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Nitrolysis Synthesis Of TEX By N2O5/HNO3

Posted on:2017-04-15Degree:MasterType:Thesis
Country:ChinaCandidate:L J TangFull Text:PDF
GTID:2271330488961446Subject:Chemical engineering
Abstract/Summary:PDF Full Text Request
4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazaisowutrzitane (TEX) is considered to be the better comprehensive properties energetic material.For the preparation of TEX by mixed acid result in pollution of the environment and low yield, N2O5/HNO3 as the nitrating agent was taken, nitrolysis synthesis of TEX was studied as follows.The synthesis process of target product 4,10-dinitro-2,6,8,12-tetraoxa-4,10 diazaisowutrzitane was optimized using N2O5/HNO3 as nitrating agent and 1,4-diformyl-2,3,5, 6-tetrahydroxypiperazine (DFTHP) as substrates. Using the single factor variable method to look for optimization of synthesis of the target product TEX. Results showed that the optimum conditions are:feed temperature of 40℃, reaction temperature of 75℃, reaction time of 40min, and charging ratio of m(DFTHP)/g:m(N2O5)/g:V(HNO3)/mL of 2:1:20, with a yield of 45.6% and TEX purity of 96.5%.The effect of surfactants, acidic ionic liquids and other catalysts on the yield and purity of TEX were discussed. Using sixteen alkyl three methyl bromide (CTAB), [Et3N(CH24SO3H][HSO4] or 10%CF3SO3H/resin as catalysts, the yield of TEX can be further increases by 3%-14%.At the same time, the reaction was also studied in the other three different substituted piperazines under optimal conditions, obtained under the experimental conditions of this paper, using DFTHP as the substrate when the best yield.Compared with the mixed acid method of the preparation process, the synthesis process of TEX using N2O5/HNO3 as nitrating agent, eliminating sulfuric acid pollution, showing good prospects for industrial applications. A series of studies on the catalyst can also be seen that the yield of the reaction is still great space for improvement. Different substrates nitrolysis also shows that the diversity of synthetic pathway.
Keywords/Search Tags:TEX, nitrogen pentoxide, nitrolysis, surfactant, acidic ionic liquid, synthesis
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