Center for Energetic Concepts Development, Department of Mechanical Engineering, University of Maryland

References for Chapter 4 "Synthesis"

1. Synthesis of HMX from DPT by Green Nitrolysis with Dinitrogen Pentoxide, He Zhi-yong, [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Luo Jun, [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Lü Chun-xu, [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Xu Rong, [Institute of Chemical Materials, CAEP, Mianyang Sichuan 621900, China], Li Jin-shan, [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2010, 33(2):1-4.

Abstract: In order to achieve a clean synthesis process of HMX, nitrolysis of DPT in two nitration systems was investigated. Nitrolysis of DPT in N2O5/organic solvent systems was investigated to yield little HMX but mainly complex by-products with low melting point ,indicating that the solutions of N2O5 in organic solvents was not suitable for this process. Nitrolysis in N2O5/HNO3 system was investigated. The effect of reaction time, reaction temperature, amount of ammonium nitrate and ratio of raw materials on the yield of HMX were studied, finding that yield of HMX increases first and then decreases along with the increasing usage of N2O5 and N2O5/HNO3 system was suitable for the nitrolysis of DPT because it could give HMX in a high yield up to 58% and purity of 99% under optimized conditions :n(N2O5):n(DPT)=2:1,n(HNO3):n(DPT)=36:1,react time 30min and react temperature 25°C.

2. Synthesis and Performance of Polyaryloxyphosphazene, Wang Zhi-feng, [Ningbo Branch of Academy of Ordnance Science, Ningbo 315103, China], Cao Ji-ping, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Yao Nan, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], WANG Jian-zhong, [Ningbo Branch of Academy of Ordnance Science, Ningbo 315103, China], Chinese Journal of Explosives & Propellants. 2010, Chinese Journal of Explosives & Propellants. 2010, 33(2):61-64.

Abstract: Polyaryloxyphosphazene was obtained with aryloxy substituting chlorine atom of the linear polydichlorophosphazene, which was synthesized by solution polymerization of hexachlorocyclotriphosphazene. The polymer was characterized by IR spectrum and analyzed by GPC, DMA, TGA, and thermal conductivity. The results show that the polymer obtained is polyaryloxyphosphazene with number-average molecular weight ranging from 38343 to 44625 and dispersion degree ranging from 3.0305 to 4.8857.The peak temperature of the initial thermal decomposition is 374.23℃ and of main decomposition reaction is 397.78℃.The weight of the polymer which shows obvious weight loss at the temperature of 461.14℃ and 529.95℃ could remain 45.40% at the temperature of 565.37℃ and then keep constant. It can be expected that the polymer has good thermal stability at high temperature. The glass transition temperature of the polymer is-24.09℃ and the thermal conductivity 0.21 W/(m•K).

3. Progress of Study on the Synthesis of Azole Energetic Ionic Compounds, Liu Xiao-jian, [School of Life Science, Beijing Institute of Technology, Beijing 100081, China], Zhang Hui-juan, [School of Life Science, Beijing Institute of Technology, Beijing 100081, China], Lin Qiu-han, [School of Life Science, Beijing Institute of Technology, Beijing 100081, China], Li Yu-chuan, [School of Life Science, Beijing Institute of Technology, Beijing 100081, China], Li Ya-yu, [Beijing Institute of Aerospace Testing Technology, Beijing 100074, China], Pang Si-ping, [School of Life Science, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2010, 33(1):6-10.

Abstract:The synthesis of energetic salts comprising imidazole, triazole, tetrazole and pentazole as precursors are reviewed with 36 references. The physiochemical properties of these new energetic salts, such as melting point, density, enthalpy of formation and detonation performance, as well as the effect of molecular structure and substituted groups on properties are summarized. The applications of these compounds in explosives and propellants are discussed.

4. Synthesis of 3, 4-Epoxybutanol Nitrate, Mo Hong-chang, Gan Xiao-xian, Li Na, Xing Ying, Han Tao, Zhang Zhi-gang, Li Lei, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2010, 33(1):24-26.

Abstract: 3,4-Epoxybutanol nitrate was synthesized with 3-butane-1-ol as raw material via two-step reactions, nitration and epoxidation, and characterized by IR,1HNMR and elemental analysis. The optimum nitration reaction conditions are as follows: n(HNO3)∶n(EBO)=1.5∶1.0,reaction temperature,-10℃ and the reaction was quenched after addition was over when temperature began to descend. The yield of nitrating reaction is 65.2%.The purity of the product is 98.2%.

5. Synthesis of 3, 4-Diphenylfuroxan with High Efficiency, Xue Yun-na, Yang Jian-ming, Li Chun-ying, Lü Jian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2010, 33(1):34-37.

Abstract: 3,4-Diphenylfuroxan was synthesized using benzil as starting material via hydro amine addition and oxidative cyclization.Its molecular structure has been identified with IR,1H NMR,13C NMR and elemental analyses.The effect of the category,dosage,mass fraction of oxidants and reaction temperature on the cyclization were investigated.Under the condition of HClO(mass fraction 7.39%) as oxidant,n(HClO)∶n(diphenylgly-oxime)=3,reaction temperature 80℃,atmospheric pressure and reaction time 1.5h,the yield of 3,4-diphenylfuroxan was 92.8%.

6. Syntheses of CHZ and PA Energetic Compounds and Their Effects on Thermal Decomposition of CL-20, Zhang Guo-tao, Zhang Tong-lai, Liu Jun-wei, Zhang Jian-guo, Yang Li, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2010, 33(1):38-42.

Abstract: Three kinds of energetic complexes, Co(CHZ)4(PA)2•3H2O,Cu(CHZ)4(PA)2•4H2O and Pb(CHZ)2(PA)2•4H2O(CHZ= carbodihydrazide, PA=picric acid),were synthesized with carbohydrazide, picric acid and corresponding metallic(Co, Cu, Pb) salts. The molecular formulas of these coordination compounds were derived by using elemental analyses and FTIR techniques. The friction, impact and flame sensitivities of the complexes were tested followed by the standard methods. The effects of the energetic complexes on the thermal decomposition of CL-20 were studied by means of DSC and TG-DTG techniques. The results show that the addition of those complexes make the onset temperature and peak temperature of CL-20 shift to low temperature. The kinetic parameters Ea and A of the first exothermic decomposition process for complexes/CL-20 mixture were calculated by Kissingér′s method and Ozawa-Doyle’s method. Cu(CHZ)(PA) and(CHZ)(PA) make the Ea value of the exothermic processes of CL-20 decrease from 222.8kJ/mol to 186.6kJ/mol and 183.0kJ/mol.

7. Synthesis, Crystal Structure and Sensitivity of [Mn(IMI)_6](ClO_4)_2, Ren Yan, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Yan Ying-jun, [Jiangxi Journalism and Publication College, Nanchang 330224, China], Yang Li, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Zhang Tong-lai, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Zhang Jian-guo, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Yu Kai-bei, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2009, 32(6):15-19.

Abstract: An energetic compound [Mn(IMI)6](ClO4)2(IMI:imidazolium) was synthesized by reaction of imidazolium with Mn(ClO4)2 in aqueous solution. Single crystal of [Mn(IMI)6](ClO4)2 was obtained. The compound was characterized by elemental analysis, TG-DTG and single crystal X-ray diffraction analysis. The results show that the crystal belongs to a monoclinic system with P2(1)/n space group and cell parameters of a=11.721(2)nm,b=7.2191(13)nm,c=16.402(3)nm,β=90.064(3)°,V=1387.9(4)nm3;Dc=1.585g/cm3;Z=2;F(000)= 678,μ=0.160mm,R1=0.0367,ωR2=0.1372.The title compound [Mn(IMI)6](ClO4)2formed by [Mn(IMI)6]2+ and(ClO4)-belongs to an ionic compound. The central Mn(II) ion is six-coordinated with six imidazole molecules. At a heating rate of 10K/min, the thermal decomposition process of the title compound consists of one endothermic peak and one exothermic peak with 9.9% residues. The mechanic sensitivity test results show that this compound is an insensitive energetic compound.

8. Synthesis and Thermal Decomposition Kinetics of TATB without Chloride, Ma Xiao-ming, Li Bin-dong, Lü Chun-xu, Lu Ming, [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2009, 32(6):24-27.

Abstract: In order to solve the influence of chloride in the traditional synthesis of TATB, taking phoroglucinol as primary material,1,3,5-triamino-2,4,6-trinitrobeneze(TATB) was synthesized by nitration with N2O5,methylation and amination, and its structure was identified by NMR,IR and MS. The effect of amination reaction on the yield and thermal decomposition property of TATB was investigated, the total yield of crude TATB was 92%.High-purity TATB was obtained by organic solvent recrystallization with yield of 75%.Thermal properties of TATB was analyzed by DSC and TG, the thermal decompositon activation energy and pre-exponential factor of TATB obtained by Ozawa′s equation are ETATB=135.28kJ/mol, ATATB=2.340×109s-1.

9. Application of Crystal Modifier in the Synthesis of Nitrophenol Potassium Salts, Tang Zhan, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Yang Li, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Yan Ying-jun, [Jiangxi Journalism and Publication College, Nanchang 330224, China], Zhang Tong-lai, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Zhang Jian-Guo, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Qian Xiao-jing, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2009, 32(6):28-30, 34.

Abstract:In order to attain the amount of crystal modifier in synthesis of nitrophenol potassium salts, the grained KPA was synthesized with the nonionic surfactant that containing H in the functional group served as crystal modifier. The surface tension and data of the surfactant, which will provide theoretical support for the dosage of surfactant, was studied. The grained KPA obtained in different conditions was studied with X-ray powder diffraction and the important growth facet that has more influence on the morphology was analyzed. The results show that the surfactant can reduce the strongest diffraction peaks and affect the dominant crystal facet, so they can control crystal morphology of KPA. Grained crystal can be gained if choosing appropriate surfactant and dosage through measuring surface tension of surfactant.

10. Structure, Thermodynamics and Sensitivity Property of (TAGH)ClO_4, Qi Shu-yuan, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Zhang Tong-lai, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Ao Guo-jun, [East China Research Institute of Microelectronics, Hefei 230022, China], Zhang Jian-guo, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Yang Li, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2009, 32(6):35-39.

Abstract: Triaminoguandine perchlorate was synthesized with triaminoguandine and perchloric acid as primary materials. The crystal structure was determined by X-ray single crystal diffraction analysis.The results show that the title compound belongs to monoclinic system with P2(1)/c space group and cell parameters of a=1.0213(11)nm, b=1.4869(15)nm, c=1.0936(11)nm, β=102.91(2)°. The title compound, with formula of CH9ClN6O4,is an ionic compound formed by [C(N2H3)3]+ and ClO-4.There are a lot of intramolecular and intermolecular hydrogen bonds, which make it stable. The title compound was characterized by elemental analysis, FTIR, DSC, TG-DTG. The results show that the title compound lost 99.7% at 457.03℃ with a heating rate of 10℃/min. The sensitivity test results show that it has low friction sensitivity and has no frame sensitivity and impact sensitivity under the sensitivity test conditions.

11. Synthesis and Characterization of 3, 4-Bis(pyrazine-2′yl) furoxan, Li Ya-nan, Zhang Zhi-zhong, Zhou Yan-shui, Chen Bin, Wang Bo-zhou, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2009, 32(6):34-37.

Abstract: 3,4-Bis(pyrazine-2′-yl)furoxan(DPF) was synthesized using 2-cyanopyrazine as raw material, via four-step reactions of oxime, diazotization, denitrification and cyclization and the overall yield was 51.0%.The structures of target compound and intermediates were characterized by IR,NMR,MS and elemental analysis. The mechanism of cyclization reaction was investigated. The affecting factors of reactions were optimized. The optimum reaction conditions of cyclization were: molar ratio nexp∶ntheory=1.10-1.25 for Na2CO3, reaction temperature 2 to 10℃ and reaction time 4h.The yield of DPF is about 75.6% and purity 99.0%.

12. Synthesis, Crystal Structure and Quantum Chemistry of C_3N_2H_5~+C_6N_3O_7H_2~, Li Dan, [School of Chemical Engineering/Shaanxi Key Laboratory of Physico-inorganic Chemistry, Northwest University, Xi'an 710069, China], Ren Ying-hui, [School of Chemical Engineering/Shaanxi Key Laboratory of Physico-inorganic Chemistry, Northwest University, Xi'an 710069, China], Zhao Feng-qi, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Yi Jian-hua, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chang Chun-ran, [School of Chemical Engineering/Shaanxi Key Laboratory of Physico-inorganic Chemistry, Northwest University, Xi'an 710069, China], Song Ji-rong, [Conservation Technology Department, The Palace Museum, Beijing 100009, China], Chinese Journal of Explosives & Propellants. 2009, 32(6): 48-52.

Abstract: C3N2H5+C6N3O7H2- were prepared by mixing imidazole ethanol solution and picric acid (PA) ethanol solution. Single crystals suitable for X-ray measurement were cultured at room temperature. The crystal is rhombic system, space group Pbca with crystal parameters of a=0.8950nm, b=1.3474(3)nm, c=2.0164nm, α=β=γ=90°, V=2.4317(3)nm3, Dc=1.624g/cm3, Z=8, F(000)=1216. The theoretical investigation of the title compound as a structure unit was carried out by HF/6-311+G(d) and B3LYP/6-311+G(d) methods in Gaussian 03 package, and the atomic net charges and the population analysis was discussed.

13. Synthesis and Characterization of 7-Chloro-4, 6-dinitro-benzofuroxans, Huo Huan, Wang Bo-zhou, Liu Qian, Luo Yi-fen, Zhang Ye-gao, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2009, 32(4):31-33.

Abstract: Taking 4-chloro-2-nitroaniline as primary material, 7-chloro-4, 6-dinitro-benzfuroxan was synthesized by the process of oxidation, cyclization, nitration and rearrangement. Its structure was characterized by IR, NMR and elemental analysis. The effect of the nitration reaction temperature and 5-chlorobenzfuroxan/nitric acid mole ratio on the yield was studied. The best condition of nitration reaction was reaction temperature, 60℃; 5-chlorobenzfuroxan/nitric acid mole ratio, 1∶10. The yield is 39%.

14. Energized Synthesis and Characterization of 1, 3, 5-Tris (2-hydroxy ethyl) -1, 3, 5-triazinane-2, 4, 6-trione, Xu Ruo-qian, JiYue-ping, Ding Feng, Yang Wei, Liu Wei-xiao, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2009, 32(4):38-40, 44.

