In-situ Synthesis of ZSM-5 with Different Si/AlRatios on Honeycomb-shaped Cordierite and their Behavior on NO Decomposition

Zeolites ZSM-5 with different Si/Al ratios were in-situ synthesized on the surface ofhoneycomb-shaped cordierite support for the first time. Characterizations of XRD and SEM wereperformed and it has been proved that the zeolite ZSM-5 was grown on the surface of the cordieritehomogeneously. NO decomposition on the Cu exchanged ZSM-5/cordierite monolith catalysts wasalso studied. It was found that the monolith catalysts have a fine initial activity at 673K and GHSVof 10,000h-1. Such method should be a good way to make auto exhaust converter with monolithcatalyst for NOx removal.

Synthesis,Crystal Structure and Thermal Decomposition of a New Energetic Potassium Salt of Bis(dinitromethyl)difurazanyl Ether

A new energetic organic potassium salt bis（dinitromethyl）difurazanyl ether potas- sium salt [K2（BDFE）] was synthesized, and structurally characterized by elemental analysis, IR spectra, t3C NMR and single-crystal X-ray diffraction. K2（BDFE） crystallizes in monoclinic system, space group C2/c with a = 17.342（3）, b = 12.6943（17）, c = 8.0972（11） A, β = 110.630（2）°, V = 1668.3（4） A3, Z = 4, Dc = 2.000 g/cm3, F（000） = 1000,μ= 0.675 mm-1, S = 1.058, the final R = 0.0499 and wR = 0.1452. The K ion is eight-coordinated with eight O atoms from one water molecule and four bis（dinitromethyl）difurazanyl ethers （BDFE）, forming a distorted dodecahedral structure. Thermal decomposition of the title complex was studied by using DSC and TG-DTG. There are primarily two exothermic decomposition processes between 200 and 370 ℃.

Synthesis, Characterization and Thermal Decomposition Mechanism of Cetyltrimethyl Ammonium Tetrathiotungstate

The synthesis, characterization and thermal decomposition mechanism of cetyltrimethyl ammonium tetrathiotungstate （CTriMATT） were studied herein. The as-synthesized CTriMATT was characterized by Elemental analysis, X-ray diffraction （XRD）, Fourier transform infrared （FT-IR）, Ultraviolet visible （UV-Vis） spectra. The results showed that the as-synthesized CTriMATT had high purity and good crystallinity. The introduction of alkyl groups induced a shift of the stretching vibration band of W-S bond to lower wavenumber, while it had no influence on the position of WS4^2-. Thermogravimetric analysis （TG）, differential thermal analysis （DTA） and in situ XRD characterizations revealed that CTriMATT began to decompose at 423 K in nitrogen and was converted to WS2 eventually. In addition, the decomposition product of CTriMATT at 673 K in nitrogen was characterized by N2 adsorption （BET） and scanning electron microscopy （SEM）. The results demonstrated that WS2 with higher specific surface area, and pore volume could be obtained from the thermal decomposition of CTriMATT in nitrogen.

Characterization and performance of Cu/ZnO/Al_2O_3 catalysts prepared via decomposition of M(Cu,Zn)-ammonia complexes under sub-atmospheric pressure for methanol synthesis from H_2 and CO_2

Methanol synthesis from hydrogenation of CO2 is investigated over Cu/ZnO/Al2O3 catalysts prepared by decomposition of M（Cu,Zn）-ammonia complexes （DMAC） at various temperatures.The catalysts were characterized in detail,including X-ray diffraction,N2 adsorption-desorption,N2O chemisorption,temperature-programmed reduction and evolved gas analyses.The influences of DMAC temperature,reaction temperature and specific Cu surface area on catalytic performance are investigated.It is considered that the aurichalcite phase in the precursor plays a key role in improving the physiochemical properties and activities of the final catalysts.The catalyst from rich-aurichalcite precursor exhibits large specific Cu surface area and high space time yield of methanol （212 g/（Lcat·h）;T=513 K,p=3MPa,SV=12000 h-1）.

