Recycling of exercise torpedo will produce a large amount of fuel containing seawater.To ensure the safety of processing of seawater contaminated OTTO-Ⅱ,DSC and HPLC was used to study the composition and stability after mixing of pure OTTO-Ⅱ with seawater at different temperatures and durations.Results show that DBS decreases with the increase of mixing temperature,which may be related to the saponification of DBS at high temperature.Thermal decomposition performance of OTTO-Ⅱ is not obviously affected by seawater.This research may provide technical and safety reference for the separation and recovery of fuel containing seawater.

An energetic plasticizer 4,4,4-trinitrobutyric acid 2-azido-1-azidomethyl-ethyl ester(DPTB) was synthesized via esterifi-cation reaction from 4,4,4-trinitrobutyric acid(TNB) and 1,3-diazido-propan-2-ol(DAG),in which,TNB was prepared via nitration-hydrolysis and addition reaction using 4,6-dihydropyrimidine as raw material,and DAG was prepared via azidation by 1,3-dichloro-propan-2-ol as raw material.The structure of DPTB was characterized by IR,NMR and elemental analyses.In synthesis,traditional esterification method was replaced by dicyclohexylcarbodiimide (DCC)/dimethylaminopyridinium p-toluenesulfonate (DPTS) catalytic esterification method.The effects of material ratio,reaction temperature,reaction time and solvent dosage on the esterification reaction were investigated.The thermal decomposition properties of DPTB were studied by thermogravimetry (TG) and differential scanning calorimetry(DSC).Results shw that replacing traditional esterification method with DCC/DPTS catalytic esterification method makes the yield of DPTB promote from 1 7.9％ to 44.9％.There are two exothermic peaks at 215 ℃ and 230 ℃ on DSC curve of DPTB.Its TG curve can be divided into two stages:first-stage is from147 ℃ to 220 ℃ accompanied with 76.68％ mass loss;second-sstage is from 220 ℃ to 351 ℃ accompanied with 1 5.23％ mass loss and the total mass loss from start to the end of decomposition reaction is 91.19％.

A new method for the synthesis of 1,4,5,8-tetranitro-1,4,5,8-tetraazabicyclo[4. 4. 0]decalin (TNAD) was studied. This compound was prepared from the raw material 1,4,5,8- tetraazabicyclo[4. 4. 0]decalin (THAD) via salt-forming reaction and nitrolysis. The total yield could reach as high as 90%, and the purity is 98. 7%. Structure of the product was characterized by IR, 1 H NMR and elemental analysis. The effects of nitrification system, reactant ratio, reac-tion temperature and reaction time on the yield have been investigated. Results show that the optimum reaction conditions of the reaction are determined as:n (THAD.4HNO3)︰n(98%HNO3)︰n (AC2O) = 1︰24︰15. Meanwhile, the best reaction temperature is 25 ℃ and the best reaction time is 2 h.

TMNTA was synthesized using tris( hydroxymethyl) nitromethane as raw material,via the two?step reactions of esterif?ication, azidonation with a total yield of 83.0%.Its structures were confirmed by IR,NMR and elemental analysis.The affecting fac?tors of azidonation were studied.The optimum conditions of the reactions were:nexp:ntheory=1.10 for NaN3(molar ratio),10%~25% of the total volume of acetone?H2 O and reaction time 1 h. Some physicochemical properties of TMNTA were obtained by the tests.Results show that the density is 1.45 g/cm3,decomposition temperature is 235.7℃,glass transition temperature is-26.23 ℃, H50=44.7cm(2 kg),friction sensitivity is 4%(66°).

N,N′,N″-trihydroxyisocyanuric acid (THICA) with MnO2 promotes the aerobic oxidation of toluene derivatives to corresponding acids in PEG-1000-based dicationic acidic ionic liquid (PEG1000–DAIL). It is demonstrated that THICA/MnO2 is very active and selective and several toluene derivatives are efficiently oxidized to corresponding acids under mild conditions. Both the catalyst and PEG1000–DAIL can be reused after simple separation. A plausible mechanism is also proposed based on the experimental observations. Copyright © 2015 John Wiley & Sons, Ltd.

Triazidotriacetin( TAA)was synthesized via esterification and azidonation using propanetriol as raw material. The over-all yield was 84. 1%. The structures of intermediates and target compound were characterized by IR,NMR and elemental analysis. The factors affecting esterification and azidonation reactions were discussed. Results show that the optimum conditions of azidona-tion reaction are determined as:the dosage of NaN3 is 1.10 times of theoretical value,i. e. nexp ∶ ntheo=1.10(molar ratio),the dosage of water is 5% ~25% of the total volume of acetone-water mixed solvent,and the reaction time is 10 h. The yield of TAA is 95. 0% and its purity more than 96. 8%.

以偕二硝基丙二醇、甲醛和叔丁胺为原料,经过Mannich反应缩合得到1,3-二叔丁基-5,5-二硝基六氢嘧啶中间体。中间体经硝化反应合成出目标物1,3,5,5-四硝基六氢嘧啶（DNNC）,总收率达到76%,纯度达到99%。采用红外、核磁、质谱和元素等分析手段对其结构进行了表征,借助差热扫描分析方法（DSC）研究了DNNC的热性能,并测定了其机械感度。结果表明,DNNC的分解温度为222.2℃,摩擦感度为60%,撞击感度为28.5 cm。表明DNNC具有较好的热稳定性和较低的机械感度。

The coordination compound of [Ni(IMI)6](NO3)2(IMI:imidazolium)was prepared by reaction of imidazole with nickel nitrate,single crystal of [Ni(IMI)6](NO3)2 was obtained.The elemental analysis,IR and single X-ray diffraction analysis showed that the crystal belongs to a monoclinic system with P21/n space group and cell parameters of a=1.235 0(3)nm,b=1.235 0(3) nm,c=1.480 0(3) nm,β=90.579(2)°,V=1.955 0(7)nm3,Dc=1.491 g/cm3,Z=4,F(000)=900,R1=0.034 4,wR2=0.095 5.The compound [Ni(IMI)6](NO3)2 formed by [Ni(IMI)6]2+ and(NO3)-belong to an ionic compound.The central Ni(II) ion is six-coordinated with six imidazoles.