Abstract: Taking 1, 3, 5-tris(2-hydroxyethyl)-1, 3, 5-triazinane-2, 4, 6-trione as primary material, 1, 3, 5-tris(2-nitroethyl)-1, 3, 5-triazinane-2, 4, 6-trione(TNEIC) and 1, 3, 5-tris(2-azidoethyl)-1, 3, 5-triazinane-2, 4, 6-trione(TAEIC) were synthesized via nitration and azidonation. The optimum conditions of nitration were: HNO3/H2SO4 (volume ratio), 1∶1; reaction temperature, 25℃; reaction time, 0.25 h and the optimum reaction yield are 92.0%. By elemental analysis, infrared spectroscopy (IR), nuclear magnetic resonance spectroscopy (1H NMR), and identified the target product structure, analysis using DSC, the thermal properties of the compounds were determined. The results show that TAEIC has a low melting point and will be used in melt-cast explosive.

15. Preparation of Fe_2O_3/CNTs and Its Catalytic Mechanism on Thermal Decomposition of RDX, Cui Qing-zhong, Jiao Qing-jie, Zhao Wei-dong, [National Key Laboratory of Explosive Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2009, 32(4):42-44.

Abstract: 1-Methyl-2, 4, 5-trinitroimidazoles (MTNI) was synthesized with 1-methylimidazole as initial material by two steps nitrification reaction. Its structure was characterized by IR, 1 H NMR and elemental analysis. The effect of the drip order, ratios of volume for nitric and sulfuric acid, reaction time, temperature on the yield of 2, 4-dinitroimidasole (2, 4-MDNI) and MTNI was investigated. The results show that the conditions of good yields are: the drip order of additive of the first step, ratios of volume for nitric and sulfuric acid 1∶2, the drip order of anti-additive for the second step, ratios volume for nitric and sulfuric acid 1∶4, reaction time 2 h, temperature 110~115℃.

16. New Technology for Synthesis of 1-Methyl-2, 4, 5-trinitroimidazoles, Wang Xiao-jun, Cao Duan-lin, Li Yong-xiang, Song Lei, Wang Jian-long, [College of Chemical Engineering and Environment, North University of China, Taiyuan 030051, China], Chinese Journal of Explosives & Propellants. 2009, 32(3):16-18.

Abstract: 1-Methyl-2, 4, 5-trinitroimidazole (MTNI) was synthesized with imidazole as starting material via a 5-step sequence of reactions (nitration, thermal rearrangement, methylation, etc). The total yield is 15.6%, and its purity is more than 98%. The structure of MTNI was characterized by IR, NMR and elemental analyses. The thermal decomposition performance of MTNI was tested by DSC. The results show that the detonation performances were comparable to those of RDX, and better than TATB. MTNI is a new insensitive high explosive with its friction sensitivity similar with TNT and impact sensitivity similar with comp B. The exothermic decomposition of MTNI proceeds in three stages. The corresponding peak temperature is 177,223 and 298℃, and decomposition heat 327.67, 11.2 and 54.84kJ/mol, respectively.

17. Synthesis of Acrylated Span80 and Its Application in Emulsion Explosive, Qian Hua, Liu Da-bin, Ye Zhi-wen, [Collage of Chemical and Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2009, 32(2):11-13, 20.

Abstract: The acrylated Span80 was synthesized by the starifying method of acryloyl chloride. The effects of reaction time, temperature and solvent etc. on acrylated Span80 were investigated. The optimum conditions of the reaction were: triethylamine as catalyst, n(acrylic acid)∶n(thionyl chloride)∶n(Span80)∶n(triethylamine)= 1.0∶2.1∶1.0∶1.4,reaction time 3 h, reaction temperature 50℃ and 80 mL toluene /mol-acrylic acid as solvent. The iodine value of acrylated Span80 obtained by using optimum conditions was 94.9 7 g I2/100 g sample. The effect of acrylated Span80 and ordinary Span80 on properties of emulsion explosive was compared by SEM and the performance test. The results show that this acrylated Span80 has better emulsified property than ordinary Span80.

18. Green Synthesis of Glycidyl Nitrate, Wang Qing-fa, [Key Laboratory for Green Chemical Technology of State Education Ministry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China], SHI Fei, [Shandong Silk Textile Vocation College, Zibo Shandong 255300, China], ZHANG Xiang-wen, [Key Laboratory for Green Chemical Technology of State Education Ministry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China], WANG Li, [Key Laboratory for Green Chemical Technology of State Education Ministry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China], MI Zhen-tao, [Key Laboratory for Green Chemical Technology of State Education Ministry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China], Chinese Journal of Explosives & Propellants. 2009, 32(2):14-16.

Abstract: A mild and high efficient method to prepare glycidyl nitrate by selective nitration of glycidol with dinitrogen pentoxide as the nitrating agent was developed. The influences of molar ratio of dinitrogen pentoxide to glycidol, reaction temperature and reaction time on the nitration of glycidol were investigated. The results indicated that the selectivity of 100% and the yield of 94% for glycidyl nitrate were obtained by carrying out the reaction at-15℃ for 6 min with the molar ratio of dinitrogen pentoxide to glycidol at 1∶1.

19. Preparation of Zirconium 3-Nitrophthalate and Its Effect on Combustion of Double-base Propellant and RDX-CMDB Propellant, Zhang Heng, Zhao Feng-qi, Zhang Xiao-hong, Pei Qing, Hao Hai-xia, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2009, 32(1):1-4.

Abstract: Zirconium 3-nitrophthalate(Zr(3-NO2-PHT)2•2H2O) was synthesized by using 3-nitrophthalic acid, sodium hydroxide, and zirconyl nitrate as raw materials, and the structure was determined by elemental analysis, X-ray fluorescence diffraction and FT-IR spectra. The catalytic action of zirconium 3-nitrophthalate on double-base propellant and RDXCMDB propellant was analyzed. The results show that the burning rates of the double-base propellant and RDX-CMDB propellant increase obviously in the low pressure range and the pressure exponents of the double-base propellant decrease obviously in the middle and high pressure range. Especially, when Zirconium 3-nitrophthalate together with copper salts is used, the catalytic efficiency is higher.

20. Synthesis and Crystal Structure of 3, 3'-Dinitro-5, 5'-azo-1H-1, 2, 4-triazole(DNAT), Jia Si-yuan, WANG Xi-jie, Wang Bo-zhou, Xiong Cun-liang, Liu Qian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2009, 32(1):25-25, 39.

Abstract: 3,3'-Dinitro-5,5'-azo-1H-1,2,4-triazole(DNAT) was synthesized by the oxidative coupling of 5-amino-5-nitro1,2,4-triazole(ANTA) as raw material. Its structure was characterized by IR, NMR and elemental analyses. The crucial factors and mechanism in the coupling reaction were explored and the synthetical conditions were optimized. Some properties of DNAT were measured. The H50of 17.08cm (drop hammer 5kg) and friction sensitivity of 60%(pressure 3.92MPa,pendulum angle 90°)were obtained. The single crystal of DNAT•4H2O was cultivated, and its crystal structure was determined by X-ray crystallography. The crystal of DNAT•4H2O is monoclinic crystal system with space group P2(1)/n and Dc=1.550g•cm-3.

21. Synthesis and Characterization of 5-Vinyltetrazole, Liu Qing, Gan Ning, Han Tao, Zhang Zhi-gang, Li Na, Mo Hong-chang, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2009, 32(1):29-31.

Abstract: Hydroxyethyltetrazole was synthesized by the 1,3-polar cycloaddition of 3-hydroxypropanenitrile and NH4N3 that produced by the reaction of NaN3 and NH4Cl.The ultrasonic technology was applied in this reaction and the yield was up to 90.5%.5-Chloroethyltetrazole was prepared by the halogenation of hydroxyethyltetrazole and SO2Cl2 and the yield was 77%.5-Vinyltetrazole was obtained by the elimination of 5-chloroethyltetrazole under the condition of alkaline, and the yield was 70%.5-Chloroethyltetrazole and 5-vinyltetrazole were characterized by IR,1 HNMR and elemental analyses. The results show that the final product was the target product. This method has the advantages of high and stable yield and convenient preparation.

22. Synthesis and Characterization of Picrylfurazanether Compounds, Ge Zhong-xue, Qiu Shao-jun, Jiang Jun, Wang Xi-jie, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31 (6):17-20.

Abstract: In order to obtain high energy density materials with excellent synthetic performances, picryl(3-nitrofurazan-4) ether(FOP) and bis(3-nitrofurazan-4) picryl ether(DFOP) were synthesized by condensation of sodium hydroxyl nitrofurazan with picryl chloride(PcCl) and 2,4-dichloro-1,3,5-trinitrobenzene(DCPc), respectively. The products were characterized by FTIR, 1H NMR,13 C NMR,MS and elemental analyses. The optimal reaction conditions obtained are:FOP of the yield as 31% from PcCl, the mole ratio of PcCl to sodium nitrohydrofurazan 1.0∶1.1,reaction temperature 80℃,reaction time 16h,and for DFOP of the yield as 42% from DCPc, the mole ratio of DCPc to sodium nitrohydrofurazan 1.0∶2.7,reaction temperature 80℃,reaction time 2h.

23. Synthesis and Characterization of 1-Methyl-2, 4, 5-trinitroimidazole, Wang Wei, Yang Wei, Ji Yue-ping, Ding Feng, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31 (6):32-34, 38.

Abstract: 1-Methyl-2,4,5-trinitroimidazole(MTNI) was synthesized with imidazole as starting material via a 5-step sequence of reactions(nitration, thermal rearrangement, methylation, etc).The total yield is 15.6%,and its purity is more than 98%.The structure of MTNI was characterized by IR,NMR and elemental analyses. The thermal decomposition performance of MTNI was tested by DSC. The results show that the detonation performances were comparable to those of RDX, and better than TATB.MTNI is a new insensitive high explosive with its friction sensitivity similar with TNT and impact sensitivity similar with comp B. The exothermic decomposition of MTNI proceeds in three stages. The corresponding peak temperature are 177,223 and 298℃,and decomposition heat 327.67,11.2 and 54.84kJ/mol, respectively.

24. Synthesis and Characterization of Energetic Intermediate 5-Hydrazinotetrazole, Zhu Ya-hong, Sheng Di-lun, Chen Li-kui, Ma Feng-e, [Shaanxi Applied Physicochemical Research Institute, Xi'an 710061, China], Chinese Journal of Explosives & Propellants. 2008, 31(6):39-41.

Abstract: 5-Hydrazinotetrazole was synthesized with 5,5'-azotetrazolate as starting material by the acidizing of hydrochloric acid and recrystallizing of sodium acetate processes. Its structure was characterized by Fourier transform infrared, melting point and elemental analyses. The key factors affecting acidizing and recrystallizing of synthesis were discussed. The results show that the mass fraction of material used during acidizing is 10% for 5,5'-azotetrazolate solution and 10%-15% for hydrochloric acid solution. The yield of 5-hydrazinotetrazole is 55%-60%,and melting point is 196-198.9℃.

25. Synthesis and Characterization of 4, 4'-Dinitrodifurazalyl Ether, WANG Xi-jie, Ge Zhong-xue, Jiang Jun, Wang Bo-zhou, Zhang Ye-gao, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(6):12-14, 27.

Abstract: 4, 4’-Dinitrodifurazalyl ether (FOF-1) was synthesized from 3,4-diamino-furazan(DAF) after Caro-acid oxidation and etherification of nitro-group. Its structure was characterized by IR, MS, NMR and elemental analysis. The reaction mechanism of intermolecular etherification of nitro-group was preliminarily discussed. In addition, the synthetic procedures were optimized, and the optimal conditions of oxidization and intermolecular etherification reaction were determined. The best condition was obtained as follows: the oxidation reaction time is 3.5h,initial content of H2SO4 is 51.7%,the etherification reaction time is 2.5h, content of water is less than 0.03%, the overall yields is 42% and the purity is 99.6%.

26. Synthesis and Properties of Energetic Binder PNIMMO, Mo Hong-chang, Gan Xiao-xian, Xing Ying, Li Na, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(5):24-27.

Abstract: Using 1, 4-butanediol as initiator, boron trifluoride etherate as catalyst and CH2Cl2 as solvent, poly (3-nitratomethyl-3-methyl oxetane) (PNIMMO) was prepared by 3-nitratomethyl-3-methyloxetane via cationic ring-opening polymerization. The effect of molar ratio for catalyst and initiator, reaction temperature and the dropping rate of monomer on polymerization were discussed. The optimum conditions were determined as: molar ratio for catalyst and initiator was 0.50 - 0.75; reaction temperature was around 10℃ and dropping monomer slowly. The polymer was characterized by IR and 13C NMR. The results show that the glass transition temperature, the enthalpy of decomposition and the decomposition peak temperature of the polymer are -24.52℃, +1212J/g and 221.78℃, respectively. The mechanical properties of polyurethane film cured by N-100 are 3.5 - 3.7MPa for δ and 260%-280% for ε at room temperature.

27. Research Progress on Polynitroimidazoles and Their Derivatives, Yang Wei, Ji Yue-ping, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(5):46-50.

Abstract: Synthesis and properties of poly-nitro-imidazoles, such as di-nitro-imidazole, tri-nitro-imidazole and their derivatives and their application in energetic materials and medicines were summarized with 26 references. Nitro-imidazole was synthesized by nitration, thermal rearrangement and methylation with the imidazole or iodoimidazole as primary substance. Considering that tri-nitro-imidazole is a new insensitive high explosive with high formation enthalpy, fine thermal stability and relatively good safety characteristics.

28. Synthesis and Characterization of 3-Propargyl-5, 5-dimethylhydantoin, Zhang Li-na, Yang Rong-jie, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2008, 31(5):18-21.

Abstract: In order to improve the mechanical properties of solid propellant, a new bonding agent, 3-propargyl-5, 5-dimethylhydantoin (PDMH) was synthesized by the Gabriel method. The condition of the reaction was: n(DMH)∶n(propargylbromine)∶n(methyl alcohol solvent of KOH)=1∶1∶1, water as solvent, reaction temperature 65℃, reaction time 3h. The yield of PDMH was 50%. Chemical structure of PDMH was identified by FT-IR, NMR, MS and TGA-DTA. Melting point of PDMH is 170 - 171℃ and its decomposition temperature 185.5℃, it is expected to be used in composite solid propellant.

29. Synthesis and Characterization of 1, 5-Diazido-3-nitrazapentane(DIANP), Ji Yue-ping, Lan Ying, Li Pu-rui, Wang Wei, Ding Feng, Liu Ya-jing, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(3): 44-46.

Abstract: 1, 5-Diazido-3-nitrazapropant (DIANP) was synthesized from DINA and sodium azide, via azidation, extraction, washing, discolors filtration and vacuum distillation. Its structure was characterized by IR, NMR and elemental analyses. Relative properties were analyzed. The parameters affecting the yield, such as ratio, solvent, temperature and reaction time, were discussed. The results show that the optimum reaction condition of synthesizing DIANP is: the mass ratio of DINA to sodium azide, about 1∶0.59; solvent, DMSO; reaction temperature, 80 - 85℃ and reaction time, 7-8h. The yield of DIANP is about 80% and purity 98%.

