七元瓜环桥联丙烯酸聚合物的合成及其性质研究
发布时间：2018-12-20 10:48
【摘要】：瓜环作为一类新型的主体大环化合物,与其相应的化学,即瓜环化学现在已成为大环化学及超分子化学研究领域中的一个重要部分。瓜环端口的亲水性羰基氧原子和疏水性的空腔,以及较强的刚性结构,使得它在超分子化学领域占有重要的位置。在瓜环化学的研究中,瓜环基聚合物的合成及性质已成为其重要研究方向之一。按作用方式可分为:1)建立在配位作用基础上的瓜环基配位聚合物;2)建立在瓜环主客体相互作用基础上的瓜环基超分子聚合物;3)建立在羟基瓜环的化学键基础上的瓜环基聚合物。本文在已有工作的基础上,开展建立在羟基瓜环基础上的瓜环基聚合物研究,主要内容包括:1)七元瓜环桥联丙烯酸聚合物的合成及结构表征;2)七元瓜环桥联丙烯酸萘酚酯的合成、结构表征;3)七元瓜环桥联丙烯酸萘酚酯对染料的吸附性能研究;4)单羟基七元瓜环((HO)Q[7])的合成;5)(HO)Q[7]单羟基七元瓜环的表征:i)利用瓜环外壁作用,以[CdCl4]2 阴离子诱导方式,制备单羟基七元瓜环与碱土金属离子(AE2+)的多孔配位聚合物;ii)对所得(HO)Q[7] AE2+ [CdCl4]2 基多孔配位聚合物对易挥发物质吸附的研究。根据苏海全课题组报道的一锅法,选取丙烯酸作为聚合单体,过硫酸铵既是氧化瓜环反应的氧化剂也是瓜环与丙烯酸聚合反应的引发剂,合成一系列七元瓜环桥联丙烯酸聚合物,产率约为30~80%。所得七元瓜环基桥联丙烯酸聚合物通过一维核磁共振波谱技术、二维核磁共振波谱技术、热分析、红外光谱、扫描电镜、透射电镜及凝胶色谱等方法对其结构进行了表征。该方法拓宽了对空腔较大瓜环的实用研究,提高了瓜环的利用率,给研究者选用更多瓜环或单体材料提供了更多的可能性。基于七元瓜环桥联丙烯酸聚合物上的进一步衍生化,通过与萘酚酯化反应,降低七元瓜环桥联丙烯酸聚合物的水溶性。所得七元瓜环桥联丙烯酸萘酚酯通过红外光谱和固体碳谱进行表征。通过紫外分光光度计检测七元瓜环桥联丙烯酸萘酚酯聚合物对染料的吸附情况,由与七元瓜环和瓜环与聚丙烯酸形成的双重孔道协同作用的,该改性聚合物具有相较于单纯的聚丙烯酸单位质量吸附量有明显增加,特别是中性红,具有较高的选择性。更为突出的性质是用乙醇洗涤已吸附染料的七元瓜环桥联丙烯酸萘酚酯就可以将染料释放,材料可以重复利用。采用法国学者Bardelang和Ouari报道的单羟基瓜环氧化法,合成单羟基七元瓜环;利用瓜环外壁正电性的结构特征,(即瓜环的外壁作用),容易与[Cd Cl4]2 等阴离子相互作用,从而导致瓜环,特别是七元瓜环,容易与碱金属(A+)、碱土金属(AE2+)等离子发生配位作用,进而形成配位聚合物的特点,制备单羟基七元瓜环与AE2+的多孔配位聚合物;开展对所得(HO)Q[7] AE2+ [CdCl4]2 基多孔配位聚合物对易挥发物质吸附的研究。
[Abstract]:As a new type of main macrocyclic compounds, melons have become an important part in the field of macrocyclic chemistry and supramolecular chemistry. Hydrophilic carbonyl oxygen atoms hydrophobic cavities and strong rigid structures at the end of melons make them play an important role in the field of supramolecular chemistry. In the research of melons ring chemistry, the synthesis and properties of melon-based polymers have become one of the important research directions. It can be divided into: 1) coordination polymer based on coordination, 2) supramolecular polymer based on host and guest interaction of melon ring; 3) Cucurbit-based polymers based on the chemical bonds of hydroxy melons. In this paper, based on the existing work, the study of the hydroxy ring based melon ring polymer is carried out. The main contents are as follows: 1) the synthesis and structure characterization of the seven-member melon ring bridged acrylic acid polymer; 2) Synthesis and structure characterization of naphthol acrylate, 3) adsorption property of naphthol acrylate, 4) synthesis of monohydroxyl heptachlorocyclic naphthol acrylate, 4) synthesis of mono hydroxyl heptachlorocyclic naphthol acrylate [7]. Characterization of) (HO) Q [7] mono-hydroxyl hepta-ring: i) porous coordination polymer with alkali earth metal ions (AE2) was prepared by [CdCl4] _ 2 anion induced by the outer wall of: i). Ii) study on the adsorption of volatile compounds by (HO) Q [7] AE2 [CdCl4] 2 based porous coordination polymers. According to the one-pot method reported by Su Hai, the acrylic acid was chosen as the polymerization monomer. Ammonium persulfate was not only the oxidant of the epoxidation of melon ring, but also the initiator of the polymerization between the melon ring and acrylic acid. A series of seven-member melons-bridged acrylic polymers were synthesized and the yield was about 30. 80%. The structure of the quaternary melon-bridged acrylic polymer was characterized by 1D NMR, 2D NMR, thermal analysis, IR, SEM, TEM and gel chromatography. This method broadens the practical research on the large hollow melon rings, improves the utilization rate of the rings, and provides more possibilities for the researchers to select more melons or monomers. Based on the further derivation of the acrylic polymer bridged by the seven-member melon ring, the water solubility of the acrylic polymer bridged with the seven-member melon ring was reduced by esterification with naphthol. Naphthol acrylate was characterized by IR and solid carbon spectra. Ultraviolet spectrophotometer was used to detect the adsorption of naphthol acrylate polymer on the bridge of seven-member melon ring. The adsorption of the dye was synergistic with the double channels formed by the ring and polyacrylic acid. The modified polymer has higher selectivity than that of pure polyacrylic acid, especially neutral red. The more prominent property is that naphthol acrylate can be released by washing the adsorbed dye with ethanol, and the material can be reused. Mono-hydroxyl seven-member melons were synthesized by the method of epoxidation of mono-hydroxyl melons reported by French scholars Bardelang and Ouari. It is easy to interact with [Cd Cl4] 2 + anions by using the positive structural characteristics of outer wall of melon ring (that is, the outer wall of melon ring), which leads to the ring, especially the seven-member ring, easily interacting with alkali metal (A),. The coordination of alkaline earth metal (AE2) plasma and the formation of coordination polymers were investigated. The porous coordination polymers of mono-hydroxyl seven-member melon ring and AE2 were prepared. The adsorption of volatile substances by (HO) Q [7] AE2 [CdCl4] 2 based porous coordination polymers was studied.
