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Preparation Of Low-Chlorine-Content Hypercrosslinked Polystyrene Resin And Its Properties

Posted on:2015-03-26Degree:MasterType:Thesis
Country:ChinaCandidate:C G ZhengFull Text:PDF
GTID:2251330428472332Subject:Organic Chemistry
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The hypercrosslinked polystyrene (HC-PS) network was first suggested and synthesized by Davankov and Tsyurup. The prominent performance and broad application prospects of this novel resin attracted extensive attention in the field of adsorption materials. After many years of effort, a lot of progresses have been made in the research of HC-PS. Nevertheless there are several issues on the application of HC-PS in hemopurification. In order to resolve these issues, the following three parts of work have been completed in this thesis.1. In order to replace the high toxic solvent, nitrobenzene, which is used in traditional process for manufacture of HC-PS adsorbents for hemoperfution, a seris of HC-PS resins were synthesized under various reaction temperature by using solvents with less toxicity, such as chlorobenzene and o-dichlorobenzene, as the reation media, and anhydrous FeCl3, AlCl3or TiCl4as the catalyst. The color, pore structure and hydrophilicity of these resins were investigated. The results showed that the resins possess good hydrophilicity when FeCl3was used as catalysts. Three HC-PS resins, which were synthesized by using chlorobenzene or o-dichlorobenzene as the reation media, and FeCl3as the catalyst, is similar to conventional HC-PS resin in appearance and structure. The three resins were selected to test their adsorption performance for creatinine, pentobarbital sodium and vitamin B12. The results showed that the three HC-PS resins possess similar adsorption performance to the conventional resins, which are expected to be employed in hemopurification instead of the conventional HC-PS resins.2. There exist some residual chloromethyl groups in conventional HC-PS resin used in hemopurification. In the storage time of the hemoperfutor filled with water and resins, hydrolysis of residual chloromethyl groups causes production of hydrochloric acid, which would decrease the pH of the water in the hemoperfutor, and might lead to cruor in the course of cure. For this reason, a seris of reactions, including the reduction, amination, esterification and Williamson reaction, were used to reduce the residual chlorine in the resins. Their chlorine content and pore structures were tested, and three of the resins were selected to measure the adsorption performance for creatinine, pentobarbital sodium and vitamin B12. The results showed that the chlorine contents of the resins treated by above methods declined obviously and the case of pH decreasing was improved. Two of them possessed similar adsorption properties to the conventional HC-PS resin and another got better adsorption performance.3. HC-PS resin shows a strong absorption band at1700cm"1in the IR spectrum. There are still some controversy on the attribution and causes of the absorbance band. To reveal this problem, we conducted the following works. A HC-PS resin was treated by NaBH4and the results implied that the strong band was caused by carbonyl group. Some HC-PS resins were prepared from chloromethylated polystyrene under various conditions. The conditions were diverse in the solvent, catalyst, temperature or gas circumstance from each other. The IR spectra of the resins were studied and the changes’caused by the different reaction conditions were observed in order to explore the factors cause the side reaction of oxidation. The results showed that both of oxygen and solvent may cause the oxidation, the catalyst and water in the reaction system could also affect the oxidative degree.
Keywords/Search Tags:hypercrosslinked polystyrene, adsorption properties, harmfulless solvents, low chlorine content, oxidation
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