30. Synthesis of 1, 3, 5-Tri-Substituted Perhydro-s-triazines, Yu Qin-wei, Yang Jian-ming, Zhao Feng-wei, Lü Jian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(3):50-52.

Abstract: 1, 3, 5-Tri-substituted perhydro-s-triazines were synthesized from nitriles (acetonitrile, propionitrile, butyronitxle and benzonitrile), and 1, 3, 5-trioxane. The products were characterized by 1H NMR, IR, MS and elemental analysis. The effects of ratios of raw materials, reaction temperature and reaction time on the yield were investigated by orthogonal experiment. Results show that on the optimal reaction conditions, the yields of the corresponding 1, 3, 5-tri-substituted perhydro-s-triazines synthesized from acetonitrile, propionitrile, butyronitrile, benzonitrile and 1, 3, 5-trioxane were 95.7%, 96.1%, 84.2% and 98.1%, respectively.

31. Synthesis and Properties of ETPE Based on BAMO/AMMO, Gan Xiao-xian, Li Na, Lu Xian-ming, Han Tao, Xing Ying, Liu Qing, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):81-85.

Abstract: Bromopolyether was prepared from 3-bromomethyl-3-methyl oxetane (BrMMO) by cation ring-opening polymerization. Azide polyether PAMMO was synthesized by theazido reaction of bromopolyether. Azide polyether PBAMO was prepared from 3, 3-bisbromomethyl oxetane (BAMO) by directly ring-opening polymerization. Using tetrahydrofuran as solvent, PBAMO as hard block, PAMMO as soft block, 2, 4-toluene diisocyanate (TDI) as diisocyanate monomer, butane-1, 4-diol urethane oligomer as linking compound, an energetic thermoplastic elastomer (ETPE) of number average molecular weight about 25,000 was prepared by one-step solution polymerization. ETPE that prepared was meltable and soluble. Its tensile strength and elongation at room temperature were about 5MPa and 400%, respectively.

32. Synthesis and Characterization of Bis(1, 3-diazido-2-propyl) formal(BDPF), Ji Yue-ping, Wang Wei, Ding Feng, Chen Bin, Yu Tao, Liu Wei-xiao, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):86-88.

Abstract: The intermediate bis(1, 3-dichloro-2-propyl) formal (BCPF) was prepared by condensation reaction in the presence of a catalyst with 1, 3-dichloro-2-propanol and polyformaldehyde as primary materials. The title compounds bis(1, 3-diazide-2-propyl) formal (BDPF) was obtained by BCDF reacted with a metal azide in a solvent with the yield of 98% and purity of 98%. Their structures were characterized by IR, NMR and elemental analysis. The effect of catalyst, solvent and reaction temperature on above mentioned reactions was studied. The optimum reaction conditions are: for condensation reaction, reaction temperature 0-5℃, 4mL sulfuric acid as catalyst, ethylene dichloride as dissolvent; for hydrazoate reaction, reaction temperature 95 - 99℃, dimethyl sulfoxide as dissolvent, reaction time 4h.

33. Synthesis and Characterization of 3-Bromonomethyl3-Methyloxetane Homopolymer, Dong Jun, Gan Xiao-xian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):89-92.

Abstract: Using 1, 4-butanediol (BDO) as initiator, boron-trifluoride etherate as catalyst, 3-bromomethyl-3-methyloxetane (BrMMO) as monomer, CH2Cl2 as solvent, an organic binder, 3-bromomethyl-3-methyloxetane homopolymer (PBrMMO), was synthesized by cationic ring-opening polymerization mechanism. The monomer conversion rate changes with time under low-temperature conditions were studied, and the BrMMO conversion rate-time curve was obtained. The effect of catalyst concentration and temperature of reaction system on polymerization were studied. The results show that the optimum conditions of the controlled polymerization are: n(BF3•Et2O)∶n(BDO)=0.5∶1.0, add the BrMMO in reaction system at 0℃ and keep reacting for three days. The structure and characterization of the final product were characterized by IR, 1H NMR, DSC and TGA.

34. Study Progress of Several High Energy Density Materials(HEDM), Zhang Zhi-zhong, Wang Bo-zhou, Ji Yue-ping, Zhou Yan-shui, Zhou Cheng, Liu Qian, Zhu Chun-hua, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):93-97, 101.

Abstract: The current situation of investigating five HEDMs (DNTF, ADN, TNAZ, FOX-12 and FOX-7) in China was summarized. Their synthesis methods, physicochemical and explosive properties, compatibility and applications in the formulation of explosive and propellant were introduced. DNTF shows an outstanding performance in composite explosives and explode network and is used as oxidant in propellant.ADN can be used as high energetic oxidant of the low specific signal propellant. TNAZ can be used in casting explosive and gun propellant.FOX-12 and FOX-7 are potential compositions of insensitive explosives, with 24 references.

35. Synthesis and Characterization of 1H, 4H-3, 6-Dinitropyrazolo [4, 3-c]pyrazole Amine Salts, Luo Yi-fen, Ge Zhong-xue, Wang Bo-zhou, Zhang Hai-hao, Xiong Cun-liang, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):98-101.

Abstract: Taking 1H, 4H-6-nitropyrazolo [4, 3-c] pyrazole-3-carboxy as primary material, 1H, 4H-3, 6-dinitropyrazolo [4, 3-c] pyrazole (DNPP) was synthesized by one step reaction of decarboxylation and nitration. By using DNPP as primary material, two DNPP amine salts, TAG-DNPP and GUDNPP, were synthesized with solid triaminoguanidinium (TAG) nitrate and solid guanidylurea (GU) hydrochloride, respectively. Their structures were confirmed by IR, 1 H NMR, 13C NMR and elemental analysis. The reaction mechanism of decarboxylation and nitration was investigated. Some reasons was analyzed for triaminoguanidinium 3, 6-dinitropyrazolo [4, 3-c] pyrazole as the gun propellant additive. The results show that the pyrolysis residue of TAG-DNPP can form new melon compounds. These novel compounds make flame temperature suppress and burning rate of the gun propellants improve.

36. Synthesis and Characterization of 3-Nitropyrazole and its Salts, Li Hong-li, Xiong Bin, Jiang Jun, Zheng Xiao-dong, Li Zhi-peng, Ma Yu-xia, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):102-104, 108.

Abstract: In order to synthesize the salts of 3-nitropyrazole, N-nitropyrazole was synthesized with pyrazole as raw material, and HNO3-Ac2O-HAc system as nitration agent. N-nitropyrazole at high temperature was rearranged as 3-nitropyrazole.Its organic copper and lead salts were synthesized by the reaction of 3-nitropyrazole with some inorganic copper and lead salts. The structure of products was characterized by melting point, IR, NMR and elemental analysis, showing that the products were target products. The optimum reaction yield was 85.5% for nitration, 92.8% for rearrangement reaction and 79.3% for total yield.

37. Synthesis and Properties of Azido Terminated Glycidyl Azide Polymer, Li Na, Gan Xiao-xian, Xing Ying, Mo Hong-chang, Zhang Zhi-gang, Han Tao, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(1):20-22.

Abstract: Using 1, 4-butanediol as initiator, boron-trifluoride etherate as catalyst, polyepichlorohydrin (PECH) was synthesized by the opening-ring polymerization of epichlorohydrin. Using the method of tosylation, tosylate terminated epichlorohydrin polymer as intermediate was synthesized by PECH and 4-toluenesulfonylzchloride in pyridine, azido terminated glycidyl azide polymer (ATGAP) was obtained by the reaction of intermediate and sodium azide. The structure of ATGAP was characterized by IR, 1H NMR and 13C NMR, showing that the final product was target product. The glass transition temperature of ATGAP was -73 ℃. Its thermal decomposition temperature was 252.7℃. ATGAP has small viscosity and can be used as an energetic plasticizer.

38. Synthesis of Poly(ether glycol)s Containing Isocyanurate Segments, Chang Hai, Fan Xiao-dong, Wang Sheng-jie, [Department of Applied Chemistry, School of Science, Northwestern Polytechnical University, Xi'an 710072, China], Chinese Journal of Explosives & Propellants. 2007, 30(6):13-16.

Abstract: The cationic ring-opening polymerizations of epoxide based monomers were studied using tris(2-hydrooxyethyl) isocyanurate (THEIC) as initiator and tri-fluoro-boron plus ether complex system as catalyst. It was found that the ring opening polymerizations of epoxide based monomers with THEIC can be carried out in a heterogeneous medium smoothly. However, using THEIC initiator, the reaction rate for epichlorohydrin is faster than that of propylene oxide and 2-butoxyxirane, respectively. By simply adjusting the monomer feeding sequence, the block poly(ether glycol) copolymers containing isocyanurate segments can be prepared successfully.

39. Synthesis of LLM-116 by VNS Reaction, Wang Ying-lei, Zhang Zhi-zhong, Wang Bo-zhou, Luo Yi-fen, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(6):20-23.

Abstract: 3,5-Dinitropyrazole ammonium salt was synthesized by rearranging 1, 3-dinitropyrazole as initial material and bubbling ammonia, and acidified to 3, 5-dinitropyrazole. 1, 1, 1-Trimethyhydrazinium iodide (TMHI) as a VNS agent was reacted with 3, 5-dinitropyrazole in the presence of t-Buok as catalyst to get 4-amino-3, 5-dinitropyrazole (LLM-116) through the VNS reaction. Their structures were confirmed by IR, NMR, MS and elemental analyses. The VNS reaction mechanism and factors of influencing the reaction were discussed. The results show that under optimal condition of TMHI as VNS reaction reagent and the reaction at 25 ℃ for 4 h, the yield of LLM-116 was 60%.

40. Preparation and Crystal Structure of [Cu(DNI)_2(H_2O)_2]•3H_2O, Cui Rong, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Zheng Xiao-dong, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Mao Zhi-hua, [Analytical and Testing Centre of Sichuan University, Chengdu 610041, China], Zhang Zhi-zhong, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Feng Li-min, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Yao Yi-lun, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Li Hong-li, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Jiang Jun, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(6):27-30.

Abstract: [Cu(DNI)2(H2O)2]•3H2O was prepared by the reaction of the aqueous solution of sodium 2, 4-dinitroimidazolate and copper sulfate. The single crystal of [Cu(DNI)2(H2O)2]•3H2O suitable for X-ray determination was obtained by slow evaporation method. The single crystal structure of [Cu(DNI)2(H2O)2]•3H2O has been determined by single crystal X-ray diffraction analysis. The crystal is triclinic, space group P-1 with crystal parameters of a=7.2560(10)×10-1 nm, b=7.762(2)×10-1 nm, c=16.685(3)×10-1 nm, α=87.13(3)°, β=83.81(3)°, γ=62.25(3)°, V=826.8(3)×10-3 nm3, Z=2, Dc=1.871 g•cm3, μ=1.411 mm-1, F(000)=470. The final deviation factor R is 0.0388. According to the analytical results of IR, the elemental analyses and X-ray diffraction, the chemical component of the 2, 4-DNI copper complex is C6H10CuN8O13 and its formula is [Cu(DNI)2(H2O)2]•3H2O.

41. Synthesis of 3-Bromonomethyl-3-Methyloxetane, Dong Jun, Gan Xiao-xian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2008, 31(2):89-92.

Abstract: The 3-bromomethyl-3-methyloxetane (BrMMO) was synthesized by the closed-ring reaction between 2, 2-dibromomethyl propanol (BBMP) as primary substance and alkali. The effect of kinds of alkali and its amount on the closed-ring yield of BBMP was discussed. The effect of the base concentration, reaction temperature and the reaction time on the yield of BrMMO in the closed-ring reaction was discussed. Under the reaction conditions of n(BBMP)∶n(NaOH)=1.0∶1.1, NaOH mass fraction 12%, reaction temperature 78℃, reaction time 4h, the yield of BrMMO was 65%. The structure of BrMMO was identified by elemental analysis, IR and 1 H NMR. The results showed that it was the target compound BrMMO. This experiment process was easy to do, raw material was liable to attain, and the solvent can be retrieved, so the pollution was small.

42. Synthesis of 2-Nitroimino-5-nitrohexahydro-1, 3, 5-triazine(NNHT), Zhang Hai-hao, Wang Bo-zhou, Liu Qian, Xiong Cun-liang, Jia Si-yuan, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(6):48-50.

Abstract: Taking formaldehyde, tert-butyl amine and nitroguanidine as primary materials, 2-nitroimino-5-nitrohexahydro-1, 3, 5triazine (NNHT) was obtained by the process of nitration and Mannich reaction. Its structure was identified by NMR, IR and elemental analysis. The effect of temperature on Mannich reaction was investigated, the yield reached 89% while the temperature was 80℃. The conditions of nitration were further optimized, the yield rose to 94% while the reaction was controlled under the room temperature. Instead of 100% nitric acid, industrial nitric acid was used in the nitration under the room temperature, and the yield was 88%.

43. Synthesis of BBMO and BAMO by Phase Transfer Catalysis Method, Zhang Zhi-gang, Lu Xian-ming, Gan Xiao-xian, Han Tao, Xing Ying, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(5):32-35.

Abstract: Using water and toluene as solvent, quaternary ammonium salt as phase transfer catalyst, under the effect of NaOH, 3, 3-dibromomethyl oxetane (BBMO) was synthesized by the cylization of 1, 1, 1-tribromomethyl-1-hydroxymethyl methane. Using water as solvent, quaternary ammonium salt as phase transfer catalyst, 3, 3-diazidomethyl oxetane (BAMO) was obtained by the substitution of BBMO with NaN3.The structure of BBMO and BAMO was identified by HNMR and FTIR. The yield and purity are 81% and 97.2% for BBMO, and 80.9% and 98.37% for BAMO. The results show that the synthesis of BBMO and BAMO by phase transfer catalysis possesses advantages of safety, high yield and high purity.

44. Synthesis and Application of the Heat-resistant Explosive PCS, Deng Ming-zhe, Ye Zhi-hu, Zhao Sheng-xiang, Tian Zhan-huai, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(5):42-44.

