本文選題：Zr-MOFs材料 + 一元羧酸�。� 參考：《長春工業(yè)大學》2017年碩士論文

【摘要】：金屬-有機骨架材料(MOFs)作為一種新興的高度有序的結(jié)晶多孔材料,在過去的幾十年里,已成為化學與材料科學學科研究的熱點。因其具有永久性的孔隙率和較大的比表面積,以及結(jié)構(gòu)表面多樣的特異性官能團,使其在氣體存儲、吸附與分離、催化、藥物緩釋等方面表現(xiàn)出良好的應(yīng)用前景。追求更高比表面積是MOFs材料研究的永恒目標。本實驗中采用微波輔助法通過添加不同的一元羧酸作為合成穩(wěn)定劑,來合成Zr-MOFs材料:UiO-66、UiO-67和UiO-66-NH2,希望能獲得具有更高比表面積的Zr-MOFs材料,采用的一元羧酸有甲酸、乙酸、丙酸、丙烯酸、丁酸、異辛酸、苯甲酸。對合成出的Zr-MOFs進行了粉末X射線衍射分析、掃描電鏡、N2物理吸附、熱重等一系列表征,發(fā)現(xiàn)除甲酸外,加入其他一元羧酸均能合成出形貌較好的Zr-MOFs材料,但不同的一元羧酸對Zr-MOFs材料的結(jié)晶度、晶粒尺寸以及比表面積有影響。乙酰丙酸是一種十分具有應(yīng)用價值的生物質(zhì)平臺分子,是合成各種輕化工產(chǎn)品的基本原料。對產(chǎn)物進行分離提純是乙酰丙酸制備過程的重要問題。本實驗中分別以UiO-66、UiO-67和UiO-66-NH2作為吸附劑用于吸附乙酰丙酸水溶液,發(fā)現(xiàn)UiO-66和UiO-66-NH2對乙酰丙酸有吸附作用。并以UiO-66為重點研究對象,對Ui O-66吸附乙酰丙酸的過程做了一系列研究,如UiO-66對乙酰丙酸的吸附速率,以及乙酰丙酸溶液的濃度以及溫度等條件對UiO-66吸附乙酰丙酸能力的影響。實驗發(fā)現(xiàn),當乙酰丙酸水溶液濃度為70.0 mg/mL時,UiO-66對其飽和吸附量可達到291 mg/g。同時簡單的模擬乙酰丙酸的工業(yè)生產(chǎn)環(huán)境,在乙酰丙酸水溶液中加入糠醇和甲酸,發(fā)現(xiàn)UiO-66對乙酰丙酸的選擇性吸附較強,糠醇與甲酸的存在對UiO-66吸附乙酰丙酸的能力基本無影響。對吸附后的UiO-66晶體進行了脫附再生實驗,發(fā)現(xiàn)經(jīng)過5次脫附再生后,晶體骨架完好,對乙酰丙酸仍有較高的吸附能力,可重復(fù)性使用。
[Abstract]:As a new and highly ordered crystalline porous material, metal-organic skeleton material has become a hot topic in the field of chemistry and material science in the past few decades. Because of its permanent porosity, large specific surface area and various specific functional groups on the structural surface, it has a good application prospect in gas storage, adsorption and separation, catalysis, drug slow release and so on. The pursuit of higher specific surface area is the eternal goal of MOFs materials research. In this experiment, the microwave-assisted method was used to synthesize Zr-MOFs materials: UiO-66, UiO-67 and UiO-66-NH2 by adding different monocarboxylic acids as synthetic stabilizers, hoping to obtain Zr-MOFs materials with higher specific surface area. The monocarboxylic acids used were formic acid, acetic acid and propionic acid. Acrylic acid, butyric acid, isooctanoic acid, benzoic acid. The synthesized Zr-MOFs was characterized by X-ray diffraction of powder, physical adsorption of N2 by scanning electron microscope, thermogravimetric analysis and so on. It was found that Zr-MOFs materials with good morphology could be synthesized by adding other carboxylic acids except formic acid. However, different monocarboxylic acids affect the crystallinity, grain size and specific surface area of Zr-MOFs materials. Levulinic acid is a kind of biomass-platform molecule with great application value, and it is the basic raw material for the synthesis of various light chemical products. The separation and purification of the product is an important problem in the preparation of levulinic acid. In this experiment, UiO-66 UiO-67 and UiO-66-NH2 were used as adsorbents to adsorb levulinic acid aqueous solution respectively. It was found that UiO-66 and UiO-66-NH2 could adsorb levulinic acid. A series of studies on the adsorption of levulinic acid by UiO-66 were carried out on the basis of UiO-66, such as the adsorption rate of UiO-66 on levulinic acid, the effect of concentration and temperature of levulinic acid solution on the ability of UiO-66 to adsorb levulinic acid. It was found that when the concentration of levulinic acid solution was 70.0 mg/mL, the saturated adsorption capacity of UiO-66 could reach 291 mg / g. At the same time, the industrial production environment of levulinic acid was simulated. Furfuryl alcohol and formic acid were added to the aqueous solution of levulinic acid. It was found that the selective adsorption of levulinic acid by UiO-66 was stronger. The presence of furfuryl alcohol and formic acid had little effect on the ability of UiO-66 to adsorb levulinic acid. The desorption and regeneration experiments of the adsorbed UiO-66 crystal were carried out. It was found that after 5 times of desorption and regeneration, the crystal skeleton was intact, and the adsorptive capacity of levulinic acid was still high, and it could be used repeatedly.
【學位授予單位】：長春工業(yè)大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O641.4;TB383.4

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