纳米金属钴粒子的制备及对高氯酸铵热分解的影响

The monodispersed Co nanoparticles were successfully prepared by means of hydrogen plasma method in inert atmosphere. The particle size, specific surface area, crystal structure and morphology of the samples were characterized by transmission electron microscopy （TEM）, BET equation, X-ray diffraction （XRD）, and the corresponding selected area electron diffraction （SAED）. The catalytic effect of Co nanoparticles on the decomposition of ammonium perchlorate （AP） was investigated by differential thermal analyzer （DTA）. Compared with the thermal decomposition of pure AP, the addition of Co nanoparticles （2%-10%, by mass） decreases the decomposition temperature of AP by 145.01-155.72℃. Compared with Co3O4 nano-particles and microsized Co particles, the catalytic effect of Co nanoparticles for AP is stronger. Such effect is attributed to the large specific surface area and its interaction of Co with decomposition intermediate gases. The present work provides useful information for the application of Co nanoparficles in the AP-based propellant.     

纳米级金属和金属复合物粉末对高氯酸铵和高氯酸铵/聚合丁二烯复合固体推进剂热分解特性的影响

Effects of metal (Ni, Cu, Al) and composite metal (NiB, NiCu, NiCuB) nanopowders on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellant ammonium perchlorate/hydroxyterminated polybutadiene (AP/HTPB) were studied by thermal analysis (DTA). The results show that metal and composite metal nanopowders all have good catalytic effects on the thermal decomposition of AP and AP/HTPB composite solid propellant. The effects of metal nanopowders on the thermal decomposition of AP are less than those of the composite metal nanopowders. The effects of metal and composite metal nanopowders on the thermal decomposition of AP are different from those on the thermal decomposition of the AP/HTPB composite solid propellant.     

制备方法对BaNi0.2Mn0.8Al11O19－δ催化燃烧二甲醚的催化活性的影响

Catalytic combustion of dimethyl ether （DME） over hexaaluminate catalyst BaNi0.2Mn0.8Al11O19-δ has been investigated. The catalysts were prepared with the sol-gel method and reverse microemulsion method respectively and characterized by thermogravimetry-differential thermal analysis, X-ray diffraction and transimission electron microscope. It was found that the formation of Mn, Ni modified hexaaluminate was a relatively slow process via two solid state reactions and spinel structure was a transition phase. At the same calcined temperature and time, the catalyst prepared with the reverse microemulsion method could form the hexaaluminate phase more easily than that prepared with the sol-gel method. The catalyst BaNi0.2Mn0.8Al11O19-δ prepared with the reverse micro-emulsion method appeared a plate-like morphology, while it appeared a needle-like morphology when using the sol-gel method. The catalytic activities of catalysts BaNi0.2Mn0.8Al11O19-δ prepared with two different methods for DME combustion were tested. It showed that catalyst prepared with the reverse microemulsion method had better catalytic activity, i.e. T10% of DME had decreased by 45℃, about 90% conversion of diemthyl ether at 380℃.     

La_(0.8)Sr_(0.2)MnO_3的燃烧法制备及对HMX热分解的影响(英文)

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&;#61485; and adsorbed oxygen (Oad) could result in an advance in the onset temperature of HMX thermal decompo-sition. The mixture system of Mn3+ and Mn4+ 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 decom-position 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.     

Pt对NiB非晶态合金催化剂对苯加氢性能的影响

A support (denoted AM) was prepared using pseudo-boehmite and mordenite. Ni-B and NiPtB amorphous catalysts were prepared on the support by the impregnation method followed by chemical reduction with a KBH4 solution. And the catalysts were characterized by X-ray diffraction (XRD), environment scanning electron microscope (ESEM), inductively coupled plasma (ICP), H2-temperature programmed reduction (H2-TPR), differential thermal analysis (DTA), and BET. Benzene hydrogenation was used as a probe reaction to evaluate the effect of addition of small quantities of Pt on the NiB/AM catalyst. The results show that Pt can promote the reduction of NiO and the formation of active sites, leading to smaller catalyst particles and better dispersion of active metal particles on the support. The catalytic activity, sulfur resistance and thermal stability were remarkably improved by Pt doping of the NiB/AM catalyst.     