Abstract: The heat-resistant explosive 2, 2′, 4, 4′, 6, 6′-hexanitro-diphenyl sulfone (PCS) was synthesized by oxidation with CrO3 as oxidant in HNO3 medium of a intermediate, 2, 2′, 4, 4′, 6, 6′-hexanitro-diphenyl sulfide (DPS), which was prepared by condensation reaction using 2, 4, 6-trinitrochlorobenzene and sodium thiosulfate as starting materials. The total yield was over 85%. The DSC exothermic peak temperature of the product was 360.1 ℃, and its purity was 98.3%. In heat-resistant test under the condition of 200 ℃ and 48 h, the mass loss of PCS was only 0.62%. The vacuum stability test result under the condition of 120 ℃ and 48 h was 0.35ml/5g. The impact and friction sensitivity were 100% and 94%, respectively. The charge density of the mixed heat-resistant explosive JF1 that mainly based on PCS was prepared. The application test results show that JF1 can completely replace ordinary explosive to use in oil explosive materials.

45. Development of Hexanitrohexaazaisowurtaitane at abroad, Wang Xin, Peng Cui-zhi, [CNGC North Institute for Scientific and Technical Information, Beijing 100089, China], Chinese Journal of Explosives & Propellants. 2007, 30(5):45-48.

Abstract: The current situation about the synthesis method and industrialization production ability of CL-20 at abroad are overviewed, and the application of CL-20 in propellant and explosive formulations, including CL-20 based explosive formulations LX-19, PAX-12, PAX-11, PAX-29, DLEC038 and PBXW-16, is introduced with 21 references.

46. Synthesis of Polyurethane Thermoplastic Elastomer for Gun Propellants, Li Yu, Jian Xiao-xia, Zhou Wei-liang, Xu Fu-ming, [Department of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094], Chinese Journal of Explosives & Propellants. 2007, 30(4):58-61.

Abstract: A thermoplastic polyurethane elastomer is synthesized for the need of the binder in a novel gun propellant with polyethylene glycol (PEG) as soft segments, which has good miscibility with nitrate ester, 4′ 4-methylenetis (phenyl isocyanate) and ethylene glycol as hard segments. The principle of molecular designation of the elastomers is analyzed and discussed.DSC, FTIR and DMA are applied to characterize the elastomers. Results show that the elastomers have structure characteristic of polyurethane structure and good microphase segregation in accordance with the molecular designation. Soft segment′s Tg show that the elastomers have good low temperature mechanical properties.

47. Synthesis and Theoretical Analysis of 2-(3-nitrophenyl) Fullerenopyrrolidine, Peng Ru-fang, [China Academy of Engineering Physics, Mianyang Sichuan 621900, China], Jin Bo, [College of Material Science and Engineering, Southwest University of Science and Technology, Mianyang Sichuan 621010, China], Tan Bi-sheng, [College of Material Science and Engineering, Southwest University of Science and Technology, Mianyang Sichuan 621010, China], Chu Shi-jin, [College of Material Science and Engineering, Southwest University of Science and Technology, Mianyang Sichuan 621010, China], Chinese Journal of Explosives & Propellants. 2007, 30(3):22-25.

Abstract: A new fullerene derivative 2-(3-nitrophenyl) fullerenopyrrolidine (mNPF) containing energy-producing groups was prepared with glycine, m-nitrobenzaldehyde and fullerene as primary materials, and the reaction conditions were investigated by orthogonal test. The optimum reaction conditions with 82.1% yield(based on consumed C60) are: molar ratio of C60,m-nitrobenzaldehyde and glycine 1∶4∶6, reaction temperature 100℃,reaction time 24h,volume of toluene solvent 80mL.The structure of mNPF was characterized by UV-vis,FT-IR,1 HNMR,13 CNMR and MS. The feasibility of reaction was studied by semiempirical calculations PM3 method. The thermal stability of mNPF was studied by DTA, showing that mNPF has good thermal stability.

48. Synthesis of 2-(2-Nitrophenyl)fullerenopyrrolidine, PENG Ru-fang, [. Graduate School, CAEP, Mianyang Sichuan 621900, China], Jin Bo, [College of Material Science and Engineering, Southwest University of Science and Technology, Mianyang Sichuan 621010, China], Ma Dong-mei, [College of Material Science and Engineering, Southwest University of Science and Technology, Mianyang Sichuan 621010, China], Chu Shi-jin, [College of Material Science and Engineering, Southwest University of Science and Technology, Mianyang Sichuan 621010, China], Chinese Journal of Explosives & Propellants. 2007, 30(2):29-32.

Abstract: A new nitrofulleropyrrolidine derivative 2-(2-nitrophenyl) fullerenopyrrolidine (NPF) was synthesized with fullerene, glycine and o-1-nitrobenzaldehyde as primary materials by 1, 3-dipolar cycloaddition reaction. Its structure was characterized by UV-Vis, FT-IR, 1H NMR, 13C NMR and MS. Effects of the ratios of raw materials, temperature, reaction time and the volume of toluene on the reaction were investigated by orthogonal method. The results show that the reaction conditions of synthesizing NPF with the yield of 81.2% (based on consumed C60) are: molar ratio of C60, o-nitrobenzaldehyde and glycine 1∶4∶6, reaction temperature 80℃, reaction time 48h, volume of toluene solvent 70 mL.

49. Synthesis and Application of Geminal Dinitro Energetic Plasticizers, Chen Bin, Zhang Zhi-zhong, Ji Yue-ping, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(2):67-70, 74.

Abstract: According to the structure and synthesis character of the geminal dinitro energetic plasticizers, the current situation about the synthesis, the property and application of geminal di-nitro aldehyde acetals, esters and ether energetic plasticizers is summarized with 21 references. The preparation technique of aldehyde acetals energetic plasticizers BDNPF and BDNPA is introduced. Their physico-chemical properties, energy characteristics, thermal performance and application in the formulations of explosives and propellants are reviewed, considering that synthesis and application of geminal dinitro energetic plasticizers are the key point in energetic plasticizer study.

50. The Green Synthesis of 1, 2-Propylene Glycol Dinitrate, Shi Fei, Wang Qing-fa, Zhang Xiang-wen, Wang Li, Mi Zhen-tao, [Key Laboratory for Green Chemical Technology of State Education Ministry, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China], Chinese Journal of Explosives & Propellants. 2007, 30(2):75-77.

Abstract: In order to solve the environmental pollution of synthesizing 1, 2-propylene glycol di-nitrate (PGDN) with propylene oxide (PO) as raw material and the mixture of nitric acid and sulfuric acid as nitrating agent, a new method for preparation of PGDN by nitrating PO with di-nitrogen pent-oxide (N2O5) as a clean nitrating agent was presented. This reaction is environmental friendly with high atomic economy. Effects of the drip order, molar ratio of N2O5 to PO, reaction temperature and solvents on the yield and selectivity of PGDN were studied. The results show that the optimum reaction conditions are: dropping the PO into the solution of N2O5/organic solvent, the molar ratio of N2O5 to PO above 1.1∶1.0, the reaction temperature 15℃ and dichloromethane as solvent. Under the above optimum conditions, the yield of PGDN is about 96.3%, and the selectivity is nearly 100%.

51. Synthesis and Properties of 3, 4-Bis(4′-aminofurazano-3′)furoxan, Zhou Yan-shui, Li Jian-kang, Huang Xin-Ping, Zhou Cheng, Zheng Wei, Zhang Zhi-zhong, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2007, 30(1):54-56.

Abstract: 3, 4-bis(4′-aminofurazano-3′) furoxan was synthesized using dicyanopropane as starting material by , diazotization and condensation steps in turn, with overall yield 50%.Some physical and detonation properties were also measured, with density 1.795g/cm3, melt point 170 - 171℃, detonation velocity 7177m/s (1.530g/cm3), temperature of decomposition 260℃, friction sensitivity 8% (90°), impact sensitivity 60% (10kg, 25cm), and vacuum stability test 0.4 - 0.7mL (5g, 100℃, 48h). The thermal stability and compatibility of DATF were investigated by DSC. The results show that DATF has better thermal stability, lower sensitivity and good compatibility with energetic materials of RDX, HMX, NC and NC/NG system.

52. A Review on 3-Nitro-1, 2, 4-Triazol-5-One and its Salts, Ma Hai-xia, [School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Song Ji-rong, [College of Chemical Engineering/Shaanxi Key Laboratory of Physico-Inorganic Chemistry, Northwest University, Xi'an 710069, China], Hu Rong-zu, [College of Chemical Engineering/Shaanxi Key Laboratory of Physico-Inorganic Chemistry, Northwest University, Xi'an 710069, China], Chinese Journal of Explosives & Propellants. 2006, 29(6):9-15.

Abstract: The synthesis and properties of a new energetic material 3-nitro-1, 2, 4-triazol-5-one (NTO),including synthesis methods, crystal structure, quantum chemistry, thermal behaviors and toxicity were reviewed in details. The molecule structure and thermodynamic properties of twenty-one kinds of NTO complexes of alkali, alkaline earth, transition metals and rare earth metals were introduced emphatically and the thermal decomposition products of NTO alkali complexes were concluded as carbonate with Li, Na and K, and those of Rb and Cs complexes of NTO were carbonate, metal oxide and polymers. The relationship between the enthalpy of activation (ΔH~≠) and the value (T_(pdo)) of the peak temperature among NTO alkali metal complexes was obtained with 73 references.

53. Amination of Nitrotoluenes via Vicarious Nucleophilic Substitution(VNS) of Hydrogen, Li Jia-rong, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Zhao Jian-min, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Wei Xiao-jie, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Zhao Xiao-fan, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Dong Hai-shan, [Institute of Chemical Engineering and Material, CAEP, Mianyang Sichuan 621900, China], Chinese Journal of Explosives & Propellants. 2006, 29(6):30-32.

Abstract: The VNS amination reaction of nitrotoluene with ATA in DMSO in the presence of MeONa via vicarious nucleophilic substitution (VNS) of hydrogen was studied. The results indicated that 3-amino-2, 4-dinitrotoluene was obtained by VNS amination of DNT in the yield of 10.5%, and 3, 5-diamino-2, 4, 6-trinitrotoluene was obtained via VNS amination of 2, 4, 6-trinitrotoluene in the yield of 27.6%. The yields were lower under microwave radiation than that at room temperature. The amination of TNT in hydroxylamine gave DATNT in poor yield. The products were characterized by IR, nuclear magnetic resonance, elemental analyses and MS.

54. Preparation and Performance of Double Base Propellant Modified by NGEC, Wang Fei-jun, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Yang Fei-fei, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Wang Jiang-ning, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Shao Zi-qiang, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China]. Chinese Journal of Explosives & Propellants. 2006, 29(6):51-53.

Abstract: In order to enhance the mechanical performance of double-base propellant at low temperature, the cellulose was converted to cellulose glycidyl via basification and etherization reactions. A novel energetic binder named nitric acid ester of cellulose glycidyl ether (NGEC) with different esterification and etherification degree was synthesized by nitrating cellulose glycidyl. The mechanical performance and the section appearance of the two double base propellants based on NGEC and NC were surveyed and analyzed. The detonation heat and specific volume of the two propellants were tested and contrasted. The results show that the double-base propellant based on NGEC has better mechanical performance, detonation heat and specific volume level over aging those of double base propellant based on NC and its inner-structure turns more uniform. Its compressive strength σm (+50℃), elongation εm(25℃) and specific impulse are no less than 11.0MPa and 40% and 2218N•s•kg•-1, respectively.

55. HZSM-5 Assisted Clean Nitration of Toluene with Dinitrogen Pentoxide, Qian Hua, Ye Zhi-wen, Lü Chun-xu, [School of Chemical and Engineering, Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2006, 29(5):9-13.

Abstract: In order to solve the problem of synthesizing p-mononitrotoluene involving the concentrated mineral acids as the catalysts produces huge amounts of wastes along with a large amount of undesired o-MNT due to the nonselective nitration of toluene, the nitration of toluene by N2O5 has been investigated with solid acids catalysts HZSM-5. By the use of new nitrating agent, the reaction eliminated the use of concentrated sulfuric acid and was environmental friendly with high atom economy. The excellent selectivity of HZSM-5 makes the ratio of p-mononitrotoluene increase greatly. Effects of reaction temperature, reaction time, amount of catalyst and the ratio of Si/Al on the nitration were investigated, showing that under optimum conditions, the yield of nitration of toluene was 42%, and para-selectivity was 78.9%.

56. Research on Coating HNIW with Water-borne Branched Polyurethane, Liao Su-ran, [Textile and Chemical Engineering Department, Henan Textile College, Zhengzhou 450007, China], Luo Yun-jun, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Yang Yin, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Sun Jie, [Institute of Chemical Materials, CAEP, Mianyang Sichuan 621900, China], Tan Hui-min, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2006, 29(5):22-24, 28.

Abstract: The waterborne branched polyurethane (WBPU) was synthesized from toluene diisocyanates (TDI), TDB-2000, TMN-450, dimethylolpropionic acid (DMPA) and 1, 4-butanediol (BDO) as raw materials under acetone reflux. The cast films obtained were characterized by FT-IR, 1H NMR and DSC. The DSC curve presented an endothermic decomposition bimodal profile, showing that water-borne branched polyurethane resin degraded obviously at about 299℃ and 380℃. The SEM photographs and FT-Raman spectra revealed that hexanitr-ohexaazaisowurtzitane (HNIW) was coated with water-borne branched polyurethane by means of latex deposition. The impact sensitivity results show that the characteristic height H(50) of HNIW coated by water-borne branched polyurethane increases from 25.1cm to 31.6cm, indicating that the water-borne branched polyurethane can dec-rease the impact sensitivity of HNIW.

57. Synthesis and Properties of a Novel Azido Energetic Curing Agent, Zheng Xiao-dong, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Ma Xiao-dong, [Military Office, Xi'an North Huian Chemical Industrial Co. Ltd, Xi'an 710302, China], Qiu Shao-jun, [School of Materials Scienceand Engineering, Northwestern Polytechnical University, Xi'an 710072, China], Li Hong-li, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Jiang Jun, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Gan Xiao-xian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2006, 29(5):63-66.

Abstract: To improve the mechanical properties of the binder system, a novel azido poly-isocyanate energetic curing agent (EC) was synthesized via additional reaction of azido polyether polyol and hexamethylene diisocyanate (HDI). The material ratio, reaction temperature and post processing steps on the reaction were studied. The DSC results show that for EC, there was an exothermic peak at 252.89℃ and the glass transition temperature (Tg) was found at -47.13℃; for the EC/GAP system, thermal decomposition peak was at 254.56℃ and the glass transition temperature (Tg) was found at -45.78℃. And the EC/GAP/50% TEGDN system has good physical and chemical compatibility, there were two peaks at 213.05℃ and 250.89℃, and the glass transition temperature (Tg) was found at-69.08℃. The tensile strength and break elongation value of GAP/EC system is 0.67MPa and 129%, respectively, which is better than that of 0.5MPa and 56.5% of GAP/N100 system at 20℃.

