本文選題：水滑石 + 有機改性��； 參考：《武漢理工大學》2015年碩士論文

【摘要】：水滑石材料具有較大的內(nèi)表面和孔徑、交換容量大、耐高溫等優(yōu)點,在阻燃劑、醫(yī)藥、離子交換與水污染凈化等領域得到廣泛應用。本論文探索水滑石材料的可控制備方法,以獲取多孔、大比表面積、層間疏水性等吸附材料,以增強其對水中對硝基苯酚(PNP)的吸附性能,主要研究結(jié)果如下:以六亞甲基四胺(HMT)為沉淀劑,十二烷基苯磺酸鈉(SDBS)為表面活性劑,分別以酒石酸鈉、檸檬酸鈉、水楊酸鈉為結(jié)構(gòu)導向劑,通過水熱法合成了分等級多孔鋅鋁系水滑石ZnAl-LDH材料。表征結(jié)果表明,SDBS插層ZnAl-LDH材料在結(jié)構(gòu)導向劑的調(diào)節(jié)下,形貌可從不規(guī)則納米片分別轉(zhuǎn)變成類球狀結(jié)構(gòu),絨球狀和中空微球結(jié)構(gòu)。其中,經(jīng)過水楊酸鈉改性的微球型疏水性ZnAl-LDH具有最大的比表面積(128.9 m2/g)和孔體積(0.37 cm3/g),對PNP的吸附效率也最高,其飽和吸附量為101.6 mg/g。分別以酒石酸鈉,檸檬酸鈉和十二烷基苯磺酸鈉(SDBS)為插層改性劑,六亞甲基四胺(HMT)為沉淀劑,運用一步水熱法制備得到三種不同改性劑陰離子插層的鋅鋁水滑石。分別運用X射線衍射(XRD)和掃描電鏡(SEM),以及N2的吸附-脫附等溫技術(shù)對樣品的形貌和結(jié)構(gòu)特性進行了表征,結(jié)果表明,改性后的三種水滑石的形貌及比表面積各異,其中由酒石酸鈉改性的鋅鋁水滑石具有最大的比表面積(176.9 m2/g),其對硝基苯酚的吸附效率也最高,其飽和吸附量為154.4 mg/g。改性后的鋅鋁水滑石的層間距分別由0.757 nm增大到2.94,3.42,3.73 nm,表明三種改性劑成功插層進水滑石層間。通過對對硝基苯酚的靜態(tài)吸附實驗可知,經(jīng)過三種改性劑改性后的鋅鋁水滑石對對硝基苯酚的吸附效率增大,吸附速率增加,吸附動力學行為符合準二級動力學方程,其吸附等溫線符合Langmuir等溫吸附模型。用共沉淀和離子交換法兩種方法制備了環(huán)糊精(CMCD)插層改性的鋅鋁水滑石。經(jīng)環(huán)糊精改性后,原始的硝酸根型的鋅鋁水滑石的層間距由原來的0.874nm增大到1.60 nm,表明CMCD與層板間硝酸根發(fā)生了離子交換,成功插入水滑石層間,并在層間以軸線垂直于水滑石層板的方式排列。吸附實驗表明,環(huán)糊精插層改性后的鋅鋁水滑石相對于原始的硝酸根型的水滑石,對對硝基苯酚的吸附速率加快,吸附效率提高,吸附量也增大,由原來的68.3 mg/g增大到98.0mg/g,這是由于環(huán)糊精分子具有的圓桶形結(jié)構(gòu),空腔內(nèi)部為疏水性,外表面為親水性,這種特殊的分子結(jié)構(gòu)使的環(huán)糊精分子也可以作為“主體”,通過分子間相互作用(如電荷傳遞、范德華力、疏水作用和醚氧鍵等)與“客體”分子形成包合物,從而提高其對對硝基苯酚的吸附量,其對對硝基苯酚的等溫吸附與Freundlich等溫模型更吻合,吸附動力學行為符合準二級動力學方程。
[Abstract]:Hydrotalcite is widely used in the fields of flame retardants, medicine, ion exchange and water pollution purification because of its large inner surface and pore size, large exchange capacity, high temperature resistance and so on. In this paper, the controllable preparation method of hydrotalcite was explored to obtain porous, large specific surface area and interlaminar hydrophobicity in order to enhance the adsorption properties of p-nitrophenol PNPs in water. The main results are as follows: using hexamethylenetetramine (HMT) as precipitant, sodium dodecylbenzene sulfonate (SDBS) as surfactant, sodium tartrate, sodium citrate and sodium salicylate as structural guides, respectively. The porous zinc-aluminum hydrotalcite ZnAl-LDH was synthesized by hydrothermal method. The characterization results show that the morphology of the ZnAl-LDH intercalated with SDBs can be changed from irregular nanochips to spherical, velvet and hollow microspheres with the adjustment of the structure guidance agent. Among them, sodium salicylate modified microsphere hydrophobic ZnAl-LDH has the largest specific surface area of 128.9 m2 / g) and pore volume of 0.37 cm ~ 3 / g 路g ~ (-1). The adsorption efficiency of PNP is also the highest, and its saturated adsorption capacity is 101.6 mg / g. Using sodium tartrate, sodium citrate and sodium dodecyl benzene sulfonate as intercalation modifiers and hexamethylenetetramine HMTas as precipitators, three kinds of anionic intercalation zinc-aluminum hydrotalcite with different