Using 2-(5-ethyl-2-pyridyl)ethanol as starting materials,pioglitazone hydrochloride is synthesized by condensation,reduction,diazotization,cyclization,hydrolysis and saltilization,and the yield is 32%.The structure of compound is confirmed by IR,1H NMR and elemental analysis.

Neopentyl glycol diazo dinitrate(PDADN) was synthesized by one-pot process which consisted of two steps, i.e.nucleophilic substituion of 1, 3-dibromo-2, 2-dihydroxylmethylpropane(DBDMP) with sodium azide(SA), and nitration of the substituted intermediate (1, 3-diazido-2, 2-dihydroxylmethylpropane) with nitric acid(NA), but carried out in one pot without separating the intermediate. The factors affecting the yield and purity of PDADN, such as ratio of DBDMP/SA/NA, nitration temperature (T) and time (t) were investigated. The optimized process conditions were: DBDMP/SA/NA (molar ratio)=1.0/2.1/8.0, T=(15~19)°C, and t=18 min. The yield and purity of the resulting PDADN could be up to 84% and 98% repectively, and the product's structure was identified with IR, NMR and elemental analysis. To compare with the traditional preparation of PDADN, the one-pot process simplifies the procedures, improves PDADN's yield and purity, mildens the reaction conditions, and is easy to be industrialized.

介绍了叠氮硝酸醋含能增塑剂的应用性能和研究现状.分析比较了硝酸醋类、硝酸醋局部叠氮化和完全叠氮化等叠氮硝酸醋的性能.指出叠氮硝酸醋类化合物是一种具有应用前景的新型含能增塑剂,并对含能增塑剂的研究方向提出了建议.

Reaction of 2,6-dihydroxyacetophenone (1) with benzoyl chloride under phase-transfer catalysis by tetrabutyl ammonium bisulfate formed 5-hydroxyflavone (2) in 65% yield at 60℃ with n (1):n (tetrabutylammoniumbisulfate)=1∶1.3. 1 was synthesized from resorcinol in four steps including cyclization, esterification, rearrangement and ring-opening. The structures of 1 and 2 were identified by IR and 1H NMR. Mechanisms for formation of 1 and 2 were also proposed.

Synthesis of 4-oxo-4-phenyl-2-butenoic acid ethyl ester from maleic anhydride, benzene and ethanol was achieved. The overal yield reached 81%.

7-Hydroxyflavone(Ⅲ) was obtained by means of phase-transfer catalysis from 2,4-dihydroxyacetophenone and benzoyl chloride using tetrabutylammonium bisulfate as phase transfer catalyst through one-pot reaction.The yield of Ⅲ was 60%.Mechanism for Ⅲ formation was proposed,and mass spectrum of Ⅲ was resolved.2,4-Dihydroxyacetophenone(Ⅱ) was also synthesized from resorcinol(Ⅰ) and acetic acid,the yield of Ⅱ was 70%.

The phenylphosphonic diamide was synthesized from phenylphosphonic dichloride and ammonia.The influencing factors of nitride reaction were investigated.The optimum reaction condition were:the reaction temperature is-25～-20 ℃,the reaction solvent is diethyl ether,the ammonia is 0.6 L/min,the yield of phosphonic diamide is over 90%.The process is simple,the reaction condition is mild and the process of synthesis is easy to implementation.

[Pb(DNI)2(H2O)4] was prepared by mixing the aqueous solution of sodium 2,4-dinitroimidazolate and lead nitrate.The single crystal structure of [Pb(DNI)2(H2O)4] has been determined by single crystal diffraction analysis.The crystal monoclinic space group Cc with crystal parameters of a=6.517(3)×10-1 nm,b=17.131(6) ×10-1 nm,c=14.082(7)×10-1 nm,α= 90.00(3) °,β=97.80(4)°,γ=90.00(4) °,V=1 557.5(12)×10-3 nm3,Z=4,Dc=2.531 g/cm-3,μ=11.001 mm-1,F(000)=1 120.The final deviation factor R is 0.022 6.According to the IR spectra analysis,the element analysis and the X-ray diffraction analysis,the chemical component of the 2,4-DNI lead complex is C6H10O12N8Pb and its formula is [Pb(DNI)2(H2O)4].

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, ~(1)HNMR and elemental analysis.

1-methyl-3-n-propyl-pyrazole-5-carboxylic acid was synthesized by some processes such as ester condensation, cyclization, hydrolysis from diethyl oxalate and 2-pentanone, the total yield was (73.26%.) The product was characterized by IR, ()~1HNMR and elementary analysis etc.

以1,3-二氯丙醇-(2)为原料成功地合成了硝化甘油二叠氮取代物--1,3-二叠氮基-2-硝酸酯基丙烷(DANG),并对DANG性能进行了初步测试.试验结果表明,DANG的凝固点明显低于NG的凝固点,而危险等级与硝甘相当或略低.