离子液体修饰超顺磁性纳米颗粒用于青霉素G酰化酶固定化(英文)

Functionalized ionic liquids containing ethyoxyl groups were synthesized and immobilized on magnetic silica nanoparticles(MSNP) prepared by two steps,i.e.,Fe3O4 synthesis and silica shell growth on the surface.This magnetic nanoparticle supported ionic liquid(MNP-IL) were applied in the immobilization of penicillin G acylase(PGA).The MSNPs and MNP-ILs were characterized by the means of Fourier transform infrared spectroscopy(FTIR),scanning electron microscopy(SEM),transmission electron microscopy(TEM),and vibrating sample magnetometer(VSM).The results showed that the average size of magnetic Fe3O4 nanoparticles and MSNPs were ~10 and ~90 nm,respectively.The saturation magnetizations of magnetic Fe3O4 nanoparticles and MNP-ILs were 63.7 and 26.9 A?m2?kg?1,respectively.The MNP-IL was successfully applied in the immobilization of PGA.The maximum amount of loaded enzyme was about 209 mg?g?1(based on carrier),and the highest enzyme activity of immobilized PGA(based on ImPGA) was 261 U?g?1.Both the amount of loaded enzyme and the activity of ImPGA are at the same level of or higher than that in previous reports.After 10 consecutive operations,ImPGA still main-tained 62% of its initial activity,indicating the good recovery property of ImPGA activity.The ionic liquid modified magnetic particles integrate the magnetic properties of Fe3O4 and the structure-tunable properties of ionic liquids,and have extensive potential uses in protein immobilization and magnetic bioseparation.This work may open up a novel strategy to immobilize proteins by ionic liquids.     

Investigation on specific heat capacity and thermal behavior of sodium hydroxyethyl sulfonate

The thermal decomposition process was studied by the TG–DTA analyzer. The results show that the decomposition process of sodium hydroxyethyl sulfonate consisted of three stages: the mass loss for the first, the second and third stages may be about the groups of CH_3CH_2OH, CH_3CHO and SO_2 volatilized, respectively. The decomposition residuum of three stages was analyzed by FT-IR, and the results of FT-IR agreed with the decomposition process predicted by theoretical weight loss. The specific heat capacity of sodium hydroxyethyl sulfonate was determined by differential scanning calorimetry(DSC). The melting temperature and melting enthalpy were obtained to be 465.41 K and 25.69 kJ·mol~(-1), respectively. The molar specific heat capacity of sodium hydroxyethyl sulfonate was determinated from 310.15 K to 365.15 K and expressed as a function of temperature.     

An efficient green route for hexamethylene-1,6-diisocyanate synthesis by thermal decomposition of hexamethylene-1,6-dicarbamate over Co3O4/ZSM-5 catalyst:An indirect utilization of CO2