Combustion Synthesis of La0.8Sr0.2MnO3 and Its Effect on HMX Thermal Decomposition

Perovskite-type La0.8Sr0.2MnO3 was prepared by stearic acid gel combustion method.The obtained powders were characterized by X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FT-IR),scaning electron micrograph(SEM)and X-ray photoelectron spectroscopy(XPS)techniques.The catalytic activity of La0.8Sr0.2MnO3 was investigated on thermal decomposition of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX)by thermal gravity-differential scanning calorimetry(TG-DSC)techniques.The experimental results show that La0.8Sr0.2MnO3 is an effective catalyst for HMX thermal decomposition.The surface-adsorbed species such as H2O,OH - and adsorbed oxygen(Oad)could result in an advance in the onset temperature of HMX thermal decomposition.The mixture system of Mn 3+ and Mn 4+ ions and lattice oxygen could play key roles for the increase of the decomposition heat of HMX because these exothermic reactions could be catalyzed by La0.8Sr0.2MnO3 between CO and NOx(from the thermal decomposition of HMX)and the oxidation reaction of CO.According to the previous researches and our results,perovskite-type La0.8Sr0.2MnO3 may be used as a novel catalyst or modifier for nitrate ester plasticized polyether(NEPE)propellant.

Synthesis and Thermal Decomposition Mechanism of Rare Earth Benzoates

The rare earth metal benzoates were synthesized using hydrothermal reaction. The complexes were characterized by elemental analysis, IR and X-ray powder diffraction. They can be represented by general formula RE (C6H5COO)(3)(RE = La, Nd, Sm, Eu, Gd, Dy and Er). All of them are monoclinic and have layered structure. The mechanism of thermal decomposition of rare earth metal benzoates was studied by using TG, DTA, IR, and gas chromatography-mass spectrometry. The thermal decomposition of the rare earth benzoates in nitrogen proceeded in two stages; firstly it decomposed to form RE2O(CO3)(2) and organic compounds, then RE2O(CO3)(2) decomposed further to form rare earth metal oxides and carbon dioxide. The organic compounds obtained from the first step of the reaction are mainly benzophenone, 9,10-anthraquinone, 1, 3-Diphenylisobenzofuran and so on.

Salt-Assisted Combustion Synthesis of NdCoO_3 Nanoparticles and Their Catalytic Properties in Thermal Decomposition of Ammonium Perchlorate

Highly dispersed perovskite NdCoO3 nanoparticles were prepared by a novel salt-assisted combustion process. The effects of NaCl content and calcination temperature on the characteristics of the products were characterized by X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and BET surface area measurement. The facile introduction of NaCl in the conventional combustion synthesis process was found to result in the formation of well-dispersed perovskite nanoparticles and increase specific surface areas of the resultants from 1.7 to 43.2 m2·g-1. The catalytic properties of the typical NdCoO3 samples for thermal decomposition of ammonia perchlorate (AP) and their correlation with the NdCoO3 microstructure were investigated by Differential Scanning Calorimetry (DSC). The DSC results indicate that the addition of the amorphous NdCoO3 nanoparticles to AP incorporates two small exothermic peaks of AP into a strong exothermic peak, decreases the temperature of the AP exothermic peak to 314.0 ℃ by reduction of 138.3 ℃ and increases the apparent decomposition heat from 515 J·g-1 to over 1441 J·g-1, showing the intense catalytic activity for thermal decomposition of AP. It is also clear that the catalytic activity of the resultant NdCoO3 is related to their microstructure. According to Kissinger′s method, the kinetics parameters of the thermal decomposition of AP catalyzed by the as-prepared NdCoO3 samples were calculated to account for the order of their catalytic activity.

