稀土配合物[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3的标准生成焓及热分解动力学研究

合成了高氯酸镨和咪唑(C₃H₄N₂), DL-α-丙氨酸(C₃H₇NO₂)混配配合物晶体. 经傅立叶变换红外光谱、化学分析和元素分析确定其组成为[Pr(C₃H₇NO₂)₂(C₃H₄N₂)(H₂O)](ClO₄)₃. 使用具有恒温环境的溶解-反应量热计, 以2.0 mol•L^－1 HCl为量热溶剂, 在T＝(298.150±0.001) K时测定出化学反应PrCl₃•6H₂O(s)＋2C₃H₇NO₂(s)＋C₃H₄N₂(s)＋3NaClO₄(s)＝[Pr(C₃H₇NO₂)₂(C₃H₄N₂)(H₂O)](ClO₄)₃(s)＋3NaCl(s)＋5H₂O(1)的标准摩尔反应焓为Δ_rH_m^ө＝(39.26±0.11) kJ•mol^－1. 根据盖斯定律, 计算出配合物的标准摩尔生成焓为Δ_fH_m^ө{[Pr(C₃H₇NO₂)₂(C₃H₄N₂)(H₂O)](ClO₄)₃(s), 298.150 K}＝(－2424.2±3.3) kJ•mol^－1. 采用TG-DTG技术研究了配合物在流动高纯氮气(99.99%)气氛中的非等温热分解动力学, 运用微分法(Achar-Brindley-sharp和Kissinger法)和积分法(Satava-Sestak和Coats-Redfern法)对非等温动力学数据进行分析, 求得分解反应的表观活化能E＝108.9 kJ•mol^－1, 动力学方程式为dα/dt＝2(5.90×10⁸/3)(1－α)[－ln(1－α)]^－1exp(－108.9×10³/RT).     

三种负反馈放大电路仿真软件的比较

介绍了目前比较流行的Multisim、Protel和Pspice三种电路仿真软件的特点;给出了仿真电路图;分析了三种仿真软件在负反馈放大电路的支流分析、参数扫描分析、傅里叶分析及温度扫描分析中的作用和特点。     

对甲苯磺酸/SiO2催化合成乙酸正丁酯的研究

用对甲苯磺酸／SiO2催化乙酸与正丁醇酯化反应合成了乙酸正丁酯，对反应条件进行了研究，实验结果表明对甲苯磺酸／SiO2催化剂对乙酸和正丁醇的酯化反应有良好的催化活性，反应的最佳条件为：乙酸与正丁醇的摩尔比为1.0:2.0，催化剂的用量的反应物料总质量的2.5%，带水剂环乙烷为10ml，反应时间为2.0h，此时的酯化率可达98.1%，而在同样的条件下，不加催化剂时的酯化率仅为23.7%。     

颤振的增益调度控制实验研究

本文对机翼外挂系统颤振的半主动抑制实验进行了研究分析,在引入电磁阻尼器对风振控制的同时,根据增益调度控制原理设计并制造了控制系统,在风洞实验中实现了电磁阻尼器对系统的颤振半主动抑制,为颤振抑制的实现又提供了一种实验的方法。     

Synthesis and Crystal Structure of 1,2-Dis（1,3-diphenylpropan-2-yl）disulfane

A novel compound of 1,2-dis(1,3-diphenylpropan-2-yl)disulfane(C30H30S2,Mr=454.27)was synthesized in ethanol with 1,3-diphenyl-2-propanone as raw materials,giving high yield of product(90%).Its structure was determined by IR,1H NMR,MS,elemental analysis and X-ray diffraction.The crystal belongs to monoclinic,space group C2 with a=18.727(3),b=6.5179(9),c=13.7576(18),β=131.0610(10)o,V=1266.2(3)3,Z=2,Dc=2.136 g/cm3,μ=1.078 mm-1,F(000)=843,R=0.0490 and wR=0.1247 for 3211 observed reflections with I>2(I).X-ray analysis reveals that the molecule is not symmetrical.There exist no classical hydrogen bonds andπ-πstacking interactions.Moreover,the thermal stability of compound 3 was investigated.     

微波辐射硝基芴与丙烯酸酯Michael加成产物的合成与结构

以硝基芴和丙烯酸脂为原料,在碱性条件下,微波辐射(500 W)反应4～5 min,非常方便地合成了系列未见文献报道的Michael加成产物,该方法操作简单、产率较高(79%～87%)。其结构经IR、1H NMR、MS和元素分析进行表征,并利用X射线单晶衍射分析法测定了化合物3b的单晶结构。     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

Pdl吸附树脂催化氢化马来酸及其表观动力学

琥珀酸主要用于食品行业,此外在医药上用作抗痉挛剂,祛痰剂和利尿剂,也可用于制备增塑剂、染料、香料、摄影制剂等。通常以马来酸电解还原加氢制备,通过液相催化加氢法的制备也有所报道。鉴于高分子催化剂在有机合成中的广泛应用性及其独特高分子效应,我们采用了吸附树脂负载的金属钯催化剂,获得了比较满意的结果,反应的转化率与选择性都较高,具有一定的实用价值。     

二苄基二硫醇的合成研究

以二苄基甲酮为原料,无水乙醇为溶剂,连续通入干燥的H2S和HC l气体,在温度为0~5℃之间反应6h,最终得到产物,产率为85%,通过IR1、H NMR和MS分析证明该化合物为二苄基二硫醇.