The utilization of CO2 as rawmaterial for chemical synthesis has the potential for substantial economic and green benefits. Thermal decomposition of hexamethylene-1,6-dicarbamate (HDC) is a promising approach for indirect utilization of CO2 to produce hexamethylene-1,6-diisocyanate (HDI). In this work, a green route was developed for the synthesis of HDI by thermal decomposition of HDC over Co3O4/ZSM-5 catalyst, using chlorobenzene as lowboiling point solvent. Different metal oxide supported catalysts were prepared by incipientwetness impregnation (IWI), PEG-additive (PEG) and deposition precipitation with ammonia evaporation (DP) methods. Their catalytic performances for the thermal decomposition of HDC were tested. The catalyst screening results showed that Co3O4/ZSM-525 catalysts prepared by different methods showed different performances in the order of Co3O4/ZSM-525(PEG) N Co3O4/ZSM-525(IWI) N Co3O4/ZSM-525(DP). The physicochemical properties of Co3O4/ZSM- 525 catalyst were characterized by XRD, FTIR, N2 adsorption-desorption measurements, NH3-TPD and XPS. The superior catalytic performance of Co3O4/ZSM-525(PEG) catalyst was attributed to its relative surface content of Co3+, surface lattice oxygen content and total acidity. Under the optimized reaction conditions: 6.5% HDC concentration in chlorobenzene, 1 wt% Co3O4/ZSM-525(PEG) catalyst, 250 °C temperature, 2.5 h time, 800 ml·min?1 nitrogen flow rate and 1.0 MPa pressure, the HDC conversion and HDI yield could reach 100% and 92.8% respectively. The Co3O4/ZSM-525(PEG) catalyst could be facilely separated from the reaction mixture, and reused without degradation in catalytic performance. Furthermore, a possible reaction mechanism was proposed based on the physicochemical properties of the Co3O4/ZSM-525 catalysts.     

采用纳米Al203和碳纳米管颗粒强化CO2吸收的理论及实验研究（英文）

The influence of nano-particles on CO2 absorption was studied experimentally in a stirred thermostatic reactor. Nano-A1203 and carbon nanotube （CNT） particles which showed different hydrophobic properties were chosen for the investigation. The experimental results were compared with that of micron-size activated carbon （AC） and Al2O3 particles. From the results, no enhancement by micron-size A1203 was found, and with the increase of A1203 concentration, the enhancement factor decreased. However, nano-Al203 showed a weak enlaancement tor me COz absorption. AC and CNT particles all intensified the gas-liquid mass transfer effectively, yet the trend of the enhancement factor with stirring speed for the two particles was different. With increasing stirring speed, the enhancement factor of AC particles was decreased, wl＇iereas in CNT suspensions it was increased. The experimental phenomena demonstrated a difference in enhancement mechanism for different size particles. For nano-particles, besides the influence of adsorbability and hydrophobicity, the micro-convection caused by Brownian motion should be also taken into account. Considering the micro-convection effect, a theoretical model was developed to shed light on the absorption enhancement bv nano-oarticles.     

Synthesis of sub-micrometer lithium iron phosphate particles for lithium ion battery by using supercritical hydrothermal method简

A supercritical hydrothermal method was employed to prepare sub-micrometer LiFePO4 particles with high purity and crystallinity. The structure and morphology of LiFePO4 particles were characterized by X-ray diffraction and scanning electron microscope. The electrochemical tests were carried out to determine the reversible capacity, rate and cycling performance of the LiFePO4 particles as cathode material for lithium ion battery. Experimental results show that solvent and calcining time have significant effects on purity, size and morphology of LiFePO4 particles. Mixed solvent contained deionized water and ethanol is conducive to synthesize smaller and more uniform particles. The size of LiFePO4 particles as-prepared is about 100-300 nm. The specific discharge capacities of the LiFePO4 particles are 151.3 and 128.0 mA. h. g-1 after first cycle at the rates of 0.1 and 1.0 C, respectively. It retains 95.0% of the initial capacity after 100 cycles at 1.0 C.     

基于C_8H_(15)N_2Br为结构导向剂合成磷酸铝分子筛材料

以异丙醇铝作为铝源、磷酸作为磷源、吗啉为助剂和1-丁基-3-甲基咪唑溴盐(C_8H_(15)N_2Br)为结构导向剂,采用离子热法合成开放骨架的磷酸铝分子筛,系统考察了P_2O_5/Al_2O_3摩尔比、HF/Al_2O_3摩尔比、吗啉/Al_2O_3摩尔比和C_8H_(15)N_2Br/Al_2O_3摩尔比对磷酸铝分子筛合成的影响,通过X射线衍射(XRD)、扫描电镜(SEM)和TG-DTA等检测方法对所合成的产物的结构、形貌进行了表征。XRD分析结果表明:开放骨架磷酸铝材料合成的最佳条件为Al_2O_3∶P_2O_5∶HF∶C_4H_9NO∶C_8H_(15)N_2Br=1.0∶2.0∶(1.0-2.0)∶4.0∶4.0,SEM分析结果表明所合成的磷酸铝材料为具有规则的长方体晶体形貌。     