58. Synthesis and Properties of 3-Azidomethyl-3-Ethyloxetane and its Homopolymer, Han Tao, Gan Xiao-xian, Xing Ying, Li Na, Lu Xian-ming, Zhang Zhi-gang, Mo Hong-chang, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2006, 29(5):72-75.

Abstract: To develop new energetic binder, a new azide oxetane monomer, 3-azidomethyl-3-ethyloxetane (AMEO) was synthesized by 1, 1, 1-tri(hydroxylmethyl) propane, diethylcarbonate, 4-toluenesulfonyl chloride and sodium azide as raw materials. Its structure and properties were identified by 1H NMR, FTIR, elemental analyses and DSC. At the present of catalyst boron-trifluoride etherate, a solid energetic polymer, homopolymer of 3-azidomethyl-3-ethyloxetane PAMEO was prepared by the cationic polymerization of monomer AMEO with (1, 4)-butanediol as initiator and dichlorometane as solvent. The structure of the polymer was identified by IR, (1H NMR) and elemental analyses. The properties of the polymer were characterized by TGA, DSC, and hydroxyl equivalent and number-average molecular weight.

59. Synthesis and Characterization of Ultrafine Cupric 2, 4-Dihydroxy- benzoate(β-Cu), Li Yu, Guo Yu, Liu You-zhi, Shi Guo-liang, XIE Wu-xi, [Research Center of Shanxi Province for High Gravity Chemical Engineering and Technology, Taiyuan 030051, China], Chinese Journal of Explosives & Propellants. 2006, 29(3):32-35.

Abstract: Using impinging steam-rotating packed bed (IS-RPB), ultrafine β-Cu powder was synthesized from CuSO4•5H2O and β-H as primary substances by high gravity reactive precipitation method. The TEM, laser size analysis (LSA), BET and TG-DTG techniques were used to characterize the product. Effects of the operation conditions of rotational speed, impact velocity and post-treatment conditions on the average particle size of β-Cu were also studied systematically. The results show that the operation conditions are optimized as: rotational speed, 1000r/min, impact velocity, 28m/s and vacuum desiccation temperature, 100℃. Under the above-mentioned conditions the sheet β-Cu particles with size of 0.12μm to 0.363μm, an average particle size of 610nm and a specific surface area of 11.6265m2/g are obtained.

60. Researches and Applications of Borate Surfactants, Wang Hai-ying, Li Bin-dong, Lü Chun-xu, Zou Qi, [School of Chemical Engineering, Nanjing University of Science & Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2006, 29(3):36-38, 42.

Abstract: The structures of the borate surfactant and its improved methods of properties are briefly introduced. The progress in synthesis of borate surfactant and their applications in the fields of antistatic, anti-wear, and flame retardancy were introduced. The antistatic researches of polymeric borate surfactant are described, and their application prospect in the industrial area such as the energetic material area is reviewed with 27 references.

61. Synthesis of CL-20 by Clean Nitration, Qian hua, Lü Chun-xu, Ye Zhi-wen, [Chemical Engineering School, Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2006, 29(3):52-53, 64.

Abstract: CL-20 is a high energy material. Usually It Is prepared via nitration with nitric and sulfuric acid Concentrated, this technique aims pollutes the environment. In this section, CL-20 was synthesized with 2, 6, 8, 12-tetraacetylhexaazatetracyclo [5, 5, 0, 0 3,11,0 5.9] dodecane (TAIW) and dinitrogen pentoxide clean nitrating agent. By the use of new nitrating agent the reaction eliminated the use of concentrated sulfuric acid and environmental friendly with high was atom economy. The structure of the compound was characterized by elemental analysis, IR, 1H NMR and MS. Meanwhile, The effects of reaction temperature and reaction time on the yield were also investigated, showing that under the conditions of reaction temperature, 0℃ and reaction time, 1h, the optimum yield of CL-20 was up to 62%.

62. Synthesis Mechanism of Tetranitrodiazidopropionylhexaazaisowurtzitane, Meng Zheng, Ou Yu-xiang, Liu Jin-quan, Wang Yan-fei, [College of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2006, 29(3): 63-67.

Abstract: TAIW was formed from hydrogenolysis debenzylation of TADBIW using Pt as catalyst. TADCPIW was synthesized by α-chloropropionylation of TAIW. A mixture contained TNDCPIW was obtained by nitration of TADCPIW, and then azido groups were introduced into product. Tetranitrodiazidopropionylhexaazaisowurtzitane (TNDAPIW) with high nitrogen content and high enthalpy of formation can be obtained by the product separation using column chromatography. The structures of TNDAPIW and the intermediate compounds were identified by IR, 1H NMR and elemental analysis. The related conditions and mechanisms of reactions such as hydrogenolysis, α-chloropropionylation, nitration and azidation were discussed. The results show that because of the caged structure of TAIW and the electrophilic effect in the-acyl radical, it is necessary for the actively reacting composite such as α-chloropropionyl chloride used in the chloropropionylation reaction; the nitration reagent should be appropriately used in the nitration, if not TADCPIW will be nitrated into HNIW; as the diazo-reaction is S_N2 reaction, it is advantageous for the reaction to choose the dipolar protophilic solvent like DMF or DMSO.

63. Synthesis of Trinitropyridine and Its N-Oxide, Zhao Jian-min, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Li Jia-rong, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Wei Xiao-jie, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Li Wen-ting, [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China], Dong Hai-shan, [Institute of Chemical Engineering and Material, China Academy of Engineering Physics, Mianyang 621900, China], Chinese Journal of Explosives & Propellants. 2006, 29(3):73-76.

Abstract: 2, 2-Dinitropropane-1, 3-diol was synthesized from nitromethane in low temperature by oxidative nitration method. Silver was successfully recycled with a yield upon 93% and reused in the synthesis of 2, 2-dinitropropane-1, 3-diol. Potassium 2, 2-dinitroethanol, the key intermediate compound for synthesis of trinitropyridine (TNPy), was prepared through one-pot method with a yield upon 62%, which is 10% higher than conventional method. Controlling the pH value in the range of 1 - 2, trinitropyridine N-oxide (TNPyO) was synthesized by the cyclization of potassium 2, 2-dinitroethanol in 68% nitric acid at 50 - 60℃.Maintaining the temperature between 80-90 ℃, TNPyO can be further reduced to produce TNPy by refluxing for 1 h; the yields of TNPyO and TNPy are 50% and 15%, respectively. TNPyO can also be prepared from potassium 2, 2dinitroethanol under phosphoric acid and sulfuric acid. The products were characterized by IR, nuclear magnetic resonance, elemental analysis and EI-MS.

64. Synthesis of Rich-Nitrogen Compound of 3, 3′-Azobis(6-Amino-1, 2, 4, 5-Tetrazine), Wang Bo-zhou, Lian Peng, Liu Qian, Wang Xi-jie, Zhang Zhi-zhong, Huang Xin-ping, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2006, 29(2):15-18.

Abstract: 3, 3′-azobis (6-amino-1, 2, 4, 5-tetrazine) (DAAT) was synthesized with triaminoguanidine nitrate and 2, 4-pentanedione as primary substances by condensation, oxidation, hydrazinolysis, oxidation-bromation, aminolysis and hydrolysis in turn. DAAT is a new rich-nitrogen energy material with remarkable thermal stability and insensitivity against friction and impact. DAAT decomposes at relatively high temperatures (250℃) measured by DSC. The details of each reaction process and yields were described; the results are according with the references. The overall yield of DAAT is 19%. Its structure was confirmed by IR, HNM and DSC. The mechanisms of the condensation and oxidation-bromation reactions were presented.

65. Study on the Synthesis of TEX, Xu Rong, Zhou Xiao-qing, Zeng Gui-yu, Liu Chun, [The Institute of Chemical Materials, CAEP, Mianyang Sichuan 621900, China], Chinese Journal of Explosives & Propellants. 2006, 29(2):26-28
.
Abstract: 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 temperature. The purity and overall yield of TEX are 99.5% and 34.8%, respectively. The effect of THDFP dry time, the temperature of adding material and reaction temperature on the synthesis of TEX were studied. Results show that THDFP of full dried for synthesis is favored, should control the temperature of adding material in the range 45～50℃ and the reaction temperature in the range of 75～80℃.

66. Experimental Studies on the 2, 4, 6-Trinitro-m-Xylene Crystal, Guo Jin-Yu, Zhang Tong-Lai, Zhang Jian-Guo, LIU Yan-Hong, [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2006, 29(2):58-62, 65.

Abstract: The crystal of 2, 4, 6-trinitro-m-xylene (TNMX) has been synthesized, cultured and characterized by X-ray single crystal diffraction, 1H NMR, MS and FT-IR techniques. TNMX is crystallized into orthorhombic, PbCn space group, a=(5.749(2))×10-10m, b=15.043(3)×10-10m, c=11.415(2)×10-10m, α=β=γ=90.00°, V=987.2(3)×10-30m3, Z=4, Dc=1.623g/cm3 (calculated density), final R indices[I2σ(I)], R1=0.0359, wR2=0.1006, R indices for all data, R1=0.0459, wR2=0.1045. By means of weak interactions among the nitro O atoms from different TNMX molecules, two-dimensional frameworks come into being in this complex. The DSC and TG-DTG thermal analyses have also carried to predict its thermal decomposition mechanism. Based on thermal analyses, the crystal was predicted to decompose completely in one step.

67. Optimization of the Synthetical Craft of 2, 6-Diamino-3, 5-Dinitropyrazine-1-Oxide, Guo Feng-bo, Liu Yu-cun, Liu Deng Cheng, Yu Yan-wu, [Department of Environmental and Safety Engineering, North University of China, Taiyuan 030051, China], Chinese Journal of Explosives & Propellants. 2006, 29(1):17-19, 22.

Abstract: LLM-105 was synthesized with 2, 6-dichloropyrazine as primary substance by substitution, nitration, and ammoniating and oxidation steps in turn and the overall yield of LLM-105 is greater than 36%. The purity of LLM-105 is more than 98%. Its structure was characterized by elemental analysis, IR, MS and NMR. Effects of the consumption of CH3ONa, the volume proportion of HNO3 and H2SO4, the consumption of NH3•H2O and the volume proportion of trifluoroacetic acid and H2O2 on the overall yield of LLM-105 were investigated. The optimal conditions of synthesizing LLM105 were ascertained as: for the substitution reaction, under the conditions of reflux, reaction time, 2h; the consumption of CH3ONa is 120% for the nitration reaction, reaction time 4h; reaction temperature 60～70℃,the volume proportion of HNO3 and H2SO4, .83; or the ammoniating reaction, under the conditions of 2h and 60℃, the consumption of NH3•H2O, 200%; for the oxidation reaction, under the conditions of 24h and room temperature, the volume proportion of trifluoroacetic acid and H2O2,∶10.

68. Progress in the Synthesis of TATB Free from Chloride, Zhou Xin-li, [School of Chemical Engineering, Nanjing University of Science & Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2006, 29(1):26-28.

Abstract: Based on references, synthesis methods of insensitive explosive TATB are summarized. Modified synthesis methods of TATB containing chloride compounds are simply introduced. The progresses in the synthesis of TATB free from chloride by different raw materials and synthesis process are mainly introduced, especially using direct amine hydrogen synthesis principle and process of TATB according to vicarious nucleophilic substitution of hydrogen (VNS) are emphasized, including influences of raw materials, mole specific, amine agent and its addition methods, methods of quenching reaction on yield, particle size, purity and physical appearance. It is shown that VNS is a new method for preparation of energetic materials containing multi nitro and amino aromatic compounds.

69. Synthesis and Properties of N-guanylurea Dinitramide, Liu Qian, Wang Bo-zhou, Zhang Zhi-zhong, Zhu Chun-hua, Lian Peng, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China]

Abstract: N-guanylurea dinitramide (GUDN) was synthesized with N-guanylurea hydrochloride as primary substance by hydrolysis and double decomposition reaction in turn and the overall yield of GUDN is 79%. The structure of GUDN was identified by elemental analysis, IR and UV. Some properties of GUDN were determined as: density, 1.755g/cm3, friction sensitivity, (2.45MPa, 20mg, 66°); H50 197cm (2kg) etc. And its properties were compared with properties of ADN. GUDN has low sensitivity, good thermal stability and unhygroscopicity. The results obtained by DSC show that GUDN is compatible with common energetic materials such as HMX and RDX. Application tests indicate that GUDN can be used in double base propellant.

70. A Review of Recent Advances of Energetic Plasticizers, Ji Yue-Ping, Li Pu-rui, Wang Wei, Lan Ying, Ding Feng, [Xi'an Modern Chemistry Research Insititute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2006, 29(1):29-31.

Abstract: The current situation about the synthesis and application of energetic plasticisers based on the kinds of energetic group is summarized. The primary role of energetic plasticisers in energetic material formulation is considered to modify the mechanical properties of charge to improve safety characteristics. The nitrate ester plasticizers’ is a sensitive explosive easily initiated by fricition and impact. The value of HD for most of the energetic nitrate esters is 1.1.The novel energetic compounds or oligomeric containing azido geminal dinitro and nitramine group with excellent properties are considered as primary research subject of energetic plasticisers. The shortcoming in the synthesis technology, variety and application of energetic plasticizer in domestics is analysed. The suggestions in the synthesis and application of novel energetic plasticizers are presented.

71. Synthesis of Polyurethane Elastomer Used in the Coating of Some Propellant and Its Application, Zhu Kai-jin, Xiao Zhong-liang, [Department of Chemical Engineering, North University of China, Taiyuan 030051, China], Chinese Journal of Explosives & Propellants. 2005, 28(4):55-57.

Abstract: By utilizing toluene diisocyanate (TDI) and liquefied diphenylmethane diisocyanate (MDI) to synthesize polyisocyanate, and then to synthesize the adhesive of polyurethane as main component of certain propellant coating, a coating with good mechanical property and low smoke fog property is obtained. The results show that it is fit to choose the ratio 7∶3 of TDI to MDI, the reaction temperature 80℃, the reaction time (30min) and the solidified time 4～5d. The originality of the study rests on that TDI and liquefied MDI are simultaneously used as the synthetic material of polyisocyanate to make the coating of some propellant.

72. Progress of the High Density Hydrocarbon Fuel of Exo-tetrahydrodicyclopentadiene, Du Yong-mei, Li Chun-ying, Lü Jian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2005, 28(4):58-60.

Abstract: The current situation of synthetic methods of exo-tetrahydrodicyclopentadiene including hydrogenation of dicyclopentadiene and isomerization from endo-tetrahydrodicyclopentadiene to exo-tetrahydrodicyclopentadiene is summarized. Different hydrogenation catalysts and process are generalized and several hydrogenation catalysts are compared. Continuous and intermittent process is recapitulated. Isomerization catalysts and mechanism of isomerization with Lewis acid catalysts are introduced. Development direction of hydrogenation catalysts and isomerization catalysts is presented. New synthetic methods of exo-tetrahydrodicyclopentadiene are suggested.