Thermal decomposition and cobalt species transformation of carbon nanotubes supported cobalt catalyst for Fischer-Tropsch synthesis

The effect of calcination condition on the cobalt species and Fischer-Tropsch synthesis （FTS） was studied. It was found that higher calcination temperature resulted in decreased FTS activities because CNTs were consumed by oxidation in air at temperature higher than 230 ℃. Cobalt species went through transformation from Co304 to metallic Co in Ar by autoreduction at temperature over 500℃. The autoreduction route might be Co3O4→CoO→C0 or Co3O4→Co2C→Co. Reduction at temperature higher than 500 ℃ also resulted in decreased FTS activities due to the methanation of CNTs in hydrogen.

Synthesis Characterization Non-isothermal Kinetics of the Thermal Decomposition and Redox Properties Derived from Copper(Ⅱ) Binuclear Coordination Compound of 1,4-Bis-(1'-Phenyl-3'-Methyl-5'-Pyrazolone-4')-1,4-Butanedione

The paper reports the synthetic procedure and character of Copper(II) binuclearcoordination compound of 1,4-bis-(1'-phenyl-3'-methyl-5'-pyrazolone Thenon-isothermal kinetics of thermal decomposition of the complex has been stUdied from the TG-DTGcurves by means of the Achar et al. and Coats-Redfern methods,the most probab1e kinetic equation canbe expressed as dofdtrAe -E / RT * l /(2Q).The corresponding kinetic compensation effect expressions arefound to be lnuA=0. 1794E+0. 1689.The non-isothermal thermal decomposition process of the complex isone-dimensional diffusion.But electrochemical studies of the complex(Cu2L'2)from cyclic voltamrnetriccurves by means of powder microelectrodes technique'',shows one two-electron irreversible process.

Nickel ferrite spinel as catalyst precursor in the dry reforming of methane:Synthesis,characterization and catalytic properties

Dry reforming of methane by CO2 using nickel ferrite as precursor of catalysts was investigated.Nickel ferrite crystalline particles were prepared by coprecipitation of nitrates with NaOH or ammonia followed by calcination,or by hydrothermal synthesis without calcination step.The textural and structural properties were determined by a number of analysis methods,including X-ray diffraction （XRD）,Raman spectroscopy and X-ray photoelectron spectroscopy （XPS）,among which X-ray diffraction （XRD） was at room and variable temperatures.All synthesized oxides showed the presence of micro or nanoparticles of NiFe2O4 inverse spinel,but Fe2O3 （hematite） was also present when ammonia was used for coprecipitation.The reducibility by hydrogen was studied by temperature-programmed reduction （TPR） and in situ XRD,which showed the influence of the preparation method.The surface area （BET）,particle size （Rietveld refinement）,as well as surface Ni/Fe atomic ratio （XPS） and the behavior upon reduction varied according to the synthesis method.The catalytic reactivity was investigated using isopropanol decomposition to determine the acid/base properties.The catalytic performance of methane reforming with CO2 was measured with and without the pre-treatment of catalysts under H2 in 650-800 C range.The catalytic conversions of methane and CO2 were quite low but they increased when the catalysts were pre-reduced.A significant contribution of reverse water gas shift reaction accounted for the low values of H2 /CO ratio.No coking was observed as shown by the reoxidation step performed after the catalytic reactions.The possible formation of nickel-iron alloy observed during the study of reducibility by hydrogen was invoked to account for the catalytic behavior.

Microwave assisted synthesis, spectroscopic, thermal, and antifungal studies of some lanthanide(Ⅲ) complexes with a heterocyclic bishydrazone

A bishydrazone formed by the condensation of isatinmonohydrazone and salicylaldehyde reacted with lanthanide（Ⅲ） chloride to form complexes of the type [Ln（HISA）2Cl3], where, Ln=La（Ⅲ）, Ce（Ⅲ）, Pr（Ⅲ）, Nd（Ⅲ）, Sm（Ⅲ）, Eu（Ⅲ）, or Gd（Ⅲ） and HISA= [（2-hydroxybenzaldehyde）-3-isatin]bishydrazone. Both reactions were carried out under microwave conditions. The ligand and the metal complexes were characterized on the basis of elemental analysis, molar conductance, magnetic susceptibility measurements, UV visible, infrared, far infrared, and proton NMR spectral data. The ligand acted as neutral tridentate, coordinating through the carbonyl oxygen, azomethine nitrogen, and phenolic oxygen without deprotonation. The ligand and lanthanum（Ⅲ） complex were subjected to X-ray diffraction studies. The X-ray diffraction pattern of ligand exhibited its crystalline nature and that of the lanthanum（Ⅲ） complex indicated its amorphous character. The thermal decomposition behaviour of the complex, [La（HISA）2Cl3], was examined in the temperature range of 40-800 ℃ using TG, DTG, and DTA. The ligand and the metal complexes were screened for their antifungal activities.

