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Study on the Preparation Process of HMX¡¢TEX Catalyzed by Solid Acid

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Tutor: LuMing
School: Nanjing University of Technology and Engineering
Course: Applied Chemistry
Keywords: solid super acid,heteropoly acid,HMX,TEX,density functional theory
CLC: TQ564
Type: Master's thesis
Year:  2014
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1,3,5,7-Tetranitro-1,3,5,7-tetrazacyclooctane (HMX) and4,10-Dinitro-2,6,8,12-Tetraoxa-4,10-Diazatetracyclo-[]-dodecane (TEX) are relatively good overall performance of energetic materials. Solid acid as acid catalysts with easy recovery, less corrosive to equipment.which have been applied in the preparation of HMX and TEX.The best preparation process of DPT was obtained in the SO42-/ZrO2-WO3/HNO3system:SO42-/ZrO2-WO3(0.15)(2.2g) was added to14mL of anhydrous nitric acid, then urea (3g) was added, and stirred for90min at5¡æ,The mixture was poured into ice-water (30g) and reacted for60min at15¡æ, then22mL of a37%formaldehyde solution and H2O(50mL) was added. The mixture was stirred for40min at40¡æ, then cooled to20¡æ, and neutralized to pH7.0with aqueous ammonia. The yield of DPT was36.5%.The optimal synthesis conditions of HMX were investigated in the magnetic solid acid system (SO42-/ZrO2-TiO2-Fe2O3/HNO3). SO42-/ZrO2-TiO2-Fe2O3(1:1)(1.8g) was added to14mL of anhydrous nitric acid, and DPT(2.18g) was added to the mixture under the temperature of5¡æ,stirred for30min.The mixture was heated to30¡æand stirred for40min.Then the mixture was poured into ice-water (30g) and the reaction was ended. The yield of HMX was43.6%.The nitrolysis process of DPT was researched by quantum chemistry in concerning of the low yield of HMX. Electron cloud density, bond length, bond energy, bond order were analyzed. The BED of C(23)-N(13) and C(3)-N(13) in DPT are very closely, which are respectively281.23kJ/mol and282.75kJ/mol. Therefore, the controlling of nitrated intensity has a great influence on the yield of HMX. The BED of C(27)-N(15) and C(1)-N(15) in the intermediate with eight-membered ring are respectively348.54kJ/mol and258.77kJ/mol, C(27)-N(15) is hard to break and has an influence on the yield of HMX.The optimal reaction conditions of synthesis of TEX by using1,4-diformyl-2,3,5,6-tetrahydroxypiperazine (DFTHP) as raw material and HPA as catalyst:HPA(2g) was added to20mL of frozen anhydrous nitric acid, then DFTHP(2g) and urea(0.5g) were added to the mixture and the reaction temperature was controlled below50¡æfor20min. The mixture was heated to60¡æand stirred for40min. The yield of TEX was44.7%. The mechanism of synthesis of TEX was also investigated.
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