本文選題：聚砜膜材料 + 親水性改性��； 參考：《濟南大學(xué)》2015年碩士論文

【摘要】：聚砜分離膜由于其綜合性能優(yōu)異,越來越受到廣大群眾的青睞。但是,由于聚砜膜材料親水性差,使用過程中易造成膜污染,使得分離效率降低,膜使用壽命縮短。近年來,親水性聚砜成為當(dāng)今國內(nèi)外研究的熱點,是高效聚砜膜材料的核心所在,也是提高分離膜性能的重要手段之一。目前,對聚砜親水性改性主要為整體磺化法,此方法在反應(yīng)過程中不可操控,會附帶發(fā)生一系列的副反應(yīng),如分子鏈的降解、交聯(lián),且磺化度不易控制。本文通過兩條路線,以分子設(shè)計角度,制備了結(jié)構(gòu)明確,親水性可控的聚砜膜材料。以酚酞原料,經(jīng)過系列反應(yīng),合成酚酞啉親水單體,以FT-IR、1H NMR為手段表征了其結(jié)構(gòu)。以酚酞啉(PP)、聯(lián)苯二酚(BP)和4,4’-二氯二苯砜(DCDPS)為反應(yīng)單體,控制它們的摩爾變化,制備不同親水性的聚砜膜材料。通過1H NMR對聚合物進行結(jié)構(gòu)表征。研究了聚合反應(yīng)中反應(yīng)物的配比對聚合反應(yīng)時間及反應(yīng)產(chǎn)物比濃黏度、熱性能和溶解性的影響。研究發(fā)現(xiàn),隨著酚酞啉單體含量增加,聚合反應(yīng)時間延長,聚合物比濃黏度增大,耐熱性能略有降低,聚合物在N,N-二甲基-甲酰胺等溶劑中的溶解度降低。利用浸沒沉淀相轉(zhuǎn)化法,將不同組分的聚砜樹脂制備成分離膜。研究了酚酞啉含量與分離膜的水接觸角、吸水率、尺寸變化率、拉伸斷裂強度、純水通量、微觀形貌的關(guān)系。研究發(fā)現(xiàn),隨著酚酞啉含量的增加,分離膜水接觸角降低,純水通量先升高后降低,在酚酞啉含量為75%時最大,達到260 L·m-2·h-1,吸水率升高,尺寸變化率略有增加。酚酞啉含量對分離膜的拉伸斷裂強度和微觀形貌幾乎沒有影響。以DCDPS為原料,P2O5和濃硫酸為磺化劑,制備了帶有磺酸根基團的3,3’-二磺酸鈉-4,4’-二氯二苯砜(SDCDPS)單體,并通過FT-IR、1H NMR表征確定了其結(jié)構(gòu)。以SDCDPS、六氟雙酚A(BPAF)和4,4’-二氯二苯砜(DCDPS)為反應(yīng)單體,控制它們的摩爾變化,制備不同磺化度的六氟雙酚A型聚砜膜材料。通過1H NMR對聚合物進行結(jié)構(gòu)表征。研究了聚合反應(yīng)中反應(yīng)物的配比對反應(yīng)產(chǎn)物比濃黏度、熱性能和溶解性的影響。研究發(fā)現(xiàn),隨著聚合物磺化度的增加,聚合物比濃黏度增大,耐熱性能略有降低,聚合物在氯仿、1,2-二氯乙烷等溶劑中的溶解度降低。利用浸沒沉淀相轉(zhuǎn)化法,將不同磺化度的六氟雙酚A型聚砜樹脂制備成分離膜。研究了磺化度與分離膜的水接觸角、吸水率、尺寸變化率、拉伸斷裂強度、純水通量、微觀形貌的關(guān)系。研究發(fā)現(xiàn),隨著磺化度的增加,分離膜水接觸角降低,純水通量先升高后降低,在磺化度為5時最大,達到170 L·m-2·h-1,吸水率升高,尺寸變化率略有增加。聚合物的磺化度對分離膜的拉伸斷裂強度和微觀形貌幾乎沒有影響。
[Abstract]:Polysulfone separation membrane is more and more popular because of its excellent comprehensive performance. However, because of the poor hydrophilicity of polysulfone membrane materials, membrane fouling is easy to be caused in the process of use, which results in the reduction of separation efficiency and the shortening of membrane service life. In recent years, hydrophilic polysulfone has become a hot topic at home and abroad, which is the core of high efficiency polysulfone membrane material and one of the important means to improve the performance of separation membrane. At present, the hydrophilic modification of polysulfone is mainly a whole sulfonation method, which can not be manipulated in the reaction process, and a series of side reactions will occur, such as the degradation of molecular chains, crosslinking, and the degree of sulfonation is not easy to control. In this paper, polysulfone membrane materials with clear structure and controllable hydrophilicity were prepared by two routes. Phenolphthalein hydrophilic monomer was synthesized from phenolphthalein by a series of reactions. Its structure was characterized by FT-IRN 1H NMR. Poly (sulfone) membranes with different hydrophilic properties were prepared by using phenolphthaloline (PPN), diphenyl sulfone (DCDPS) and diphenyldiphenylsulfone (DCDPSs) as reactive monomers. The structure of the polymer was characterized by 1H NMR. The effects of the ratio of reactants on the polymerization time, the specific viscosity, thermal properties