73. Nitration of Halobenzens with Fluorous Biphasic System, Yi Wen-bin, Cai Chun, [Chemical Engineering College, Nanjing University of Science & Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2005, 28(3):45-48.

Abstract: Halobenzens can be nitrated effectively in fluorous phase in the presence of ytterbium (Ⅲ) perfluorooctanesulfonate (Yb(OSO2C8F17)3) catalyst. Perfluorodecalin (C10F18) was used as a fluorous solvent for this reaction. The fluorous phase after separating catalyst can be reused many times, and P/O ratio of p-isomer to o-isomer in the products of mononitration of flurobenzene, chlorobenzene and iodobenzene can be increased to 7.20, 2.45, 4.01 and 0.91 respectively. Partition coefficients involving organic and fluorous phase under different temperatures have been measured. Effects of reaction temperature, the ratio of fluorous phase/organic phase and the water content in the reaction system on the nitration were investigated. It was observed that the optimum temperature for fluorous biphasic nitrations of flurobenzene, chlorobenzene, bromobenzene and iodobenzene were 60℃, 60℃, 80℃ and 80℃ respectively. Reducing the ratio of fluorous phase/organic phase and the water content in the reaction system can increase P/O ratio.

74. Synthesis of Ammonium Dinitramide from Ethyl Carbamate, Wang Bo-zhou, Liu Qian, Zhang Zhi-zhong, Lian Peng, Zhu Chun-hua, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2005, 28(3):49-51.

Abstract: In HNO3-H2SO4, ammonium N-nitro carbamate ethyl ester was synthesized from ethyl carbamate, then taking N2O5 as nitrating agent; ammonium dinitramide (ADN) was prepared. its yield reached to 70%. It was re-crystallized to yield a white hygroscopic powder with a melting point of 90～92℃. Its structure was identified by elemental analysis, infrared spectrum and ultraviolet spectroscopy. The main factors such as reaction medium, stuff ratio, reaction temperature were also briefly discussed; its optimum condition was obtained.

75. Synthesis and Characterization of High-Nitrogen Energetic Compounds Derived from Azotetrazolate, Xu Song-Lin, Yang Shi-qing, Yue Shou-ti, [College of Aerospace and Material Engineering, National University of Defense Technology, Changsha 410073, China], Chinese Journal of Explosives & Propellants. 2005, 28(3):52-54.

Abstract: Three new high-nitrogen energetic compounds bis-(ammonium)-5, 5′-Azotetrazolate, bis-(guan-idinium)-5, 5′-Azotetrazolate and bis-(triaminoguani-dinium)-5, 5′-Azotetrazolate have been synthesized from 5-aminotetrazole as a starting materials. Their structures were identified by IR, NMR, DSC, melting point test and elemental analysis. Their explosive performances were also introduced. It shows that these azotetrazolate compounds are possessed of positive enthalpy of formation, high gas generating ability with little or no smoke or residue produced nonhygroscopic and excellent explosive performances. They are the important ingredients of gas generating, low signature propellants, pyrotechnics and high performance explosives.

76. Synthesis and Characterization of Diacetyltetrabenzylhexaazaisowurtzitane, Chen Fei, [School of Material Science & Technology, Beijing Institute of Technology, Beijing 100081, China], Pang Si-ping, [School of Life Science & Technology, Beijing Institute of Technology, Beijing 100081, China], Yu Yong-zhong, [School of Material Science & Technology, Beijing Institute of Technology, Beijing 100081, China], Zhao Xin-qi, [School of Material Science & Technology, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2005, 28(3):55-56, 69.

Abstract: The oxidation of hexabenzylhexaazaisowurtzitane (HBIW) by cerium (Ⅳ) ammonium nitrate has been studied. Diacetyltetrabenzylhexaazaisowurtzitane (DATBIW) was obtained and its structure was characterized by FT-IR, MS and 1H NMR. The mechanism of the oxidation-debenzylation process of HBIW was deduced.

77. Synthesis of 3-Azidomethyl-3-Methyloxetane, Li Na, Gan Xiao-xian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2005, 28(3):57-59

Abstract: 3-Hydroxymethyl-3-methyl oxetane (HMMO) was prepared by the cyclization of raw materials 1, 1, 1-tri-(hydroxylmethyl) ethane and diethyl carbonate. Under lower temperature, 3-methoxytosyl-3-methyl oxetane (MTMO) was synthesized by the reaction of HMMO with 4-toluenesulfonylchloride. 3-Azidomethyl-3-methyl oxetane was synthesized by the reaction of MTMO and sodium azide. The yields of the three steps were 76%, 96%, 85%, respectively .The structure and properties of AMMO were identified by 1H NMR, FTIR, elemental analysis and DSC .The results show that final product was target compound. AMMO was an important energetic oxetane monomer. It can conduct steady cationic polymerization.

78. Synthesis and Thermal Decomposition of 1, 4-Dinitromidazole, Cao Duan-lin, [Department of Chemical and Engineering, North University of China, Taiyuan 030051, China], Liu Hui-jun, [Department of Chemistry, Education University of Yanbei, Datong 037009, China], Li Yong-xiang, [Department of Chemical and Engineering, North University of China, Taiyuan 030051, China], Chinese Journal of Explosives & Propellants. 2005, 28(3):60-62.

Abstract: 1, 4-Dinitroimidazole (1, 4-DNI) is synthesized by following the reactions: 4-dinitroimidazole was N3-acetylated by acetic anhydride in acidic solution to obtain acylate and acylate thus obtained was nitrated by the mixture of concentrated sulfuric acid, acetic anhydride and sodium nitrate to obtain 1, 4-DNI. The synthetic condition is optimized by the orthogonal experiment. The optimum parameters are as follows: n (4-nitr-oimidazole) / n (sulfuric acid) / n (sodium nitrate) / n (acetic anhydride) = 2/3/8/15, reaction temperature 30～40℃ and reaction time 3h. Thermal decomposition of 1, 4-DNI is studied by DSC.

79. Homogeneous Synthesis of Azidodeoxycellulose, Shao Zi-qiang, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Wang Fei-jun, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Wang Wen-jun, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China], Liao Bing, [GuangZhou Institute of Chemistry. Academia Sinica, Guangzhou 510650, China], Chinese Journal of Explosives & Propellants. 2005, 28(2):47-49.

Abstract: A new high energetic bonder intermediate azidodeoxycellulose for solid propellant was synthesized from the raw material cotton linters under homogeneous conditions. The process of preparing azidodeoxycellulose includes two steps. The first is the tosylation of cellulose with tosylchloride using triethylamine as catalyst and the dimethylacetamide/LiCl system as solvent to obtain cellulose tosylate with certain ester number. The second is nucleophilic substitution reaction of the cellulose tosylate with NaN3 in DMSO to obtain azidodeoxycellulose with the degree of substitution (DS) of 0.6 ～1.0. The effects of cellulose tosylate/DMSO ratio, reaction temperature and reaction time on the value of DS of azidodeoxycellulose were discussed. The samples were characterized by elemental analysis, FT-IR and X-ray diffraction.

80. Nitrolysis with Nitrogen Peroxide for Synthesis of 1, 4, 5, 8-Tetranitro-1, 4, 5, 8- tetraazabicyclo[4. 4. 0]decalin, Cai Chun, Lü Chun-xu, [Chemical Engineering School, Nanjing University of Science & Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2005, 28(2):50-51.

Abstract: 1, 4, 5, 8-Tetranitro-1, 4, 5, 8-tetraazabicyclo [4.4.0] decalin (TNAD) is used as an explosive and has several superior physical properties, such as heat-resistance and insensitivity to impact. This compound could be prepared from the raw material 1, 4, 5, 8-tetraazabicyclo [4.4.0] decalin via nitrosation with sodium nitrite in hydrochloric acid, and followed nitrolysis with N2O5 in mixed acid. In nitrolysis step, the effect of reaction medium and the reaction temperature on the yield have been investigated. The structure of compound was characterized by IR and elemental analysis. The total yield could reach as high as 85%.

81. Synthesis and Properties of 1, 1-Diamino-2, 2-Dinitroethylene, Zhou Cheng, Zhou Yan-shui, Huang Xin-ping, Wang Xi-jie, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2005, 28(2):65-67.

Abstract: 1, 1-Diamino-2, 2-dinitroethylene (DADE) was synthesized with 2-methylimidazole as primary substance by nitration and hydrolysis steps in turn and the yield of DADE is 13.4%. Its structure was char-acterized by elemental analysis, IR, MS and NMR. The effects of concentration of sulfuric acid, reaction temperature, reaction time on the yield were investigated. Some important properties of DADE were determined as: density, 1.885g/cm3, detonation velocity, 8047m/s (ρ=1.696g/cm3); friction sensitivity, 10% (3.92MPa, 90°); impact sensitivity, 6% (10kg, 25cm); H50, 89.1cm (5kg); vacuum stability test, 0.14ml/5g (100℃, 48h), explosion temperature, 285℃ (5s delay).

82. Synthesis and Characterization of 1, 1, 1-Trimethylolpropane Trinitrate, Cui Jian-lan, [Department of Chemical Engineering, North University of China, Taiyuan030051, China], Guo Wen-long, [The College of Pharmaceuticals and Biotechnology of Tianjin University, Tianjin 300072, China], Cao Duan-lin, [The College of Pharmaceuticals and Biotechnology of Tianjin University, Tianjin 300072, China], Xu Chun-yan, [The College of Pharmaceuticals and Biotechnology of Tianjin University, Tianjin 300072, China], Chinese Journal of Explosives & Propellants. 2005, 28(2):78-79.

Abstract: 1, 1, 1-Trimethylolpropane trinitrate was synthesized from the raw material trimethylolpropane via nitration reaction. The effect of nitriting agent on the yield of nitration reaction was studied and the proper additive and nitriting agent was found. The experimental results showed under the following reaction conditions: 98% nitric acid as nitriting reagent, the molar ratio of trimethylolpropane to nitric acid, 10∶1; reaction time, 2h; reaction temperature,0～20℃,the yield of the title compound was up to 99.7%, providing a new highest yield method of synthesizing 1, 1, 1-Trimethylolproane trinitrate. The product was characterized by IR, nuclear magnetic resonance and elemental analysis.

83. Kinetics of Synthesis of TADF by Hydrogenolysis Debenzylation of TADB, Ma Ai-ling, Sun Cheng-hui, Fang Tao, Zhao Xin-qi, [Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2005, 28(2):43-45.

Abstract: The reaction kinetics of synthesis of tetraacetyldiformylhexaazaisowurtzitane (TADF) by hydrogenolysis debenzylation of tetraacetyldibenzylhexaazaisowurtzitane (TADB) has been studied over Pd(OH)2/C catalyst in formic acid. The experiment was investigated in an atmosphere of hydrogen. The effects of both internal and external diffusions were eliminated by stirring adequately. The effects of catalyst and solvent were eliminated by the experiments without adding substrate. The changes of the absorption amount of hydrogen with reaction time were measured. The absorption amount of hydrogen was used to stand for the reaction extent. Kinetics calculations of the experimental data at various temperatures were carried out, according to the integrate reaction rate equation. Experimental results indicate that the reaction is the first-order with respect to TADB under the experimental conditions. The apparent activation energy (Ea) of the reaction is 50.41 kJ/mol and preexponential factor (A) (4.5326×106 min-1). It showed that the reaction of hydrogenolysis debenzylation of tetraacetyldibenzylhexaa-zaisowurtzitane in formic acid can undergo easily.

84. A New Technique for Preparation of Pentaerythritol Diazido Dinitrate, Su Tian-duo , Zhang Li-jie , Liu Heng, Zhang Hong-yu, Cui Rong, [Xi'an Mordern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2005, 28(1):52-53, 60.

Abstract: A new technique of preparing pentaerythritol diazido dinitrate (PDADN) via bromization reaction of pentaerythritol as starting material, azidonation reaction of 2, 2-bromomethyl-1, 3-propandiol and nitration reaction of 2, 2-azido-1, 3-propandiol was presented. The structure of PDADN was characterized by IR, 1H NMR and elemental analysis.

85. An Improved Synthetic Method of DADE with High Yield, Wang Xi-jie, Zhou Cheng, Wang Bo-zhou, Zhang Zhi-zhong, Fu Xia-yun, [Xi'an Modern Chemistry Research Institute, Xi'an710065, China], Chinese Journal of Explosives & Propellants. 2005, 28(1):61-62, 66.

Abstract: An improved synthetic route for DADE was investigated by the nitration of 2-methyl-4, 6-pyrimidindione in nitric acid/sulphuric acid and hydrolysis of the intermediate 2-dinitromethylene-5, 5-dinitro-dihydro-pyrimidine-4,6-dione based on the perfect detonation properties of DADE and a comparison of its reported preparation methods. Its total yield is over 83%. The structure of DADE was characterized by IR, MS, NMR and elemental analysis.

86. Synthesis and Properties of 3-azidomethyl-3-cyanoethoxylmethyloxetane Polymer, Gan Xiao-xian, Xing Ying, Li Na, Zhang Zhi-Gang, Lu Xian-Ming, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2004, 27(4):10-13.

Abstract: With indirect method, a new liquid hydroxyl-terminated azider polyether binder, 3-azidomethyl-3-cyanoethoxylmethyloxetane homopolymer (PAMCMO) was synthesized by 3-bromomethyl-3-cyanoethoxylme- thyloxetane homopolymer (PBMCMO) and sodium azide in DMF. PAMCMO had the following properties: number average molecular weights 2,500; glass transition temperature -38.75 ℃, decomposition temperature of azido group 257.35 ℃. PAMCMO had good compatibility with nitrate ester plasticizers, because the introduction of cyanoethoxyl group could increase its solubility parameter to 23.45(J/cm3)0.5.

87. Synthesis and Characterization of C/N Heterocyclic Vinyl Ester Resin, Yang Shi-shan, Wang Ji-gui, Li Dong-lin, Gan Xiao-xian, [Xi'an Modern Chemistry Research Institute, Xi'an710065, China], Chinese Journal of Explosives & Propellants. 2004, 27(4):59-62.

Abstract: C/N heterocyclic vinyl ester resin (CNVER) was synthesized by the reaction of ISEP and methacrylic acid. The technological conditions of synthesizing CNVER were optimized. Influence of the molar ratio of epoxy group and carboxy group, the amount of catalyzer and the reaction temperature on the reaction was discussed. The structure of CNVER was confirmed by IR spectrum. Styrene was chosen as a cross-linking agent of CNVER. The properties of CNVER were studied. Its elongation is 7.2% and tensile strength 74.7 MPa, indicating that the mechanical properties of CNVER are good.

