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On Synthesis Of Cucurbituril And Its Application In Recycling Noble Metals

Posted on:2007-06-24Degree:MasterType:Thesis
Country:ChinaCandidate:Y P HuFull Text:PDF
GTID:2121360182991154Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
With the one-factor experiement, the author mainly investigates the influences of the following factors: the molar rate of urea and glyoxal;the pH value;the temprature;the reaction time;and the titration speed of glyoxal and so on, on the purity degree and the yield of Glycoluri, when urea and glyoxal are used as compositions to produce Glycoluril with the catalyzer, vitriol. The best production condition which is determined in the paper is that the molar rate of urea and glyoxal is 2.5 the pH value 2. reaction time 2 hours, the temprature 70℃ and the titration speed of glyoxal is lml/min under which circumstance the the producation rate of Glycoluri will be 73%. Also the result of IR analysis indicates that the product is highly pure Glycoluri and it can be used directly to compound Cucurbituril.Then the concentration of hydrochloric acid temprature time and the density of Glycoluril in hydrochloric acid being choosen as the experiment factors in the orthorhombic experimentation (four factors four level) , the best conditions for compounding mixed Cucurbituril are determined. They are as follows: the density rate of Glycoluril in vitriol is 215 mg/ml and concentration of the catalyzer hydrochloric acid 9 mol/L the reaction temprature 100℃ and the reaction time is 3 hours among which the concentration of the catalyzer and the temprature are major factors. The Cucurbituril is showed in the spectrum of IR ~1H NMR and ~13C NMR.Because of the low seperating rate of mixed Cucurbituril by the way of hydrochloric acid recrystalization.at the beginning the author on the foundation of the effects of alkali metals and the solution of alkali metals on the solubility of different Cucurbituril suggests two methods to seperate the mixed Cucurbituril. Firstly accoding to the different solubility of Cucurbituril influenced by alkali metals and thesolution of alkali metals, we can divide the mixed Cucurbituril step by step. Secondly we can group the mixed Cucurbituril into two categories: CB[5> 7] and CB [6, 8];next seprate the each group one by one. However the experiement result shows although the different solubility of each kind of Cucurbituril under the influence of alkali metals and the solutionof alkali metals is helpful to part the mixed Cucurbituril, the method doesn't have any advantage over the hydrochloric acid recrystalization on terms of operating process, the amount of production and the purity of Cucurbituril.The improved two-step water-hydrochloric acid seperating methods is given with the experiement. Dissolve the mixed Cucurbituril at the rate of 40% in distilled water;the indiscerptible is CB[6^ 8] and CB[5> 7] are melted in the solution. Then.after vaporizing and crystallizing, the latter becomes the solid of CB[5> 7];at last, each Cucurbituril group is seperated in the way of hydrochloric acid crytalization. The method has many advantages such as no metal ion introduced lower amount of hydrochloric acid quicker process of seperation higher production, and much purer Cucurbituril. The seperated Cucurbituril have been examined by the IR and'H NMR and the content of CB[5]> CB[6]> CB[7], CB[8] in mixed one are respectively as 19% , 50%, 25%, and 6%.Finally the essay studys the removal of Au+> Ag\ Cu2+ in water by different Cucurbituril. It implys that in Au solution CB[6] and CB[8] have better effect on the removal of Au than CB[6, 8];and the more Cucurbituril in the solution the higher removal rate of Au;however too much Cucurbituril will increase the removal rate but the utilization of Cucurbituril will decrease accordingly. In the mixed solution of Au+ , Ag\ Cu2+ the removal of a bit ofCu2+ and Ag+ is better than that of Au+. CB[6> 8] even can remove all the Cu when there is little in the water. We can use different types of Cucurbituril to seperate Au+, Ag+> Cu2+ For example, we can firstly use CB[6> 8] to seperate Cu2+ and then use CB[5 > 6> 7> 8] to seperate Au+ and Ag+.
Keywords/Search Tags:Glycoluri, Cucurbituril, compounding, separating, noble metals
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