and solubility of the products were studied. It was found that with the increase of phenolphthaloline monomer content, the polymerization time was prolonged, the specific viscosity of the polymer was increased, the heat resistance was slightly decreased, and the solubility of the polymer in N- (N-dimethyl-formamide) and other solvents was decreased. The polysulfone resin with different components was prepared into a separation membrane by immersion precipitation phase inversion method. The relationships between phenolphthaloline content and water contact angle, water absorption, size change, tensile fracture strength, pure water flux and micromorphology of the membrane were studied. It was found that with the increase of phenolphthaloline content, the water contact angle of the membrane decreased, and the pure water flux first increased and then decreased. When the phenolphthaloline content was 75, the maximum value was 260 L m-2 h-1, the water absorption increased, and the size change rate increased slightly. The content of phenolphthalein had little effect on the tensile strength and microstructure of the membrane. Using DCDPS as raw material P2O5 and concentrated sulfuric acid as sulfonating agent, the monomer of 3 ~ (3 +) -sodium dichlorobenzene disulfonate (SDCDPSs) with sulfonic group was prepared, and its structure was characterized by FT-IR ~ (1H) NMR. Hexafluorobisphenol A polysulfone membrane materials with different sulfonation degree were prepared by using SDCDPS (hexafluorobisphenol A BPAF) and DCDPS4 (4) 4-dichlorobenzene sulfone (DCDPS) as reactive monomers. The structure of the polymer was characterized by 1H NMR. The effects of the ratio of reactants on the specific viscosity, thermal properties and solubility of the products were studied. It is found that with the increase of sulfonation degree, the specific viscosity of the polymer increases, the heat resistance decreases slightly, and the solubility of the polymer in chloroform 1, 2-dichloroethane and other solvents decreases. Hexafluorobisphenol A polysulfone resin with different sulfonation degree was prepared by immersion precipitation phase inversion method. The relationship between sulfonation degree and water contact angle, water absorption, size change, tensile fracture strength, pure water flux and micromorphology of the membrane was studied. It was found that with the increase of sulfonation degree, the water contact angle of the membrane decreased, and the pure water flux first increased and then decreased, and the maximum sulfonation degree was 5, reaching 170 L m-2 h-1, the water absorption increased and the size change rate slightly increased. The degree of sulfonation of the polymer has little effect on the tensile fracture strength and micromorphology of the membrane.
【學(xué)位授予單位】：濟南大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：TQ051.893

【共引文獻】

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本文編號：1825327