CL-20初始热分解反应机理的分子动力学计算

基于Reaxff反应力场,采用NPT、NVT系综和Berendsen方法,通过分子动力学计算研究了不同密度和温度下CL-20单分子和超晶胞的初始热解路径。结果表明,CL-20分子中的两种N-NO2键能生成NO2·自由基。单分子CL-20初始热分解中,两种不同类型的N-NO2化学键均能发生断裂生成NO2·自由基和R-(NO2n)(n≤5)碎片,NO2·自由基形成N2O4,N2O4分解为NO、NO3等碎片或重新生成两个NO2·自由基,NO2·自由基与其他中间体发生反应生成N2、HNO3等碎片。CL-20超晶胞的热解初始反应路径与单分子的初始热解反应路径相同,但由于非键相互作用,使得生成NO2·自由基的总量减少。超晶胞CL-20发生热解反应生成的HNO3碎片会继续分解成H2O和N2O5等碎片。     

前驱体对熔盐法合成Bi2WO6光催化剂及其性能的影响

分别以Bi(NO3)3和Na2WO4溶液直接混合所得沉淀、加氨水所得沉淀及Bi(NO3)3×5H2O+Na2WO4×2H2O为前驱体,采用熔盐法合成Bi2WO6光催化剂粉体,研究了不同前驱体所制粉体的物相、形貌,以其为催化剂,在可见光照射下降解罗丹明B溶液. 结果表明,用后二者为前驱体均可得到薄片状纯相Bi2WO6粉体. 加氨水所得沉淀为前驱体所制Bi2WO6粉体的光催化性能最好,在可见光照射下对0.01 mmol/L RhB溶液的降解率在60 min内达99%.     

超细CuCr_2O_4粉体的制备及表征

以Cu(NO32)·3H2O、Cr(NO3)2·9H2O和柠檬酸为原料,采用柠檬酸配位法合成了超细CuCr2O4催化剂,用XRD、SEM对产物进行了表征,用DTA研究了CuCr2O4对高氯酸铵(AP)热分解性能的影响,测量了加入CuCr2O4后CMDB推进剂的燃速。结果表明,在最佳合成条件下(即nCu∶nCr=1∶2,温度700℃)可制得纯四方尖晶石型CuCr2O4。加入超细CuCr2O4后,AP的高温分解温度提前至339.6℃,CMDB推进剂在6MPa下的燃速从35.84mm/s提高到61.00mm/s,压强指数从0.62降低到0.14。     

溶胶–凝胶法制备碳纳米管-In_2O_3纳米复合材料及其气敏性

以碳纳米管（carbon nanotubes,CNT）为模板,在超声波辅助条件下,利用溶胶–凝胶法合成CNT–In2O3纳米复合粉体,用该复合粉体制备CNT–In2O3气敏元件。借助X射线衍射、透射电子显微镜、傅立叶变换红外光谱仪和能量色散谱仪对产物进行表征,研究了CNT–In2O3气敏元件的气敏性。结果表明：CNT–In2O3纳米复合粉体是一种由In2O3纳米颗粒均匀包裹在直径约为20～30nm的碳纳米管上的纳米复合材料。CNT–In2O3气敏元件在低温对NO2有较高的灵敏度,该元件对NO2的灵敏度高于纯In2O。当CNT和InC13·4H2O的摩尔比为3：10时,CNT–In2O3气敏元件对NO2的灵敏度最大,且灵敏度随NO2浓度的增大而增大。该气敏元件在200℃时对NO2的响应时间为10s,恢复时间为70s。     