modifiers were prepared by one step hydrothermal method. The morphology and structure of the samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and adsorption desorption isotherms of N2, respectively. The results showed that the morphology and specific surface area of the modified three kinds of hydrotalcite were different. The zinc-aluminum hydrotalcite modified by sodium tartrate has the largest specific surface area of 176.9 m2 / g and the highest adsorption efficiency of p-nitrophenol, and its saturated adsorption capacity is 154.4 mg / g. The interlayer spacing of the modified zinc-aluminum hydrotalcite increased from 0.757 nm to 2.94 ~ 3.42 ~ 3.73 nm, respectively, indicating that the three modifiers successfully intercalated the influent talc layers. Through the static adsorption experiment of p-nitrophenol, it is known that the adsorption efficiency of p-nitrophenol is increased and the adsorption rate of p-nitrophenol is increased by the modified zinc-aluminum hydrotalcite after three modifiers, and the adsorption kinetic behavior accords with the quasi-second-order kinetic equation. The adsorption isotherm is in accordance with the Langmuir isothermal adsorption model. Zinc and aluminum hydrotalcite modified by cyclodextrin (CMCD) intercalation were prepared by coprecipitation and ion exchange method. After modified by cyclodextrin, the interlayer spacing of the original zinc-aluminum hydrotalcite was increased from the original 0.874nm to 1.60 nm, which indicated that the exchange of nitrate between CMCD and the laminates took place, and the interlayer was successfully inserted into the hydrotalcite. The layers are arranged in an axis perpendicular to the hydrotalcite laminates. The adsorption experiments showed that the adsorption rate of p-nitrophenol was accelerated, the adsorption efficiency and the amount of adsorption of the modified zinc-aluminum hydrotalcite were increased compared with the original nitric acid hydrotalcite, the adsorption efficiency and the adsorption capacity of the modified zinc-aluminum hydrotalcite were also increased. The increase from the original 68.3 mg/g to 98.0 mg / g is due to the cylindrical structure of cyclodextrin, the hydrophobicity in the cavity and the hydrophilicity on the outer surface, so that the cyclodextrin molecule can also be used as the "main body". By means of intermolecular interactions (such as charge transfer, van der Waals force, hydrophobic interaction, ether oxygen bond, etc.), inclusion complexes are formed with "guest" molecules, thus increasing the adsorption capacity of p-nitrophenol. The isothermal adsorption of p-nitrophenol is in good agreement with the Freundlich isothermal model, and the adsorption kinetics is in accordance with the quasi-second-order kinetic equation.
【學位授予單位】：武漢理工大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：X703;O647.3

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