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Synthesis and Crystal Structure of 4-(4,6-Dimethoxylpyrimidin-2-yl)-3-thiourea Carboxylic Acid Ethyl Ester

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Chinese Journal of Structural Chemistry 2008年第2期27卷 195-199页

作者： ZHANG Yang HUANG Jie SONG Ji-Rong REN Ying-Hui xu kang-zhen Department of Chemical Engineering Shaanxi Key Laboratory of Physico-inorganic Chemistry Northwest University Xi＇an 710069 China Conservation Technology Department the Palace Museum4 Jingshan Qianjie Beijing 100009 China

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.

关键词： 4-(4,6-dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester,synthesis crystal structure, ^-~ aromatic stacking interactions

Non-isothermal Decomposition Kinetics of K(AHDNE)

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Chemical Research in Chinese Universities 2012年第5期28卷 878-881页

作者： LU Lei xu kang-zhen QIU Qian-qian WANG Gang SONG Ji-rong ZHAO Feng-qi College of Chemistry and Chemical Engineering Yan'an UniversityYan'an 716000P.R.China School of Chemical Engineering Northwest UniversityXi'an 710069P.R.China Xi'an Modern Chemistry Research Institute Xi'an 710065P.R.China

The thermal behavior and non-isothermal decomposition kinetics of 1-amino-1-hydrazino-2,2-dinitro-ethylene potassium salt[K（AHDNE）] were studied under the non-isothermal conditions by different scanning calorimeter（DSC） method. The thermal behavior of K（AHDNE） presents three exothermic decomposition processes. The kinetic equation of the first thermal decomposition reaction obtained is dα/dT=（1019.63/β）3（1-α）[-ln（1-α）]2/3exp（-1.862× 105/RT）. The self-accelerating decomposition temperature（TSADT） and critical temperature of thermal explosion（Tb） of K（AHDNE） are 162.5 and 171.4 °C, respectively. K（AHDNE） has higher thermal stability than AHDNE.

关键词： 1-Amino-1-hydrazino-2 2-dinitroethylene(AHDNE) Potassium salt Non-isothermal decomposition kine- tics

Synthesis,Crystal Structure and Thermal Behavior of 4,5-Dimethoxy-2-(dinitromethylene)imidazolidine

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Chemical Research in Chinese Universities 2012年第4期28卷 716-720页

作者： WANG Min xu kang-zhen HE Fei ZHANG Hang CHEN Yong-shun SONG Ji-rong ZHAO Feng-qi School of Chemical Engineering Northwest UniversityXi'an 710069P.R.China The Palace Museum Beijing 100009P.R.China Science and Technology on Combustion and Explosion Laboratory Xi'an Modern Chemistry Research InstituteXi'an 710065P.R.China

A new energetic material,4,5-dimethoxy-2-（dinitromethylene）imidazolidine（DMDNI）,was synthesized by the reaction of 4,5-dihydroxyl-2-（dinitromethylene）-imidazolidine（DDNI） and methanol,and structurally characterized by single crystal X-ray *** crystallized in triclinic space group P1,with crystal data a=0.4324（4） nm,b=1.3599（11） nm,c=1.7503（14） nm,α=77.406（14）°,β=84.494（15）°,γ=87.976（14）°,V=0.9997（14） nm 3,Z=4,μ=0.140 mm-1,F（000）=488,D c =1.556 g/cm ^3,R 1 =0.0773 and wR 2 =*** decomposition of DMDNI was studied,and its thermal decomposition process was divided into two *** first stage was a melting process and the second stage was an exothermic decomposition *** enthalpy,apparent activation energy and pre-exponential constant of the exothermic decomposition reaction are-491.5 J/g,142.3 kJ/mol and 10 14.24 s^-1,*** critical temperature of thermal explosion is 162.47 °*** has a lower thermal stability than DDNI but it is close to that of 4,5-diacetoxyl-2-（dinitromethylene）-imidazolidine（DADNI）.