88. Preparation of Polyurethane-acrylate Core-shell Latex and its Coating of RDX, Lu Ming, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing100081, China], Sun Jie, [Institute of Chemical Materials, CAEP, Mianyang 621900, China], Chen Yu, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing100081, China], Luo Yun-jun, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing100081, China], Tan Hui-min, [School of Material Science and Engineering, Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2004, 27(3):17-20.

Abstract: Waterborne polyurethane (WPU) was prepared with TDI, DL-400 (Mn=340), DMPA and BDO as main materials, whose structure was characterized by FTIR. Polyurethane-acrylate (PUA) latex was synthesized through the method of the seed-latex polymerization with WPU, water and butyl acrylate as starting materials, two kinds of initiator, AIBN and (NH4)2S2O8-NaHSO3. Latex particles shape of PUA were determined through TEM, and the results indicated that PUA latex with core-shell structure was synthesized with AIBN as initiator, whose shell were black polyurethane particles and core white polyacrylate ones. PUA latex initiated by (NH4)2S2O8-NaHSO3 has no core-shell structure. The method was used for the first time to deposit core-shell latex to coat RDX with 10% KAl (SO4)2•12H2O solution, distilled water, 40℃. Through SEM, the surface of RDX was observed to have been covered with a layer of even film after being coated with PUA and the particles among RDX were perfectly dispersed.

89. Synthesis and Properties of 3, 3-diazidomethyloxetane and its Polymer, Lu Xian-ming, Gan Xiao-xian, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2004, 27(3):49-52.

Abstract: Using absolute alcohol as solvent, under the effect of NaOH, the 3, 3-dibromomethyl oxetane (BBMO) was synthesized by the cyclization of 1, 1, 1-tribromomethly-1-hydroxymethyl methane. 3, 3-Diazidomethyloxetane (BAMO) was obtained by the substitutation of BBMO with NaN3 using 1, 4-butylene-glycol as initiator and CH2Cl2 as solvent, a solid energetic binder (PBAMO) was synthesized by the cationic polymerization of the monomer BAMO. The structure of the polymer was identified by H NMR, FTIR, DSC and GPC. The physical chemistry properties of PBAMO are determined. The results show that PBAMO is an energetic binder with lower sensitivity; suitable melting point and lower melt viscosity and can be used as the composition of energetic thermoplastic elastomer.

90. Macro-kinetics Study of Ozone-mediated Nitration Reaction of Aromatic Compounds with Nitrogen Tetroxides, Lü Zao-sheng, [Wuhan University of Science and Technology, Hubei430081, China], Wang Xiao-yan, [Wuhan University of Science and Technology, Hubei 430081, China], Lü Chun-xu, [Nanjing University of Science & Technology, Nanjing210094, China], Chinese Journal of Explosives & Propellants. 2004, 27(3):66-69.

Abstract: The kinetics character in ozone-mediated nitration aromatic compound reaction with nitrogen tetroxide has been studied. Kinetics model has been constructed with the aid of stable state treatment method. Raman spectrum shows no nitronium ion in N2O4/O3, which demonstrates N2O4/O3 nitration aromatics, is not an affinitive electronic substitution process. Experiment results show that the reaction rate of N2O4/O3 nitration benzene and toluene is zero order in benzene and toluene, half order in N2O4, the reaction rate of N2O4/O3 nitration fluorobenzene is first order in fluorobenzene, zero order in N2O4. By competing reaction, Hamett's equation of N2O4-O3 nitrating substituted aromatics is obtained with logf~RH=-7.26σ + p-0.125. The reaction constant (ρ=-7.26) is approaching to the result of mixture acid nitrating substituted aromatics, which shows the transition state that decides isomer distribution during two kinds of nitrating reaction has similar structure.

91. Hydrogenolysis Debenzylation of TADBIW in Propionic Acid and n-Butyric Acid, Liu Jin-quan, Ou Yu-xiang, Han Wei-rong, Chen Bo-ren, [School of Science of Materials and Engineering, Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2004, 27(2):10-12.

Abstract: Tetraacetyldibenzylhexaazaisowurtzitane (TADBIW) is a product of hydrogenolysis debenzylation of hexabenzylhexaazaisowurtzitane (HBIW). Various products can be formed from hydrogenolysis debenzylation of TADBIW in different media using Pd catalyst prepared at the lab. Tetraacetylhexaazaisowurtzitane (TAIW) is obtained by hydrogenolysis of TADBIW in propionic acid and n-butyric acid. The related reaction mechanism is also discussed.

92. Development of High Strained Caged Hydrocarbons Used as High Density Fuels, Xing En-hui, Mi Zhen-tao, Zhang Xiang-wen, [Technology, Tianjin University, Tianjin300072, China], Chinese Journal of Explosives & Propellants. 2004, 27(2):13-16.

Abstract: This paper introduces the recent development of a new class of high energy hydrocarbon fuels. These caged hydrocarbons with high energy and high density have been synthesized to be used as high energy fuels or fuel additives, with the expectation that their inclusion in the fuel mixture will result in a net increase in volumetric combustion value of the current generation of power-plants. These caged hydrocarbons exhibit high density and contain a moderate amount of strain energy, which contributes to the energy output during combustion. Research and development direction of caged hydrocarbon fuels are presented.

93. The Synthesis of Hexanitrohexaazaisowutzitane by Oxidation, Pang Si-ping, [School of Life Science & Technology Beijing Institute of Technology Beijing 100081, China], Yu Yong-zhong, [School of Material Science & Technology, Beijing Institute of Technology, Beijing100081, China], Zhao Xin-qi, [School of Material Science & Technology, Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2004, 27(1):9-11.

Abstract: The way of synthesizing hexanitrohexaazaisowutzitane (HNIW) by oxidation was studied. HNIW was prepared by hydrolysis and nitration of the oxidation products of hexabenzylhexaazaisowurtzitane in 70% HNO3/AN, system with the yield being 21%. The reaction mechanism of the nitration of N-benzoyl group on hexaazaisowutzitane as the parent ring of HNIW was discussed.

94. Synthesis of Keto-RDX Using Dinitrogen Pentoxide as the Nitrating Agent, Cao Duan-lin, Cao Ming-bao, Li Yong-xiang, [Dept. of Chemical Engineering, North China University of Technology, Taiyuan030051, China], Chinese Journal of Explosives & Propellants. 2004, 27(1):12-15.

Abstract: The synthesis of Keto-RDX with Urotropine, Urea as raw materials, the mixture of nitric acide and dinitrogen pentoxide as nitrating agent was studied. The best process conditions were concluded. Under the conditions the yield of Keto-RDX can be more than 120%. By contrast, with the mixture of nitric acide and dinitrogen pentoxide as nitrating agent, mild reaction condition, higher yield and less contamination are the major advantages.

95. Synthesis and Characterization of Nitrocellulose Azidonitrate Glycidyl Ether, Shao Zi-qiang, Wang Wen-jun, Wang Fei-jun, Chen Fan-geng, Tan Hui-ming, [School of Materials Science and Engineering, Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2004, 27(1):36-39.

Abstract: A kind of new high energetic bonder—nitrocellulose azidonitrate glycidyl ether (NCAGE) for solid propellant was synthesized based on cotton cellulose pretreated by steam explosion. The process of preparing NCAGE included the following steps: (a) alkalization of the treated cellulose; (b) etherification of the alkali cellulose; (c) nitration of the water-soluble cellulose ether; and (d) azidation of nitrocellulose glycidol ether. The nitrogen content, structure and properties of NCAGE were measured and characterized by elementary analysis, DSC, FTIR and X-ray Diffraction. The results indicate that the nitrogen content of NCAGE can arrive at 15%～21% duo to the presence of - ONO2 and -N3, and the product can absolutely dissolve in solvents such as acetone, decompose at the temperature of 204℃ and has lower degree of crystalline compared to original cellulose.

96. Nitrosolysis-debenzylation to Tetraacetyldibenzylhexaazaisowurtzitane, Lu Lian-ying, Ou Yu-xiang, Wang Jian-long, [Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(4):41-43.

Abstract: Two benzyls were removed at wild conditions (at room temperature or at 30℃) from tetraacetyldibenzylhexaazaisowurtzitane (TADBIW) molecule through three methods by using inorganic materials as the nitrosolysis reagent to convert tetraacetyldinitrosohexaazaisowurtzitane (TADNSIW), the precursor for synthesis of hexanitrohexaazaisowurtzitane (HNIW). The structure of TADNSIW was determined by FT-IR, MS, (~1H) NMR and element analysis. The mechanism of debenzylation to TADBIW was put forward. The enaminecation is the intermediate of the nitrosolysis-debenzylation to TADBIW, which was approved by benzaldehyde being the by-product of the reaction.

97. The Synthesis of Large Particle Size TATB, Huang Ming, Luo Shun-huo, Tian Ye, [Institute of Chemical Materials, CAEP, Mianyang 621900, China], Chinese Journal of Explosives & Propellants. 2003, 26(4):44-46.

Abstract: The influence factors on synthesis of TATB were described. The parameters affecting particle size of TATB, such as reaction temperature, ammonia flow rate, TCTNB concentration, stirring rate were optimized. The large particle size TATB was produced by the replicate experiment according to the optimized parameters and its average diameter of the particle exceeded 70 μm.

98. Study on HTPB Based PU/PIMA Interpenetrating Polymer Networks, Gao Tong zhai, Tan Hui min, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):9-11.

Abstract: A new kind of interpenetrating polymer network (IPN) was synthesized by introducing IMA monomer into polyurethane (PU) based on hydroxy terminated polybutadiene in this paper. FTIR results demonstrated that the two monomers reacted completely. Tensile test indicated that the mechanical properties of IPNs were evidently enhanced with the introduction of PIMA. The microstructure of IPN was also investigated by TEM. The results revealed that the two phases interpenetrated proportionally and possessed preferable compatibility.

99. Synthesis and Properties of 3-Azidomethyl-3-nitratomethyloxetane and Its Polymer, Gan Xiao xian, Qiu Shao jun, Lu Xian ming, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):12-15.

Abstract: 3-Azidomethyl-3-nitratomethyloxetane (AMNMO) was obtained by the cyclization, substitution and nitration of 2, 2-dibromomethyl-1, 3-propanediol. Through the cationic polymerization of the monomer AMNMO, a liquid high energetic binder (PAMNMO) was synthesized. The possibility of PAMNMO used as a plasticizer or binder in solid propellants was studied.

100. The Inhibitor of Epoxy Resin with Isocyanurate Group, Gao Chao, Gan Xiao Xian, Qiu Shao Jun, [Xi'an Jiaotong University, Xi'an 710049, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):27-31.

Abstract: A novel epoxy resin containing isocyanurate group (ISEP) and a novel flexible curing agent (TPA) are synthesized. The mechanical properties of the composite by using biurea as filler are studied. Its tensile strength and elongation are 6.44 MPa and 124.15% at 20℃, 2.68 MPa and 85.24% at 50℃, 7.38 MPa and 24.09% at -40℃, respectively. A propellant is inhibited by this composite. The three-way smoke signature results of the inhibitor show that the transmit ratio of visible light and laser exceeds 80 percent, while 90.4% for IR. The thermal stability of the inhibitor is also studied by TGA.

101. A New Way to Synthesize Spherical KDNBF, Li Yu Feng, Zhang Tong Lai, Miao Yan Ling, Zhang Jian Guo, [State Key Lab of Prevention & Control of Explosion, Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):53-56.

Abstract: A new way was introduced to synthesize spherical crystal of potassium 4, 6-dinitrobenzofuroxanate (KDNBF). Crystal modifiers, such as PVA, Tween 80, Span, Na-CMC, Dextrin and Triton X were used to control the shape of KDNBF. Of all the crystal modifiers, Tween 80 behaved most satisfying. The product was characterized by using FT-IR, DSC and elemental analysis techniques.

102. Nitrosation of the Oxidation Products of Hexabenzylhexaazaisowurtzitane, Liu Jiang Qiang, Chen Shu Sen, Yu Yong Zhong, Zhao Xin Qi, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):60-61, 75.

Abstract: With 65% nitric acid / sodium nitrite system on the 6-benzyl-6 hexaazaisowurtzitane oxidation product 4-benzoyl-2-benzyl-6 hexaazaisowurtzitane and 5-benzoyl-1-benzyl-6-aza different alkyl Woods to nitrite solution, the remaining benzyl off will be converted to nitroso benzyl, and the four-benzoyl-2-nitroso-6 hexaazaisowurtzitane and 5-benzoyl-1-nitroso-6 hexaazaisowurtzitane.

103. Hydrolysis of Nitriles with Microwave Irradiation, Zhang Qingshan, Lu Baoping, Guo Bing-nan, [Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):73-75.

Abstract: The hydrolysis of nitriles (benzyl cyanide (1), 4-hydroxybenzonitrile (2) and 5-cyanoindole (3)) to give the corresponding acids (phenylacetic acid (4), 4-hydroxybenzoic acid (5) and 1H indole-5-carboxylic acid (6)) in the present of alkalis in water coupled with microwave irradiation was investigated. The optimum reaction conditions were determined through the test results. The optimum power of the microwave is 530 W and the optimum time of the reaction is 4 min for 1, 4.5 min for 2 and 7 min for 3, respectively. The yield is 87.9% for 4, 85.8% for 5 and 89.6% for 6 respectively.

104. Nitration of Toluene with NO_2-O_2 System, Cai Chun, Lu Chunxu, [Nanjing University of Science & Technology, Nanjing210094, China], Chinese Journal of Explosives & Propellants. 2003, 26(2):1-2, 21.

Abstract: Toluene can be nitrated effectively with the system consisted of nitrogen dioxide and pressurized oxygen in the presence of inorganic oxides as catalysts, the partial pressure of oxygen has considerable effect on reaction results. The ratio of p-MNT in the product could be increased when the pore size of catalyst is similar to the diameter of benzene ring.

105. Synthesis and Properties of 1, 7-diazido-2, 4, 6-trinitro-2, 4, 6-triazoheptane, Zhang Zhi Zhong, Wang Bo Zhou, Shi Zun Chang, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2003, 26(2):3-4, 7.

Abstract: 1, 7-diazido-2, 4, 6-trinitro-2, 4, 6-triazoheptane was synthesized with urotuopine as primary substance by nitration, chlorization and azido substitution steps in turn, the yield is 75.3%. the properties of DATH have been experimentally studied, its density 1.71 g/cm3, melt point 135～137 ℃, detonation velocity 8300 m/s(1.64), heat of combustion 1.08×104 kJ/kg, temperature of decomposition 192 ℃, friction sensitivity 12% (25 kg/cm2, 66°) impact sensitivity 95% (2 kg, 25 cm).

