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Study On Synthesis And Performance Of TEX

Posted on:2017-02-05Degree:MasterType:Thesis
Country:ChinaCandidate:L TianFull Text:PDF
GTID:2271330488961198Subject:Applied Chemistry
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4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo-[5.5.0.05,9.0311]dodecane (TEX) is a typical cage type of energetic materials which has good thermal stability and detonation per-formance. But there are some shortcomings about the traditional TEX synthesis, such as low yield and side effects. In this paper, TEX was synthesized by two steps with formamide and 40% glyoxal as raw materials. The yield of TEX increased significantly, when the surfactant was added to the mixed acid system. In addition, the study on TEX recrystallization was re-searched, the results showed that the TEX crystal had intact structure, better thermal stability and greater mechanical properties.(1) 1,4-Diformyl-2,3,5,6-tetrahydroxypiperazine(DFTHP) was synthesized with 40% glyoxal and amides as primary substances. TEX was obtained by nitrolysis of DFTHP using a mixture of fuming nitric and concentrated sulfuric acid. Its structure was characterized by nuclear magnetic resonance (NMR) and fourier transform infrared (FTIR). The reaction mechanism was proposed and the key factors affecting the yield and purity of TEX were studied. As a result, the optimal conditions obtained were as follows:nitration temperature, 55℃; volume ratio of fuming nitric and concentrated sulfuric acid,4:3, selecting PEG400 as reaction catalyst and mass ratio of PEG400 and DFTHP,0.15:1. Under the optimal conditions, the yield was 59.8%, and the purity was 99.2%.(2) The different morphologies crystals of TEX were obtained from sol vent-nonsol vent recrystallization with difference solvents such as acctone, cyclohexacctone, butyrolacetone, dimethyl sulfoxideand N,N-dimethyl formamide. When the solvent was dimethyl sulfoxideand, TEX crystal had intact structure and uniform particle size. After recrystallization, the average particle size of TEX was 18.588 μm, it was smaller than raw material TEX. When the heating rate was 10℃/min, the peak temperature of TEX was 305.88℃. Compared with the raw material TEX, the peak temperature was increased by 4.72℃, the TEX crystal had better thermal stability. After recrystallization, the impact sensitivity of TEX was 8%, the friction sensitivity of TEX was 0, and the TEX crystal had a low sensitivity. In summary, the TEX had more excellent performances than raw material...
Keywords/Search Tags:cage type of energetic materials, 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazate- tracyclo-[5.5.0.05,9.03,11]dodecane, nonionic surfactant, recrystallization
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