关键词： Crystal structure Thermal behavior 4 5-Dimethoxy-2-(dinitromethylene)imidazolidine(DMDNI) 1 1-Diamino-2 2-dinitroethylene(FOX-7)

Thermal Behavior, Specific Heat Capacity and Adiabatic Time-to-explosion of GDN

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Chemical Research in Chinese Universities 2009年第1期25卷 76-80页

作者： YANG Xing-kun xu kang-zhen ZHAO Feng-qi YANG Xin WANG Han SONG Ji-rong WANG Yao-yu College of Chemistry and Chemical Engineering Xinyang Normal University Xinyang 464000 P. R. China Xi＇an Modern Chemistry Research Institute Xi＇an 710065 P. R. China Shaanxi Key Laboratory of Physico-inorganie Chemistry Northwest University Xi＇an 710069 P. R. China

A new compound, [（NH2）2C=NH2]＋N（NO2）2-（GDN）, was prepared by mixing ammonium dinitramide （ADN） and guanidine hydrochloride in water. The thermal behavior of GDN was studied under the non-isothermal conditions with DSC and TG/DTG methods. The apparent activation energy（E） and pre-exponential constant（A） of the exothermic decomposition stage of GDN were 118.75 kJ/mol and 10^10.86 s^-1, respectively. The critical temperature of the thermal explosion（Tb） of GDN was 164.09 ℃. The specific heat capacity of GDN was determined with the Micro-DSC method and the theoretical calculation method, and the standard molar specific heat capacity was 234.76 J·mol^-1·K^-1 at 298.15 K. The adiabatic time-to-explosion of GDN was also calculated to be a certain value between 404.80 and 454.95 s.

关键词： Guanidine dinitramide Ammonium dinitramide Thermal behavior Specific heat capacity Adiabatic time-to-explosion

Synthesis,Crystal Structure and Thermal Properties of Zn（NH3）3（AFT）2

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Chinese Journal of Structural Chemistry 2019年第7期38卷 1173-1181页

作者： MA Xiao DING Zi-Mei SHANG Fan HANG Xiao-Jing WANG Xiao-Hong xu kang-zhen HUANG Jie School of Chemical Engineering Northwest University/Shaanxi Key L aboratory of Physico-in organic Chemistry Xi 'an 710069 China Xi 'an Modern Chemistry Research Institute Xi 'an 710065 China

A new coordination compound of Zn(NH3)3(AFT)2(1,ZnC6H13N17O2,AFT =4-amino-3-(5-tetrazolate)-furazan)was synthesized and characterized by elemental analysis and FT-IR *** crystal structure was determined by X-ray single-crystal *** crystal belongs to the orthorhombic system,space group Pnma with a = 18.680(3),b = 6.9438(11),c =12.268(2)A,μ= 1.592 mm-1,V= 1591.3(4)A3,M,= 420.72,Dc=1.756 g·cm^-3,Z= 4,F(000)= 860,the final R = 0.0480 and wR = 0.1262 for the observed reflections with I>2σ(Ⅰ).The zinc(Ⅱ)ion is five-coordinated by N atoms from two AFT"ligands and three NH3 *** thermal decomposition mechanism of compound 1 was tested by differential scanning calorimetry(DSC)and thermogravimetry-derivative thermogravimetry(TG-DTG)*** DSC curve exhibits two endothermic and one exothermic *** addition,the non-isothermal kinetics parameters were calculated by using the Kissinger s method and Ozawa-Doyle's ***,the entropy of activation(ΔS≠),enthalpy of activation(ΔH≠),free energy of activation(ΔG≠)and impact sensitivity(IS)was also obtained.

