5,9,14,18,23,27,32,36-八烷氧基2,3-萘酞菁镍(Ⅱ)的结构与光谱性质关系的研究

测定了一组八烷氧基萘酞菁镍（Ⅱ）配合物Ni（Ⅱ）（RO）8NPC（R＝C4H9，C8H17，C12H25，NPC＝C48H16N8）在5种有机溶剂（Py、DMSO、DMF、CH2Cl2、C6H12）中的电子吸收光谱和荧光光谱，研究了这些配合物的结构与光谱的关系。结果表明该系列RO取代萘酞菁镍（Ⅱ）配合物的Q带吸收光谱比无取代的红移75nm左右，荧光光谱屯相应红移50～80nm，而溶剂对其影响不大。     

CC14法合成α—羟基—α—甲基苯丙酮的研究

α 羟基 α 甲基苯丙酮 (ＰＨＭＰ)是一种性能优良的新型光引发剂 ,具有引发效率高、热稳定性好、耐黄变、无异味等优点[1,2 ] 。现有合成方法步骤多 ,产率低 ,后处理麻烦 ,操作复杂[3,4] ,且在反应过程中会产生ＨＣ1或ＨＢｒ等有毒副产物。本文研究了在相转移催化剂的作用下[5,6 ] ,ＣＣｌ4直接氯化水解生成α 羟基 α 甲基苯丙酮的新方法。该方法不仅减少了反应步骤 ,简化了操作 ,而且提高了产品质量。1　实验部分1 .1　仪器与试剂傅立叶红外光谱仪Ｐｅｒｋｉｎ Ｅｌｍｅｒ 1 71 0 ,ＷＸＳ 1型阿贝折光仪。异丁酸 ,ＳＯＣｌ2 ,苯 ,四氯化…     

沉淀法合成纳米晶长余辉材料Y2O2S∶Eu3+，Ti

The long-lasting phosphorescent materials, yttrium oxysulfides doped by Eu and Ti, were systhesized by coprecipitation with their subsequent thermal decomposition in the presence of sulphur. The products were characterized by XRD, TEM, phosphorescent spectra, and thermoluminescence. The XRD results indicate that the lowest synthesis temperature is 700 ℃. From the TEM, the average diameter of particles was in the range of 60～120 nm, and augmented with the increase of temperature. The materials under UV excitation presented well afterglow from the transition of ⁵D_0,1 → ⁷F_J of Eu³⁺, and the persistent time was about 2 h. The long-lasting afterglow mechanism was discussed, too.     

复合Fe2O3纳米粒子的高分子微球的结构表征

近年来，复合有机、无机粒子的高分子微球及其特殊性质越来越引起人们的兴趣与关注［1］．获得有机、无机复合微球的方法很多，如在无机粒子存在下的乳液或无皂乳液聚会[2，3]，通过可聚合的表面活性剂在粒子表面形成胶囊化层[4]以及共沉淀法等[5]．这些无机粒子包括氧化钛、氧化铁、氧化铝及氧化硅等．Haga等[6]增发现包覆在聚合物粒子中的CdS与其本体的光电性质不同；单分散的聚合物微球可以在基片上被组装成二维乃至三维有序的结构[7]．这为信息存储、立体印刷等领域提供了新途径．因此，将无机粒子与聚合物复合成为功能化粒子是一项有…     

Determination of Gossypol in Trace Level by Flow Injection Analysis with Chemiluminescence Detection

Gossypol, [1, 1′, 6, 6′, 7,7′-hexahydroxyl-5,5′-diisopropyl-3,3′-dimethyl-(2,2′-binaphtha- lene)-8,8′-dicarboxaldehyde] is a polyphenolic yellow compound naturally occurring in various parts of cotton plants1. The compound has been associated with     

含柔性间隔基的热致液晶性共聚酯的合成

 将己二酸、辛二酸、癸二酸、1,10-十二烷基羧酸经酰氯化后,分别与对羟基苯甲酸合成,得到了四种二元羧酸以及与其相应的四种二元酰氯,并发现前者具有热致液晶性。 将上述单体与对苯二酚、氯代对苯二酚以及联苯二酚用溶液缩聚的方法合成了十二种规则共聚酯,并用热台偏光显微镜、DSC、X-衍射等方法对共聚酯进行了表征。结果发现各共聚酯均为向列型热致液晶,并都具有较宽的液晶态温度范围。通过改变分子结构可使共聚酯的熔点在150—300℃之间变化。     