叔丁基过氧化氢催化分解制备丙酮及催化剂失活原因

以催化异丁烷和氧气为原料生成的叔丁基过氧化氢(TBHP)分解来制备丙酮。对制备丙酮的最优反应条件、催化体系、催化剂稳定性、循环利用性以及催化剂失活的原因进行了考察。结果表明,催化剂的酸性对反应的活性有明显的影响,β分子筛具有最优的催化性能(TBHP转化率为100%),且主要产物丙酮的选择性为49%;在28 h的反应周期内,丙酮的选择性明显下降(降低21%),说明催化剂的稳定性较差,但多次(5次)再生活性仍可恢复。通过不同产物预处理催化剂,确定了丙酮的进一步反应是催化剂失活的主要原因;使用无水乙醇稀释TBHP后反应28 h的稳定性明显提高,并且催化剂的反应性能及重复利用性并未受到影响。

3-(1H-四唑)-7-(三氟甲基)-1,2,4-三唑[5,1-c]-1,2,4-三嗪-4-氨基的制备及性能

以5-(三氟甲基)-1,2,4-三唑-3-胺为原料,两步合成了一种含氟稠环含能化合物3-(1H-四唑)-7-(三氟甲基)-1,2,4-三唑[5,1-c]-1,2,4-三嗪-4-氨基(2)。采用X射线单晶体衍射仪确定了目标化合物的晶体结构,通过核磁共振、傅里叶红外光谱、差示扫描量热仪对其进行了结构测试与性能表征,通过EXPLO5预测了爆轰性能,采用BAM标准方法进行了感度测定。结果表明,合成过程高效、无毒、简单,所得目标化合物的晶体2·DMF属于三斜晶系,Pī空间群,晶胞参数a=4.9035(10)Å,b=10.219(2)Å,c=15.194(3)Å,V=720.4(3)Å^(3),α=107.163(6)°,β=92.486(7)°,γ=96.4438(7)°,Z=2;其理论爆速爆压分别为6933 m·s^(-1)和17.1 GPa,撞击感度>40 J,摩擦感度>360 N。

原料组成对多微孔方镁石-镁铁铝复合尖晶石陶瓷显微结构与性能的影响

利用原位分解合成法,以轻烧MgO、Fe2O3和Al(OH)3为原料,成功制备了多微孔方镁石-镁铁铝复合尖晶石陶瓷,并研究原料组成对其显微结构与性能的影响。研究结果表明:当理论镁铁铝复合尖晶石含量为0%(质量分数,下同)时,试样中颈部连接形成较少,耐压强度较低;当理论镁铁铝复合尖晶石含量为4%~16%时,试样中生成的液相量增多,物质运输速率加大,形成的颈部连接较多,耐压强度较高;当理论镁铁铝复合尖晶石含量为24%时,试样中镁铁铝复合尖晶石生成带来的体积膨胀增多,增大颗粒间距,颈部连接的形成减少,试样的耐压强度减小。同时,当理论镁铁铝复合尖晶石含量为12%~16%时,多微孔方镁石-镁铁铝复合尖晶石陶瓷具有较高的显气孔率(22.3%~24.6%)、较低的体积密度(2.75~2.80 g/cm^(3))和较高的耐压强度(100.6~123.1 MPa)。