【学位授予单位】：贵州大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O634;O641.3
本文编号：2387888
[Abstract]:As a new type of main macrocyclic compounds, melons have become an important part in the field of macrocyclic chemistry and supramolecular chemistry. Hydrophilic carbonyl oxygen atoms hydrophobic cavities and strong rigid structures at the end of melons make them play an important role in the field of supramolecular chemistry. In the research of melons ring chemistry, the synthesis and properties of melon-based polymers have become one of the important research directions. It can be divided into: 1) coordination polymer based on coordination, 2) supramolecular polymer based on host and guest interaction of melon ring; 3) Cucurbit-based polymers based on the chemical bonds of hydroxy melons. In this paper, based on the existing work, the study of the hydroxy ring based melon ring polymer is carried out. The main contents are as follows: 1) the synthesis and structure characterization of the seven-member melon ring bridged acrylic acid polymer; 2) Synthesis and structure characterization of naphthol acrylate, 3) adsorption property of naphthol acrylate, 4) synthesis of monohydroxyl heptachlorocyclic naphthol acrylate, 4) synthesis of mono hydroxyl heptachlorocyclic naphthol acrylate [7]. Characterization of) (HO) Q [7] mono-hydroxyl hepta-ring: i) porous coordination polymer with alkali earth metal ions (AE2) was prepared by [CdCl4] _ 2 anion induced by the outer wall of: i). Ii) study on the adsorption of volatile compounds by (HO) Q [7] AE2 [CdCl4] 2 based porous coordination polymers. According to the one-pot method reported by Su Hai, the acrylic acid was chosen as the polymerization monomer. Ammonium persulfate was not only the oxidant of the epoxidation of melon ring, but also the initiator of the polymerization between the melon ring and acrylic acid. A series of seven-member melons-bridged acrylic polymers were synthesized and the yield was about 30. 80%. The structure of the quaternary melon-bridged acrylic polymer was characterized by 1D NMR, 2D NMR, thermal analysis, IR, SEM, TEM and gel chromatography. This method broadens the practical research on the large hollow melon rings, improves the utilization rate of the rings, and provides more possibilities for the researchers to select more melons or monomers. Based on the further derivation of the acrylic polymer bridged by the seven-member melon ring, the water solubility of the acrylic polymer bridged with the seven-member melon ring was reduced by esterification with naphthol. Naphthol acrylate was characterized by IR and solid carbon spectra. Ultraviolet spectrophotometer was used to detect the adsorption of naphthol acrylate polymer on the bridge of seven-member melon ring. The adsorption of the dye was synergistic with the double channels formed by the ring and polyacrylic acid. The modified polymer has higher selectivity than that of pure polyacrylic acid, especially neutral red. The more prominent property is that naphthol acrylate can be released by washing the adsorbed dye with ethanol, and the material can be reused. Mono-hydroxyl seven-member melons were synthesized by the method of epoxidation of mono-hydroxyl melons reported by French scholars Bardelang and Ouari. It is easy to interact with [Cd Cl4] 2 + anions by using the positive structural characteristics of outer wall of melon ring (that is, the outer wall of melon ring), which leads to the ring, especially the seven-member ring, easily interacting with alkali metal (A),. The coordination of alkaline earth metal (AE2) plasma and the formation of coordination polymers were investigated. The porous coordination polymers of mono-hydroxyl seven-member melon ring and AE2 were prepared. The adsorption of volatile substances by (HO) Q [7] AE2 [CdCl4] 2 based porous coordination polymers was studied.
【学位授予单位】：贵州大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O634;O641.3
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