手性奎宁-卟啉锰催化剂的合成及其催化性能

为了寻找催化活性、相转移活性和手性诱导为一体的卟啉配体[1-4],我们把卟啉和手性相转移源连结起来,用奎宁-卟啉化合物作配体[5],考察其锰 配合物为催化剂对烯烃环氧化反应的催化性能。奎宁-卟啉锰 配合物结构式如下:1　实验部分1.1　试剂和仪器苯乙烯和α-甲基苯乙烯在氮气保护下减压蒸馏处理。氧源ＮａＯＣｌ的浓度由碘量法测定。其余试剂均为化学纯,色谱标样环氧苯乙烯和α-甲基环氧苯乙烯按文献[6]方法合成。奎宁-卟啉配体按文献[5]合成。260-50型红外光谱仪,ＫＢｒ压片;ＵＶ-3000型紫外可见光谱仪,溶剂ＤＭＦ;ＭＴ-3型ＣＨＮ元素…     

SYNTHESIS, STRUCTURE AND ELECTROCHEMICAL STUDIES ON SINGLE MoFe_3S_4 AND WFe_3S_4 CUBANE-TYPE CLUSTER COMPOUNDS*

Single cubane-like clusters, MFe_3S_4(R_2dtc)_5 (M=Mo, R_2=—(CH_2)_4—, Bz_2; M=W, R_2=Me_2, —(CH_2)4—; dtc=dialkyldithiocarbamate) were synthesized by assembly reaction of (NH_4)_2MS_4 (M=Mo, W), FeCl_2 with R_2dtcNa (or NH_4) in DMF. The structure, IR, EPR and cyclic voltammogram are described and discussed. MoFe_3S_4(C_4H_8dtc)_5 was also obtained from the conversion of linear cluster Fe(DMF)_6[(FeCl_2)_2MoS_4] in the presence of C_4H_8dtc NH_4. Both clusters MoFe_3S_4(C_4H_8dtc)_4·2C_2H_5CN and WFe_3S_4(C_4H_8dtc)_5·2DMF crystallize in the monoclinic space group C2/c with a=12.544(2), (Mo-cluster), 12.533(4) (W-cluster); b=20.478(4), 20.121(6); c=19.582(7), 19.659(2);β=102.82(2), 102.96(3)°; and Z=4, 4. Their structures were refined to R=0.057 and 0.064 with use of 2690 and 2179 reflections (ι>3Q(I)), respectively. Many similarities in structure for Mo and W clusters indicate that both Mo and W play a very similar role in the clusters.     

α－芳甲酰基烯酮二硫缩醛的新合成方法

以碳酸钾为碱，芳甲酰丙酮（１）与二硫化碳、卤代烃反应得到２－乙酰基－２－芳甲酰基烯酮硫代缩醛（２），２在乙硫醇钾作用下脱乙酰基生成标题化合物（３）。１→３的转化具有反应条件温和、产物产率高及对３中各种缩醛基均可通用等特点。     

STUDIES OF ELECTRON SPIN RESONANCE ON BILIRUBIN FREE RADICALS

The nature of ESR signals derived from bilirubin-Ⅸα has been studied by focusing onthe samples treated with free radical generating and inhibiting systems, i.e. X-XOD, Fe/EDTA, SOD, mannitol/ascorbate, CO, KCN, etc. In all the cases, the stable signals comprisethose originated from semiquinone radical (g = 2.0012) and superoxide free radical (g_∥=2.041, g_⊥= 2.0040). The superoxide is shown binding with certain metal ions chelated bybilirubin. The free radical scavengers are able to destroy these radicals. The kinetic curveof the regeneration of bilirubin radicals has been determined and the reaction follows azero order mechanism. It is likely that both the physiological and toxic actions of bilirubinare related to the characters of its free radicals. Bilirubin is discussed as "active oxygensink" in mammalians.