1,3,5-三(甲硝胺基)-2,4,6-三硝基苯的合成、单晶结构与性能

以1,3,5-三氯-2,4,6-三硝基苯(化合物1,TCTNB)为原料,经甲胺化、硝化反应得到1,3,5-三(甲硝胺基)-2,4,6-三硝基苯(化合物3)。优化合成工艺获得了制备的最佳工艺条件,总产率达74.7%。采用傅里叶红外光谱仪、核磁共振仪、差示扫描量热仪、热重分析仪和X射线单晶衍射仪等对化合物3及其中间产物进行了表征。单晶数据显示,化合物3晶体属于三斜晶系,P1空间群。采用Kissinger法、Rogers法和Arrhenius法计算化合物3的表观活化能Ea为157.81 kJ·mol^(-1),指前因子A为12.79×10^(16) min^(-1),分解速率常数k为2.91×10^(-11),热爆炸临界温度Tb为206.52℃。采用Kamlet-Jacobs半经验方程预测化合物3的爆速为7990 m·s^(-1),爆压为26.6 GPa。

Controlled synthesis of cobalt nanocrystals on the carbon spheres for enhancing Fischer–Tropsch synthesis performance

Non-porous carbon sphere was used as support to synthesize supported cobalt Fischer-Tropsch catalysts with high activity and durability. Strong metal-support interaction was avoided and intrinsic activity of pristine cobalt nano-particles was studied. Thermal decomposition synthesis method was applied to obtain cobalt catalysts with high dispersion and narrow particle size distribution. Furthermore the cobalt size can be controlled by the molar ratio of o-dichlorobenzene/benzylamine. Compared with supported cobalt catalysts prepared by incipient wetness impregnation method and ultrasonic impregnation method,the catalyst prepared by thermal decomposition method showed higher catalytic activity, higher long chain hydrocarbons selectivity and lower methane selectivity.

Feature Abstracting and Identification of Acoustic Target in the Battle Field Based on EMD

The method of empirical mode decomposition(EMD) was used for the signal processing and featureing of acoustic target of battle field. According to the signal's characteristics of different targets, some feature vectors in token of the target properties were constructed and abstracted. In the basis of feature abstracting and statistic analysis for large amount of sample signal of the targets, using the maximum subjection classification method based on the fuzzy synthesis judgment, the three typical acoustic target helicopter, tank and traffic vehicle were recognized.

基于模态综合法和模态叠加法的密集模态结构响应重构

提出一种基于模态综合法和模态叠加法的密集模态结构响应重构方法,通过两次坐标变换将全结构缩聚为自由度更少的超单元模型,将超单元模型的模态分为密集模态和剩余模态。通过经验模态分解法分离出已知响应中单阶的剩余模态响应,进而重构出待测位置的剩余模态响应,待测位置的密集模态响应可由模态振型和剩余模态计算得到,通过模态叠加法实现在密集模态下的时域响应重构。进行了数值模拟研究,将待测位置响应的理论值与重构值进行比较以验证该方法的精度和效率,此外还详细研究了主模态数量、子结构划分方式、测量噪声和阻尼对重构结果的影响。结果表明:该文方法通过模型缩聚大大减少了重构的数据量,并且改善了传统EMD方法不能分离频率间隔较小的模态而无法实现响应重构这一不足,无论密集模态存在与否都可适用于结构的应力、应变、位移、加速度等多种动力响应的重构。

A SUBARRAY-SYNTHESIS BASED 2D DOA ESTIMATION METHOD

In some satellite communications, we need to perform Direction Of Arrival (DOA) angle estima- tion under the restriction that the number of receivers is less than that of the array elements in an array antenna. To solve the conundrum, a method named subarray-synthesis-based Two-Dimensional DOA (2D DOA) angle estimation is proposed. In the method, firstly, the array antenna is divided into a series of subarray antennas based on the total number of receivers; secondly, the subarray antennas’ output covariance matrices are esti- mated; thirdly, an equivalent covariance matrix is synthesized based on the subarray output covariance matri- ces; then 2D DOA estimation is performed. Monte Carlo simulations showed that the estimation method is ef- fective.