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Synthesis Of N-Alkyl Carbazole And The Phase Diagram Research Of Their Mixture

Posted on:2017-06-29Degree:MasterType:Thesis
Country:ChinaCandidate:X H ZouFull Text:PDF
GTID:2311330512965270Subject:Organic Chemistry
Abstract/Summary:PDF Full Text Request
In recent years,due to our country?s strong support for the development of new energy vehicles,technologies related to new energy have been the hot spot of research,the hydrogen vehicle,own to its high energy utility rate and long running distance once fueled,also attracts a lot of attention from the technological field.As one of the hydrogen carriers,organic liquid material is regarded as the most potential hydrogen carrier material.In this experiment,we researched the manufacturing procedures of N-Ethyl carbazole and N-propyl carbazole,their dual phase diagram and hydrogenation.Through phase-transfer catalysis,high pure N-methyl carbazole,N-ethyl carbazole,N-propyl carbazole,N-butyl carbazole and N-heptyl carbazole have been made,the functional groups of which have also been analyzed by IR and NMR.Based on the reported statistics that Carbazole ring has the effect on ? carbon by 6ppm,the theoretical chemical shifts are calculated,after comparison,the effect of Carbazole ring imposed on ? carbon seems to be more accurate between 6.4 and 6.5ppm.Samples of N-ethyl carbazole/N-propyl carbazole system with different ratios were cooled gradually,we adjusted the coolant temperature every two minutes in order to keep temperature gap between 5 degrees,and wrote down the temperature of the samples at the same time.The dual phase-diagram is made according to the cooling curves of samples with different N-ethyl carbazole/N-propyl carbazole ratios,which are pictured,based on the cooling temperatures and according time.Analyzing this phase-diagram,it is determined that a kind of sFigure compound(E)are also synthesized during the process.The dual phase-diagram of N-ethyl carbazole(A)/N-propyl carbazole(D)can be regarded as the constitution of the phase-diagrams of A-E system and D-E system with two eutectic temperatures at 7.4? and 4? respectively.The hydrogenation of N-ethylcarbazole and N-propyl carbazole proves the effectiveness of the catalyst,in the process,we also optimized the reaction conditions,knowing the N-ethylcarbazole and N-propyl carbazole hydrogenised completely with the temperature of 162??175? and 168 ? at segments I?II and III respectively,the hydrogenation rate of the reaction reached of 97%.
Keywords/Search Tags:phase-transfer catalysis, dual phase diagram, chemical shift, cooling curves, hydrogenation experiment, hydrogenation rate
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