聚合物分散液晶单体4,4′-二[6-(丙烯酰氧基)己氧基]联苯的合成

利用丙烯酰氯代替丙烯酸钾与4,4′-二(6-溴己氧基)联苯反应改进了制备4,4′-二[6-(丙烯酰氧基)己氧基]联苯(BAB6)的合成路线。改进前的反应温度较高,中间产物溶解度小,产物呈淡黄色,收率仅12.4%;改进后在室温反应,中间产物溶解度较高,产物呈白色,收率达到46.8%。采用1HNMR、13CNMR和元素分析对中间体和BAB6结构进行了表征。由改进后合成的单体,制备了具有快速响应的聚合物分散液晶(PDLC)膜,响应时间约2ms。扫描电子显微镜观察的结果表明,PDLC中形成了聚合物网络结构。     

室温固相研磨制备椭球形活性碳酸钙

以Span60为添加剂,利用Ca(Ac)2.H2O与Na2CO3在室温下进行固相研磨反应合成椭球形活性碳酸钙,考察了Span60用量对样品活性、分散性的影响。用X射线衍射仪(XRD)分析、扫描电子显微镜(SEM)、傅立叶变换红外吸收光谱(FTIR)、粒度分析等手段对所得样品进行了表征,探讨了椭球形碳酸钙的形成机理。结果表明,Span60对碳酸钙粒子的结构和形貌具有调控作用,微米级椭球形碳酸钙是由纳米级小颗粒组装而成。在Span60的用量4%的条件下,可制得活性高、分散性好、粒度为1~3μm的椭球形碳酸钙。     

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).     

甜、酸杨桃叶中微量元素含量的测定

用浓硝酸-高氯酸的混合溶液对酸、甜杨桃叶样品进行消化.采用空气-乙炔火焰原子吸收光谱法测定样品中ca、Cu、Mn、Fe、Pb、Mg 6种微量元素的含量.该方法简便.准确.精密度高.相对标准偏差(RSD)≤1.28%.结果可靠.     

Cu(SCN)2-水系电沉积制备CuSCN薄膜

Cu(SCN)2-水系电沉积制备CuSCN薄膜;p-CuSCN薄膜;电化学沉积;EDTA     

基于移动中和界面电泳酸碱滴定的新原理及装置

基于移动中和界面(MNB)概念,研制了一种基于电泳酸碱滴定(EABT)的新装置.其核心技术是在电泳管中建立MNB,通过对电泳管中的MNB在一定时间内迁移距离的测定,推测酸或碱的浓度.EABT实验表明:HCl浓度的对数值与MNB移动距离存在线性关系.此关系可用于检测未知酸的浓度；不同酸碱指示剂对EABT方法没有明显影响,这能有效避免在容量分析法中不同指示剂对判定终点断滴所造成的误差；EABT具有良好的精密性和稳定性,日内差和日间差的RSD值分别小于1.6％和3.8％.     

弹体材料性能对破片形成的影响

为了获得弹体材料性能对破片形成的影响规律,应用破片战斗部设计软件,数值计算了82钢、50SiMnVB钢、40CrMnSiB钢及30CrMnSiNi2A钢等4种材料形成破片的情况,得到了4种材料形成的破片的飞散角、初速及质量分布的变化规律,并进行了破片质量分布的实验研究。结果表明,不同合金钢材料对形成的破片飞散角与初速的影响不大,且沿弹体轴向方向的变化规律相同,其中破片飞散角沿弹轴方向先减小后增大,破片的最大初速出现在距起爆点约72.5%圆筒长度处;但是对破片质量分布情况的影响较大,随着材料极限抗拉强度的增加和断裂韧性的降低,弹体破碎程度升高,总破片数增加了39.3%。     

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.     

Expression and Displaying of β-Glucosidase from Streptomyces Coelicolor A3 in Escherichia coli

Two genes encoding β-glucosidase from Streptomyces coelicolor A3(2) were cloned and expressed in Escherichia coli BL21 (DE3). Two recombinant enzymes (SC1059 and SC7558) were purified and characterized. The molecular mass of the purified SC1059 and SC7558 as determined by SDS-PAGE agrees with the calculated values (51.0 and 52.2 kDa, respectively). Optimal temperature and pH for the two enzymes were both at 35 °C and 6.0. SC7558 exhibited to be much more active than SC1059 under optimal conditions, and it was recombined with ice nucleation protein which could anchor on the surface of the cell. The optimal temperature and pH of the recombinant cells were 55 °C and 8.0, respectively. The resultant cells were to be used as material for immobilized β-glucosidase, which is convenient to catalyze substrates in various complicated conditions.     

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.