水热法制备钴铝尖晶石型纳米晶液体陶瓷颜料

以硝酸钴、硝酸铝和氢氧化钠为主要原料,采用水热法通过一系列正交对比实验制备了较纯净、结晶完整,直径为100nm左右且分散性良好的CoAl2O4纳米晶。用X射线衍射仪(XRD)、透射电子显微镜(TEM)及X射线能量色散谱仪(EDS)测定了粉体的晶相组成、微观形貌和元素组成。实验结果表明:水热法制备CoAl2O4纳米晶的最佳工艺条件为水热温度T=200℃、水热时间t=16h、前驱液摩尔浓度C=0.25mol·L-1、pH值=11、Al3+:Co2+=4:1(摩尔比)。球形的CoAl2O4粉体是单晶且沿[311]方向取向生长。     

燃烧法制备纳米铁酸镉和铁酸铜及表征

以Fe（NO3）3·9H2O、Cu（NO3）2·3H2O和Cd（NO3）2·4H2O为原料,以柠檬酸为还原剂,采用燃烧法制备了CuFe2O4和CdFe2O4纳米粉体,用X-射线粉末衍射仪（XRD）、红外光谱（IR）和振动样品磁强计（VSM）等手段对样品进行了表征,结果表明样品为立方晶系铁酸铜纳米粉体和立方晶系铁酸镉纳米粉体,其平均粒径约为22nm和18nm,并具有超顺磁性。     

均相沉淀法制备掺钕钇铝石榴石纳米粉末的研究

掺钕钇铝石榴石（Nd：YAG）多晶透明陶瓷具有容易制造、成本低、光学性能好、热导率高等优点,是一种很有前途的激光工作物质。以AI（N03）·9H2O,Y2O3,Nd2O3,（NH4）2SO4和尿素为原料,正硅酸乙酯为添加剂,采用均相沉淀法制备出分散均匀、纯YAG立方晶相的Nd：YAG纳米前驱体粉末。采用XRD、FT-IR、TEM等测试手段对前驱体粉末进行表征。研究结果表明：Nd：YAG前驱体粉末在800℃时为无定型态,当温度达到890℃时析出大量的中间相YAlO3（Y=AP）和少量的Y3Al5O5（YAG）,当温度达到1000℃时就全部转化为YAG立方晶相。     

二乙醇胺辅助溶胶-凝胶法低温合成锆钛酸铅纳米粉体

以醋酸铅[Pb（CH3COO）2^-33H20]、硝酸锆[Zr（N03）4^-5H2O]和钛酸四丁酯[Ti（C4H90）4]为原料,以二乙醇胺（diethanolamine,DEA）为聚合剂．用溶胶-凝胶法制备了锆钛酸铅（PbZrxTil-x03,PZT）纳米陶瓷粉体。研究了DEA对溶胶-凝胶法合成PZT陶瓷粉体的影响...     

超级铝热剂Al/Fe_2O_3对硝化棉热分解特性的影响

采用水热法制备了纳米Fe_2O_3,并用超声分散法将其与纳米Al颗粒复合制备了超级铝热剂Al/Fe_2O_3,利用X-射线粉末衍射(XRD)、透射电子显微镜(TEM)、扫描电镜及能量散射光谱仪(SEM-EDS)对复合物的物相、组成、形貌和结构进行了分析表征,采用差示扫描量热法(DSC)和热红联用技术(TG-FTIR)研究了Al/Fe_2O_3对硝化棉(NC)热分解过程的影响。结果表明,Al/Fe_2O_3-NC和NC的热分解过程遵循Avrami-Erofeev方程f(α)=1.5(1-α)[-ln(1-α)]1/3;超级铝热剂Al/Fe_2O_3可降低硝化棉的表观活化能、临界点火温度和临界爆炸温度,在促进硝化棉O-NO_2键断裂和凝聚相二次自催化反应中起到至关重要的作用。