本文選題：多孔材料 + 氧化鐵　； 參考：《大連理工大學(xué)》2016年博士論文

【摘要】：多孔材料是材料科學(xué)中的重要研究內(nèi)容。通過多孔材料和其它功能組分的結(jié)合,將純多孔材料擴(kuò)展到雜化多孔材料,可以極大地延伸此類材料的應(yīng)用領(lǐng)域。氧化鐵種類繁多性能各異,是較為常用的功能組分。α-Fe2O3納米粒子與多孔材料結(jié)合后可以提高它的分散性,使其催化活性發(fā)揮更加充分。γ-Fe2O3和Fe304都具有強(qiáng)磁性,它們與多孔材料結(jié)合的復(fù)合物則可以利用外加磁場的作用快速的定位和收集。本論文將鐵的氧化物作為功能組分,采用不同方法制備了一系列的鐵基多孔材料。在不存在介孔模板劑的條件下,通過一步水熱晶化法,制備出一種新穎的多級孔道含鐵MFI型沸石分子篩微球,該微球由納米片定向組裝后形成。在合成體系中添加一定量的葡萄糖后,所得樣品為4-5μm的均勻微球,具有多級孔道結(jié)構(gòu),比表面積達(dá)502m2/g,而且在其內(nèi)部均勻分散了超細(xì)納米α-Fe2O3顆粒。葡萄糖在分子篩的結(jié)晶和鐵物種變化過程中發(fā)揮了重要作用。該分子篩微球在光催化氧化降解苯酚的反應(yīng)中顯示了良好的催化性能,反應(yīng)1.5 h后苯酚溶液COD脫除率就可達(dá)到100%；經(jīng)過多次循環(huán)反應(yīng)后,仍然保持了良好的催化性能,表明其穩(wěn)定性較好。此合成方法為原位合成其它功能化多孔材料開辟了新的路徑。以十六烷基三甲基溴化銨為介孔模板劑,采用溶膠凝膠法合成出核殼型磁性介孔復(fù)合材料(γ-Fe203/nSi02/mSi02).該材料具有磁性強(qiáng)、比表面積高、孔容大和介孔孔道均勻等特點(diǎn)。γ-Fe2O3/nSiO2/mSiO2由γ-Fe2O3核以及核外的兩層二氧化硅組成,內(nèi)層無孔二氧化硅能夠阻止磁性核與外部溶液接觸,外層介孔二氧化硅則能被氨基功能化并在酸性條件下帶正電荷。因此,帶負(fù)電荷的重鉻酸根離子能夠通過靜電吸附作用被此復(fù)合材料吸附。重鉻酸根離子的吸附符合朗格繆爾吸附等溫線,此復(fù)合材料最大重鉻酸根吸附能力達(dá)到1.03 mmol Cr/g。更重要的是,吸附劑可以很容易的通過外加磁場從溶液中分離回收。將Fe304納米粒子作為磁性核,以聚乙烯吡咯烷酮(PVP)為促進(jìn)劑,采用混合溶劑晶化法制備出新型核殼結(jié)構(gòu)磁性金屬有機(jī)骨架復(fù)合材料Fe3O4/IRMOF-3。聚乙烯吡咯烷酮不僅作為穩(wěn)定劑使Fe304納米粒子均勻分散,而且促使IRMOF-3前驅(qū)體在Fe304表面生長。研究結(jié)果表明,該復(fù)合材料具有高結(jié)晶度、多孔特性、快磁響應(yīng)速度以及穩(wěn)定性。Fe3O4/IRMOF-3在苯甲醛與氰乙酸乙酯的Knoevenagel縮合反應(yīng)中顯示了良好的催化性能,經(jīng)過4h的反應(yīng)后氰乙酸乙酯轉(zhuǎn)化率達(dá)到98.3%。反應(yīng)后的催化劑可以快速磁性分離回收并重復(fù)使用多次。
[Abstract]:Porous materials are important research contents in material science. Through the combination of porous materials and other functional components, the pure porous materials can be extended to hybrid porous materials, which can greatly extend the application fields of these materials. Fe _ 2O _ 3 is a common functional component, which can improve the dispersion of 偽 -Fe _ 2O _ 3 nanoparticles combined with porous materials and make its catalytic activity play more fully. Both 緯 -Fe _ 2O _ 3 and Fe304 have strong magnetic properties. The composites combined with porous materials can be rapidly located and collected by the effect of external magnetic field. In this paper, a series of iron-based porous materials were prepared by using iron oxides as functional components. In the absence of mesoporous template, a novel MFI zeolite microsphere containing iron was prepared by one step hydrothermal crystallization method. After a certain amount of glucose was added into the synthesized system, the obtained sample was a uniform microsphere of 4-5 渭 m, with a multilevel pore structure with a specific surface area of 502m2 / g, and the ultrafine 偽 -Fe _ 2O _ 3 particles were uniformly dispersed inside the system. Glucose plays an important role in the crystallization of molecular sieve and the change of iron species. The molecular sieve microspheres showed good catalytic performance in the photocatalytic degradation of phenol, and the removal rate of COD in phenol solution reached 100% after 1.5 h reaction. It shows that its stability is good. This method opens up a new way for in situ synthesis of other functional porous materials. Using cetyltrimethylammonium bromide as mesoporous template, core-shell magnetic mesoporous composite (緯 -Fe203 / nSi02 / mSi02) was synthesized by sol-gel method. The material is characterized by strong magnetism, high specific surface area, large pore volume and uniform mesoporous channel. 緯 -Fe _ 2O _ 3 / nSiO _ 2 / mSiO _ 2 consists of 緯 -Fe _ 2O _ 3 core and two layers of silica outside the nucleus. Outer mesoporous silica can be functionalized by amino groups and positively charged under acidic conditions. Therefore, the negative charge dichromate ion can be adsorbed by the composite by electrostatic adsorption. The adsorption of dichromate ion accords with Langmuir adsorption isotherm. The maximum adsorption ability of dichromate ion is 1.03 mmol Cr / g. More importantly, the adsorbent can be easily separated and recovered from the solution by an applied magnetic field. Using Fe304 nanoparticles as magnetic nuclei and polyvinylpyrrolidone (PVP) as accelerator, a novel core-shell structure magnetic metal-organic matrix composite Fe _ 3O _ 4 / IRMOF-3 was prepared by mixed solvent crystallization method. Polyvinylpyrrolidone not only acts as stabilizer to evenly disperse Fe304 nanoparticles, but also promotes the growth of IRMOF-3 precursor on Fe304 surface. The results show that the composite has high crystallinity, porous properties, fast magnetic response speed and stability. Fe3O4 / IRMOF-3 shows good catalytic performance in the Knoevenagel condensation of benzaldehyde and ethyl cyanoacetate. After 4 h reaction, the conversion rate of ethyl cyanoacetate reached 98.3%. The catalyst can be recovered quickly by magnetic separation and reused many times.
【學(xué)位授予單位】：大連理工大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2016
【分類號】：TQ138.11;TB383.4

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