的時(shí)間至少需要4-5天。因此,降低能耗、縮短加熱時(shí)間的新型合成方法的研究成為了當(dāng)今研究的熱點(diǎn)。近年來(lái),微波技術(shù)被美國(guó)化學(xué)會(huì)列為綠色化學(xué)的重要成員而倍受矚目,微波輔助法合成分子篩具有反應(yīng)速度快,反應(yīng)條件溫和,能耗低,分子篩粒徑分布窄,純度高,形貌均一等優(yōu)勢(shì),而被廣泛應(yīng)用于多種結(jié)構(gòu)分子篩的合成(如MEL,MFI等)。迄今為止,MWW型分子篩尚無(wú)成功合成的報(bào)道,將微波輔助加熱法應(yīng)用于MWW拓?fù)浣Y(jié)構(gòu)分子篩的合成是本論文的核心研究方向。論文主要包括以下四部分內(nèi)容： 應(yīng)用微波輔助法成功合成MCM-22分子篩,經(jīng)過(guò)29小時(shí)微波晶化得到與傳統(tǒng)水熱法合成5天相同100%晶化的樣品,有效地縮短了合成時(shí)間。通過(guò)XRD,SEM,FT-IR,ICP等技術(shù)進(jìn)行表征,微波輔助合成樣品具有高純度,均一形貌,A1原子有效進(jìn)入骨架等特征。并將微波與傳統(tǒng)水熱的合成樣品通過(guò)晶化曲線,SEM圖,FT-IR等進(jìn)行對(duì)比,研究微波合成的機(jī)理及其優(yōu)勢(shì)。 分別考察了微波合成方法、模板劑用量、晶化溫度和硅鋁比對(duì)合成的影響。結(jié)果發(fā)現(xiàn),模板劑的用量是成功合成MCM-22分子篩的關(guān)鍵,采用多步微波法可以較單步法進(jìn)一步縮短合成時(shí)間。其它因素與傳統(tǒng)合成法規(guī)律基本相同。 利用微波內(nèi)加熱原理,在合成體系中加入少量高介電常數(shù)溶劑作為添加劑(如甲醇,乙二醇,丙三醇),研究添加劑對(duì)合成分子篩的影響。實(shí)驗(yàn)結(jié)果發(fā)現(xiàn),少量小分子甲醇作為添加劑可以進(jìn)一步加快微波合成速度,得到高結(jié)晶度的純相MCM-22分子篩。 應(yīng)用微波輔助合成B-MCM-22分子篩,并對(duì)其他雜原子MWW型分子篩如Ti-MWW等進(jìn)行初步的研究。
[Abstract]:MCM-22 molecular sieve is the representative of MWW topology, its traditional synthesis method is mainly hydrothermal synthesis, the time of synthesis takes at least 4-5 days. Therefore, the energy consumption is reduced. In recent years, microwave technology has been listed as an important member of green chemistry by the American Chemical Society. Microwave-assisted synthesis of molecular sieve has the advantages of rapid reaction, mild reaction conditions, low energy consumption, narrow particle size distribution, high purity and uniform morphology. However, it has been widely used in the synthesis of various molecular sieves (such as MELL-MFI, etc.). So far, there is no report on the successful synthesis of MWW molecular sieves. The application of microwave assisted heating to the synthesis of MWW molecular sieve is the core of this thesis. MCM-22 molecular sieve was successfully synthesized by microwave-assisted method. After 29 hours of microwave crystallization, the same 100% crystallization samples were obtained from conventional hydrothermal synthesis for 5 days. The synthesized samples were characterized by XRDX SEMT-IR ICP and microwave assisted synthesis with high purity and uniform morphology. The Al atoms enter the skeleton effectively and the microwave is compared with the traditional hydrothermal synthesis sample by crystallization curve SEM and FT-IR to study the mechanism and advantages of microwave synthesis. The effects of microwave synthesis, the amount of template, crystallization temperature and Si / Al ratio on the synthesis of MCM-22 molecular sieve were investigated. The results showed that the amount of template was the key to the successful synthesis of MCM-22 molecular sieve. The multi-step microwave method can further shorten the synthesis time compared with the single-step method, and the other factors are basically the same as the traditional synthesis method. The influence of additives on the synthesis of molecular sieve was studied by using microwave internal heating principle and adding a small amount of solvent with high dielectric constant as additives (such as methanol, ethylene glycol, glycerol) in the synthesis system. A small amount of methanol as additive can further accelerate the microwave synthesis rate and obtain pure phase MCM-22 molecular sieve with high crystallinity. B-MCM-22 molecular sieve was synthesized by microwave assisted synthesis, and other heteroatomic MWW molecular sieves such as Ti-MWW were studied.
【學(xué)位授予單位】：華東師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2010
【分類號(hào)】：TQ424.25

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本文編號(hào)：1478076