TEX的合成研究

Study on the Synthesis of TEX

用廉价、易得的乙二醛和甲酰胺为原材料，合成了中间体1，4-二甲醛-2，3，5，6-四羟基哌嚎（THDFP），然后在质量分数98%的浓硫酸和发烟硝酸作用下，采用低温下加料，使其充分反应生成笼形化合物后，再升温进行硝化的方法，合成了笼形硝胺炸药4，10-二硝基-2，6，8，12-四氧杂-4，10-二氮杂四环[5．5．0．0^5.9 0^3.11]十二烷（TEX），其纯度为99．5％，总收率为34．8％。研究了THDEP干燥时间、加料温度和反应温度对合成TEX纯度和收率的影响。结果表明，充分干燥的THDEP对合成有利，加料温度应控制在45～50℃为宜，最佳反应温度为70～80℃。

1,4-Diformyl-2,3,5,6-tetrahydroxypiperazine （THDFP） was synthesized with glyoxal and amides as primary substance. The cage explosive 4, 10-dinitro-2, 6, 8-12-tetraoxa-4, 10-diazatetracyclo-[5.5.0.0^5.9 0^3.11] -dodecane （TEX） was prepared using the method that taking THDFP into 98% H2SO4 and fuming HNO3 at lower temperature, producing enough the cage compound, then carrying out nitration in higher tempreture. The purity and overall yield of TEX are 99.5% and 34.8% ,respectivety. The effect of THDFP dry time, the temperature of adding material and reaction tempreture on the synthesis of TEX were studied. Results show that THDFP of full dried for synthesis is favored, should controll the temperature of adding material in the range 45- 50℃ and the reaction tempreture in the range of 75-80℃.