106. Synthesis of Poly(aminotrinitropolyphenylene), Yu Zhan Long, Wu Xiao Qing, [North China Institute of Technology, Taiyuan 030051, China], Chinese Journal of Explosives & Propellants. 2003, 26(2):22-23.

Abstract: Using polytrinitropolyphenylene (PNP) as initial materials, poly (aminotrinitroPhenylene) (PATNP) has been synthesized. The structure and nature of prepared PATNP has been characterized by FTIR, DTA. The stability of PATNP is better than that of PNP and the sensitivity of PATNP is less than that of PNP. PATNP has potential applications in heat resistant explosives.

107. Oxidation of Derivatives of Hexaazaisowurtzitane, Liu Jiang Qiang, Chen Shu Sen, Yu Yong zhong, Zhao Xin Qi, [Beijing Institute of Technology, Beijing100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(1):5-7, 19.

Abstract: The oxidative debenzylation of tetraacetyldibenzylhexaazaisowurtzitane in the system of ammonium peroxydisulfate/cerium ammonium nitrate/acetic anhydride has been studied. The benzyl group of hexabenzylhexaazaisowurtzitane is removed and tetraacetyldibenzylhexaazaisowurtzitane is successfully synthesized by this method.

108. Synthesis of Nanocomposite Bi_2O_3•SnO_2 and Its Effect on Thermal Decomposition of RDX, Hong Wei Liang, Zhao Feng Qi, Liu Jian Hong, [Shenzhen University, Shenzhen 518060, China], Chinese Journal of Explosives & Propellants. 2003, 26(1):37-39, 46.

Abstract: Nano-composite oxide Bi2O3•SnO2 was synthesized by co-precipitation method using BiCl3 and SnCl4•5H2O as the reactant. The particle size, crystal form and phase were determined with XRD and TEM. Average particle size of samples was about 5 nm. The effect of nano-composite oxide Bi2O3•SnO22 on the thermal decomposition characteristics of RDX was investigated by DSC. The results show that due to the effect of nano-composite oxide Bi2O3•SnO2, the peak temperature of thermal decomposition of RDX shifts 13.7℃ downward, the decomposition enthalpy ΔH of RDX increases 665 J/g (about 59.9%), and the apparent activation energy of the thermal decomposition of RDX decreases 48.42 kJ/mol.

109. Characterization of the Structure of Large Particle TATB, Huang Ming, Luo Shun Huo, Tian Ye, [Institute of Chemical Material, CAEP, Mianyang 621900, China], Chinese Journal of Explosives & Propellants. 2002, 25(4):23-24.

Abstract: TATB is synthesized in the enclosed high pressure reactor. Anhydrous gaseous ammonia with a feed pressure of 0.42 MPa is allowed to enter the reactor at 155℃. Trichlrotrinitrobenzene is gained in toluene on the liquid vapor interface after 8 hours. The average particle size of the production is above 40 μm,and sixty percent of the particles surpassed 40 μm. The production is proved to be TATB with FT IR, MS, elementary analysis and items defined in GJB3292 98. Its SEM photograph indicates obviously edges, corners and layers structure.

110. Nitrosation of the Oxidation Products of Hexabenzylhexaazaisowurtzitane, Pang Si Ping, Yu Yong Zhong, Zhao Xin Qi, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2003, 26(3):60-61, 75.

Abstract: Nitrosation of the oxidation products of hexabenzylhexaazaisowurtzitane monoacetyltribenzoyldibenzylh exaazaisowutzitane(3),diacetyldibenzoyldibenzylhexaazaisowu tzitane(4) and triacetylmonobenzoyldibenzylhexaazai sowutzitane (5) by 65% HNO3/NaNO2, the remained benzy1 groups were removed successfully and gave the corresponding nitrosamine products monoacetyltribenzoyldinitrosohexaazaisowutzitane(6),diacetyldibenzoyldinitroso hexaazaisowutzitane(7) and triacetylmonobenzoyldinitrosohexaazaisowutzitane

111. Synthesis of TNAZ via Nitromethane, Bi Wei Yu, Liu Qian, Zhang Zhi Zhong, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2002, 25(4):31-32.

Abstract: The title compound, a known melt castable high performance explosive, was synthesized starting with commercially available nitromethane and formaldehyde via a 5 step process. The overall yield was above 40%. Also, the mechanisms of ring closing/dehydration and oxidative nitration were elucidated in lig-ht of literatures

112. Novel Development of Syntheses and Properties of 1, 3, 3- Trinitroazetidine (TNAZ), Ding Li, Li Ying Bo, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2002, 25(4):42-44, 65.

Abstract: Review of routes for TNAZ synthesis since 1990 is presented. Properties of TNAZ such as physico chemical properties are introduced also. It is stated that TNAZ is highly energetic material more powerful than RDX, and which is suitable for application as a castable explosive as well as a plasticizer.

113. Synthesis of Lead(II) and Copper(II) Salts of 4-Hydroxy-3, 5- dinitropyridine Oxide, Zheng Yu Mei, Deng Min Zhi, Zhao Feng Qi, Yuan Chao, [Shanghai Institute of Organic Chemistry Chinese Academy of Sciences, Shanghai 200032, China], Chinese Journal of Explosives & Propellants. 2002, 25(4):51-52, 13.

Abstract: The paper describes that synthesis of lead(II) and copper(II) salts of 4 hydroxy 3, 5 dinitropyridine oxide in good yields from pyridine via the multiple steps. The salts were characterized by M.S and microanalysis. DSC and TG experimental results of the salts showed that the salts could effectively catalyze the thermal decomposition of RDX, AP and NC+NG. Meanwhile, the decomposition heats of mixtures containing different salts were larger than those of the corresponding pure RDX, AP and NC+NG. The all facts suggested the salts might be better energetic burning catalysts.

114. Effect of Synthesis Method on Crystal Phase of Iron Oxide Nanocrystalline Powders, Liu Xiang Xuan, Wang Xuan Jun, Liu Zhen Yu, Zhu Ming, Li You, [Xi'an Institute of high technology, Xi'an 710025, China], Chinese Journal of Explosives & Propellants. 2002, 25(4):85-86.

Abstract: Iron oxide Nano-crystalline Powders were prepared respectively by precipitation, stearic acid gel, polyethylene glycol gel, and citrate gel and iron citrate combustion. The influence of synthesis method on the final product, such as the crystal structure, crystalline grain size, dispersivity was studied. XRD results show that the pure α Fe2O 3, Fe 3O 4 were synthesized respectively by precipitation, ironic citrate combustion, and mixture of α Fe 2O 3 γ Fe 2O 3 were gained by Sol gol method.

115. Fluorodenitration Using Tetramethylammonium Fluoride for Synthesis of Aromatic Fluorine Compounds, Cai Chun, Lu Chun xu, [Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2002, 25(3):31-32.

Abstract: Tetramethylammonium fluoride (TMAF) could be used as fluorodenitration reagent in synthesis of aromatic fluorine compounds from nitroaromatics. This process has the advantages of mild reaction condition, high yield and little by reaction.

116. Synthesis and Droperties of 3, 3'-dinitroxazafurazan, Shi Yan shan, Li Zhan xiong, Ou Yu xiang, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2002, 25(2):14-15, 27.

Abstract: dinitroxazafurazan (DNOAF) was synthesized from 3, 4 dinaminofurazan as a non hydrogen energetic compound. Its structure has been identified by IR, NMR, MS and elemental analysis .The standard formation enthalpy, detonation velocity and detonation pressure of DNOAF was calculated to be 640 kJ/mol, 9390 m/s and 40.5 GPa respectively. Calculation shows that the specific impulse is 269.2 s -1 of NEPE propellant by substituting 20% of HMX with the title compound (if HNIW was substituted for HMX, the specific impulse is 268.7 s -1.

117. Synthesis of O, O-Bis (β-azidoethyl)-α-(p-toluenesulfonamido)- Substituted-benzyl Phosphite Esters, Ye Ling, Zhou Yu Lan, Xu Rui Xing, [Capital University of Medical Science, Beijing 100054, China], Chinese Journal of Explosives & Propellants. 2002, 25(2):16-18.

Abstract: A serial of Mannich compounds, including O,O bis( β azidoethyl) α (P toluenesultonamido) substituted benzyl phosphite esters and O,O bis( β, β' diazidoispropyl) α (p toluenesulfonamido) m nitrobenzy1 phosphite ester, were firstly synthesized and their structures were verified by IR, 1H NMR and element analysis respectively. In addition, the thermo stabilities of Mannich bases were analyzed by DTA.

118. Study on the Synthesis of Ultrafine Powder of Lead Carbonate, Ma Feng Guo, Zhou Gui Zhong, Liao Shuang Quan, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2002, 25(2):12-16.

Abstract: Study on the synthesis of ultrafine powder of lead carbonate. The Ultrafine powder of lead carbonate crystallites was synthesized by chemical precipitation method. The influences of reaction temperature, reaction time and the ratio of reactants on the formation of lead carbonate crystallites were investigate. The TEM was used to characterize the samples. The graph TEM shows the product was hexaganal crystal and the size ranges from 1 to 15 micron. The results show that with chemical precipitation method, ultrafine powders of lead carbonate can be achieved.

119. Study on the Lab. Synthesis of HMX Using Dinitrogen Pentoxide as the Nitrating Agent, Ge Zhong Xue, Li Gao Ming, Hong Feng, Song Xin Chao, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2002, 25(2):45-47.

Abstract: The method of synthesizing HMX is presented in this paper. Using DADN (1, 5 diacetyl 3, 7-dinitro 1, 3, 5, 7 tetranitrotetrazacycloctane) as reactant, the HMX was synthesized in the nitrating agent of the mixture of dinitrogen pentoxide and nitric acid. The yield of HMX was more than 96%, mp 272.0 - 272.8. In addition, factors that affecting the yield of HMX were discussed preliminary.

120. Study on the Preparation Technique of M-cresol From M-toluidine, Hao Yan Xia, Chen Shu Sen, [Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 2002, 25(2):64-66.

Abstract: A new thought for preparing m cresol from m nitrotoluene via reduction, diazotiation and hydrolsis is proposed in this paper. The procedure of synthesizing m cresol from m nitrotoluene is researched mainly and the better reaction condition was acquired by the orthogonal. The yield of m cresol is above 77% under this reaction condition. Moreover, the effect of copper salt on the hydrolysis procedure of diazonium salt is discussed.

121. New Synthesis of TATB in USA, Wang Zhen-yu, Guo Hui-li, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2001, 24(4):68-70.

Abstract: Two kinds of new synthesis method of TATB are introduced. Picramide was used as reactant in one method, sonochemically-aminated TATB was synthesised in the other method.

122. Synthesis of Nanometer PbO, Bi_2O_3 and Their Effect on Burning Properties of Solid Propellants, Hong Wei Liang, Zhao Feng Qi, Liu Jian Hong, Tian De Yu, [Department of Chemistry and Biology, Normal College, Shenzhen University, Shenzhen 518060, China], Chinese Journal of Explosives & Propellants. 2001, 24(3):7-9.

Abstract: Nanometer PbO and Nanometer Bi2O3 were synthesized by solid state reaction using Pb(NO3)2, Bi(NO3)3 with NaOH at room temperature. The crystal form, particle size and morphology of nanometer PbO and Bi2O3 were characterized by XRD and TEM. The effect of two nanometer catalysts on burning Properties of RDX CMDB propellant was investigated. The results show that nanometer Bi2O3 can increase the burning rates of the propellant and lower burning rate pressure exponent.

123. Study on Nitrolysis of TADCIW, Liu Li Hua, Ou Yu Xiang, Wang Jian Quan, Cheng Bo Ren, Lei Xiang Yang, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2001, 24(3):16-19.

Abstract: The effects of nitrolysis agents and reaction conditions on the purity and yield of nitrolysis product of tetraacetyldichloroacetylhexaazaisowurtzitane (TADCIW) were investigated, and the related reaction mechanism was discussed. Tetranitrodichloroacetylhezaazaisowurtzitane (TNDCIW) with high purity could be obtained in high yield (94%～98%) by nitrolysis of TADCIW using a mixture of fuming nitric acid and concentrated sulfuric acid or a mixture of alkali metal nitrate and concentrated sulfuric acid as nitrolysis agents. Besides, the mixture acid from fuming acid and concentrated sulfuric acid could be reused. In the case of nitrolysis agent of a mixture of fuming nitric acid and phosphorus pent-oxide or a mixture of concentrated nitric acid and concentrated sulfuric acid, the yield of TNDCIW was quite low (13%～40%).

124. The Improvement of Synthetical Techniques of Tetranitrodibenzo-1, 3a, 4, 6a-Tetrazapentalene, Li Zhan Xiong, Ou Yu Xiang, Chen Bo Ren, [Beijing Institute of Technology, Beijing 100081, China], Chinese Journal of Explosives & Propellants. 2001, 24(2):32-34.

Abstract: TACOT was synthesized by the improved techniques, the time of reaction was shortened to a half, and the operation was predigested. Moreover, the total yields have been increased from 26.7% to 52.0%. These methods reduced the cost of TACOT greatly.

125. Synthetic Principle and Application of Lubricant G for Glass Fiber, Ren Chuan Rong, Li Tao Qi, Yao Yi Lun, [Xi'an Modern Chemistry Research Institute, Xi'an 710065, China], Chinese Journal of Explosives & Propellants. 2001, 24(2):69-72.

Abstract: This paper describes a new idea on condensation reaction principle of dicyanodiamide and formal dehyde according to manufacture of lubricant G for glass fiber, and the synthetic technology and the application are discussed.

126. Synthesis of 2, 4, 6-Trinitro 2, 4, 6-triazacyclo-hexanone (Keto RDX), Zhang Yue Jun, [Nanjing University of Science and Technology, Nanjing 210094, China], Chinese Journal of Explosives & Propellants. 1999, 22 (4):1-3, 6.

Abstract: This paper reports the method of synthesizing 2, 4, 6 tri-nitro 2, 4, 6 triazacyclohexanone (Keto RDX) from DPT (or PHX) and urea (or nitrourea) in several kinds of nitrating agents. There are primary investigations on reaction forms of nitrolysis fragments of DPT, PHX and BSX, and on the mechanism of forming by products. Experimental results showed that the nitrolysis fragments N, N dihydroxymethylamines that were not directly substituted by nitro groups condensed with urea or nitrourea to form Keto RDX, while N, N dihydroxymethylnitroamine did not. Using DPT as a reactant, the yield of Keto RDX was 69% (one mole Keto RDX per mol reactant), and by products were HMX, RDX and small molecule fragments. Using PHX, the yield was 36%, and by products were HMX and small molecule fragments. While using BSX, no Keto RDX product and no cyclonitroamine by products were obtained.