关键词： 4-amino-3-(5-tetrazolate)-furazan synthesis crystal structure thermal behavior

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差示分光光度法测定桑叶总黄酮含量

光谱实验室 2005年第3期22卷 506-508页

作者：康旭珍晋中学院化学系

以芦丁为观测指标,差示分光光度法测定桑叶总黄酮化合物的含量,以控制桑叶的品质。在420nm波长下,芦丁对照品在2.575-15.450μg/mL范围内,差示吸收值(△A)与浓度呈良好线性关系(r=0.9997),回归方程为△A=0.0055+0.03579C,平均加样回收率... 详细信息

以芦丁为观测指标,差示分光光度法测定桑叶总黄酮化合物的含量,以控制桑叶的品质。在420nm波长下,芦丁对照品在2.575-15.450μg/mL范围内,差示吸收值(△A)与浓度呈良好线性关系(r=0.9997),回归方程为△A=0.0055+0.03579C,平均加样回收率为102.64%,RSD为1.08%(n=6)。差示分光光度法具有操作简单、结果真实准确、重现性好等优点,可作为桑叶品质控制检测方法。

关键词：桑叶,黄酮化合物,差示分光光度法

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乙炔银-硝酸银的热分解特性

含能材料 2022年第7期30卷 666-672页

作者：徐海斌徐畅魏欣万冲徐抗震西北核技术研究所陕西西安710024 西北大学化工学院陕西西安710069

为了促进光敏炸药乙炔银-硝酸银配合物(Ag_(2)C_(2)·Ag NO_(3))的稳定生产和应用,采用X射线粉末衍射仪、傅里叶红外光谱仪、扫描电镜、差示扫描量热仪和热重-质谱-红外三联用技术等对其结构形貌和热分解特性进行了研究。结果表明,制备... 详细信息

为了促进光敏炸药乙炔银-硝酸银配合物(Ag_(2)C_(2)·Ag NO_(3))的稳定生产和应用,采用X射线粉末衍射仪、傅里叶红外光谱仪、扫描电镜、差示扫描量热仪和热重-质谱-红外三联用技术等对其结构形貌和热分解特性进行了研究。结果表明,制备的Ag_(2)C_(2)·Ag NO_(3)呈纳米球状,粒径在400~500 nm之间;Ag_(2)C_(2)·Ag NO_(3)只有1个放热分解过程,10.0℃·min^(-1)升温速率下分解峰温为234.9℃,分解过程失重率为8.72%,放热量高达1449 J·g^(-1),分解过程的表观活化能和指前因子分别为108.9 k J·mol^(-1)和10^(8.94)s^(-1);Ag_(2)C_(2)·Ag NO_(3)的气相分解产物为NO、NO_(2)和CO_(2)。

关键词：乙炔银-硝酸银 TG-MS-FTIR 热分解表观活化能气体产物

Synthesis,Crystal Structure,Specific Heat Capacity,Thermodynamic Properties and Heat of Formation of N-(benzoyl)-N-(2,4-dinitrophenyl amino) thiourea

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Synthesis,Crystal Structure,Specific Heat Capacity,Thermodyn...

Study on Heat of Formation of ZTO and its Five Coordination Compounds by Combustion Calorimeter

中国化学会第五届全国热分析动力学与热动力学学术会议

作者： Hu Wei GUO Jia-jia HUANG Jie xu kang-zhen SONG Ji-rong Department of Chemical Engineering Shaanxi Key Laboratory of Physico-Inorganic ChemistryNorthwest University Conservation Technology Department the Palace Museum

N-(benzoyl)-N’-(2,4-dinitrophenyl amino) thiourea was synthesized via the reaction of2,4-dinitrophenylhydrazine alter with potassium sulfocyanate and ethyl chloroacetate in ethyl acetate in the presence of a catalysis *** structure was characterized by elemental analysis and *** Single crystal of the title compound was obtained by slowly evaporating solvent method at the room *** crystal structure was firstly determined with X-ray single-crystal *** specific heat capacity of the title compound was determined by a Micro-DSC method,and the thermodynamic functions were calculated through thermodynamic relationship within 283.1 K-353.2 *** thermal decomposition behavior was studied under a non-isothermal condition by DSC *** combustion heat of the title compound was determined by IKA C5000 oxygen-bomb calorimeter,and its standard molar enthalpies of formation(⊿H) were calculated with Hess’ s law.

关键词： X-ray diffraction Crystal structure Specific heat capacity Thermodynamic properties

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Study on Heat of Formation of ZTO and its Five Coordination ...