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Study On The Synthesis Technique Optimization And Application Research Of 1-methyl-4,5-dinitroimidazole

Posted on:2013-04-06Degree:MasterType:Thesis
Country:ChinaCandidate:L L LiuFull Text:PDF
GTID:2231330371468566Subject:Chemical Engineering
Abstract/Summary:PDF Full Text Request
1-methyl-4,5-nitroimidazole(4,5-MDNI) is a kind of insensitive elemental explosive withmelting pointlow sensitivity and high-energy, it could replace TNT as low melting pointcomp,onents used in novel insensitive melt-cast explosives, improving the safety of melt-castexplosives in the storage,transportation and the process of using. So it is important to studythe insensitive elemental explosive.4,5-MDNI was synthesized with N-methylimidazole as initial material by mixed acidmethod. The influences of reaction temperature and reaction time on the yield of 4,5-MDNIwas studied. An optional production condition was obtained by the orthogonal experiment:molar ratio of methyl-imidazole/fuming nitro acid/fuming sulfuric acid (1:3:6), reaction time(2h), reaction temperature (8085℃), the yield (48.6%). The purity of 4,5-MDNI wasidentified through TLC and HPLC, its structure was characterized by element analysis.IR.HNMR and ESI-MS.4,5-MDNI was synthesized by microwave method for the first time, The influences ofsingle factor experiment on the yield was studied. An optional production condition wasobtained, microwave radiation power is 500W, time is 40min, molar ratio ofmethyl-imidazole, fuming nitro acid, fuming sulfuric acid(20%) is 1:5.49:6.56, the yield is32.5%. The purity of 4,5-MDNI was identified, and its structure was characterized.Explosive rate and detonation pressure of 4,5-MDNI was determined and estimated,explosive rate is 7093m/s by Model FJZ-250 high speed rotating mirror framingcamera.Detonation rate is 7605m/s, and explosion pressure is 24.2GPa by experience ofKamlet formula.Determination value with calculated value are not significant.The DSC-TGtechniques were used to study the thermal behavior of 4,5-MDNI. the reaction kineticsparameters of E=92.98KJ/mol, A=109.68S-1and r=0.997 were ascertained by using theKissinge’s equation.The solubility of 4,5-MDNI in nitric acid, distilled water and ethanol three kind of solventswere determined at different temperatures by the laser monitoringobservation technique.The shrinkage of TNT and 4,5-the MDNI were determinated, shrinkage, the shrinkage of4,5-MDNI is lower than TNT small. According to different proportion, 4,5-MDNI and RDXwere made into new melt-cast explosives, and there shrinkage were determined, thereshrinkage are lower than the shrinkage of TNT, Their theory explosive rate and detonationpressure are estimatedby experience of Kamlet formula.
Keywords/Search Tags:1-Methyl-4,5-Nitroimidazole, Optimization of Process, Microwave, Solubility, Melt-cast Explosives
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