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含能材料  2014 

5,5′-联四唑-1,1′-二氧二羟铵(TKX-50)50克量级制备放大工艺

DOI: 10.11943/j.issn.1006-9941.2014.06.006

Keywords: 有机化学,合成,5,5′-联四唑-1,1′-二氧二羟铵(TKX-50)

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Abstract:

为获得绿色低感高能炸药,研究了5,5′-联四唑-1,1′-二氧二羟铵(TKX-50)的50克量级制备方法。以乙二醛为起始原料,通过肟化、氯代、叠氮化、环合制得了关键中间体5,5′-联四唑-1,1′-二羟基二水合物(1,1′-BTO),1,1′-BTO与羟胺水溶液成盐直接制备出目标物TKX-50,产品经1HNMR,IR,MS,DSC和元素分析确证结构。重点考察了由1,1′-BTO制备TKX-50反应中投料比、时间及温度对收率的影响,确定了适宜的工艺条件:投料摩尔比n(1,1′-BTO)∶n(NH2OH·HCl)∶n(NaOH)=1∶2.2∶2.2,反应时间1h,温度80℃时,单步反应收率80.1%。合成路线总收率为41.5%。

References

[1]  Bowers R C, Romans J B, Zisman W A.Mechanisms involved in impact sensitivity and desensitization of RDX[J].Industrial & Engineering Chemistry Product Research and Development, 1973,12(1): 2-13.
[2]  Sikder N, Sikder A K, Bulakh N R, et al.1,3,3-Trinitroazetidine(TNAZ), a melt-cast explosive: synthesis characterization and thermal behavior[J].Journal of Hazardous Materials, 2004,113(1-3): 35-43.
[3]  Eaton P E, Zhang M X, Gilardi R, et al.Octanitrocubane: a new nitrocarbon[J].Propellants, Explosives, Pyrotechnics, 2002,27(1): 1-6.
[4]  赵廷兴, 李磊, 董战, 等.硝基唑类含能化合物的合成研究进展[J].有机化学, 2014,34(2): 304-315.ZHAO Ting-xing, LI Lei, DONG Zhan, et al.Research progress on the synthesis of energetic nitroazoles[J].Chinese Journal of Organic Chemistry, 2014,34(2): 304-315.
[5]  Hiskey M, Chavez D.Insensitive high-nitrogen compounds[P].DE 2001776133.
[6]  朱周朔, 姜振明, 王鹏程, 等.5,5′-联四唑-1,1′-二氧二羟铵的合成及其性能研究[J].含能材料, 2014,22(3): 332-336.ZHU Zhou-shuo, WANG Peng-cheng, LU Ming, et al.Synthesis and properties of dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate[J].Chinese Journal of Energetic Materials(Hanneng Cailiao), 2014,22(3): 332-336.
[7]  Fischer N, Fischer D, Klaptke T M, et al.Pushing the limits of energetic materials: the synthesis and characterization of dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate[J].Journal of Materials Chemistry, 2012,22(38): 20418-20422.
[8]  Lachance B, Renoux A Y, Sarrazin M, et al.Toxicity and bioaccumulation of reduced TNT metabolites in the earthworm Eisenia andrei exposed to amended forest soil[J].Chemosphere, 2004,55(10): 1339-1348.
[9]  McLellan W, Hartley W R, Brower M.Health advisory for hexahydro-1,3,5-trinitro-1,3,5-triazinane.Technical Report PB90-273533[R].Office of Drinking Water, U.S.Environmental Protection Agency: Washington DC, 1988.
[10]  李志敏, 张建国, 张同来, 等.硝基四唑及其高氮化合物[J].化学进展, 2010,22(4): 639-647.LI Zhi-min, ZHANG Jian-guo, ZHANG Tong-lai, et al.Nitro-tetrazole and its high nitrogen-contented compounds[J].Progress in Chemistry, 2010,22(4): 639-647.
[11]  黄明,李洪珍,李金山.高氮含能化合物的合成及反应性[J].含能材料, 2006,14(6): 457-462.HUANG Ming, LI Hong-zhen, LI Jin-shan.Review on synthesis of high-nitrogen energetic compounds[J].Chinese Journal of Energetic Materials(Hanneng Cailiao), 2006,14(6): 457-462.
[12]  Gbel M, Karaghiosoff K, Klaptke T M, et al.Nitrotetrazolate-2N-oxides and the strategy of N-oxide introduction[J].Journal of the American Chemical Society, 2010,132(48): 17216-17226.
[13]  杨利, 高福磊, 凡庆涛, 等.咪唑类含能化合物的研究进展[J].含能材料, 2009,17(3): 374-379.YANG Li, GAO Fu-lei, FAN Qing-tao, et al.Progress in imidazolium-based energetic compounds[J].Chinese Journal of Energetic Materials (Hanneng Cailiao), 2009,17(3): 374-379.
[14]  杨世清, 岳守体.国外四嗪四唑类高氮含能材料研究进展[J].含能材料, 2003,11(4): 231-235.YANG Shi-qing, YUE Shou-ti.Progress in high-nitrogen energetic materials derived from tetrazine and tetrazole[J].Chinese Journal of Energetic Materials(Hanneng Cailiao), 2003,11(4): 231-235.
[15]  张兴高, 朱慧, 张炜, 等.高氮化合物在含能材料中的应用研究进展[J].含能材料, 2004,12(21): 48-53.ZHANG Xing-gao, ZHU Hui, ZHANG Wei, et al.Application development of poly-nitrogen compounds in energetic materials[J].Chinese Journal of Energetic Materials(Hanneng Cailiao), 2004,12(21): 48-53.
[16]  Boneberg F, Kirchner A, Klaptke T M, et al.A study of cyanotetrazole oxides and derivatives thereof[J].Chemistry An Asian Journal, 2013,8(1): 148-159.

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