F-T合成Fe/Cu/K/Al2O3催化剂的结构性质、还原及碳化行为

采用连续共沉淀与喷雾干燥成型技术相结合的方法制备了微球状Fe/Cu/K/Al2O3催化剂, 结合TG、N2物理吸附、XRD、H2-TPR、CO-TPR、Mossbauer谱等表征手段, 研究焙烧温度对Fischer-Tropshc (F-T)合成铁基催化剂的结构性质、还原行为和碳化行为的影响. 结果表明, 较高的焙烧温度有利于碳酸盐的分解和结晶水的脱除, 促进了催化剂的还原. 随着焙烧温度的进一步升高, 催化剂的比表面积减小, 平均孔径增大, α-Fe2O3晶粒的粒径增大, 催化剂中金属与载体的相互作用增强, 从而削弱了CuO、K2O助剂的作用, 严重抑制了催化剂的还原和碳化.     

硫杂杯-1,3-2,4-氮杂双冠醚的合成与氨基酸配合性能

对叔丁基硫杂杯四酰肼衍生物(2)与邻苯二甲醛发生分子内1+2缩合反应, 合成了首例1,3-交替构象的硫杂杯-1,3-2,4-氮杂双冠醚(3), 产率为65%. 其结构经元素分析、质谱、核磁共振谱等表征证实. 用UV-Vis光谱法和1H NMR谱研究了化合物3与系列α-氨基酸的识别配合性能, 并计算出其配合常数. 结果表明, 主体分子3对所测试的α-氨基酸有较好的配合作用, 主客体分子形成1∶1的配合物.     

Unusual regioselectivity of Pd(0)-catalyzed coupling reaction of electron-deficient alkenyl halides with allenic/propargylic zinc reagents. Highly selective synthesis of 6-phenylhex-5-yn-2(or 3)-enoates/enitrile and 4-phenyl-6-substituted-hexa-2,4,5-trienoates

The Pd(0)-catalyzed coupling reaction of electron-deficient alkenyl halides with the organozinc formed by the subsequent treatment of 1-phenylalk-1-yne with n-BuLi and ZnBr2 with or without a catalytic amount of HgCl2 was studied. Both the allene-formation- and the alkyne-formation-type coupling reactions were observed with high regio- and stereoselectivity: the reaction of 1-phenylprop-1-yne afforded 6-phenylhex-5-yn-2(or 3)-enoates and -enitriles, while the reaction of 1-phenylhex-1-yne formed 4-phenyl-6-substituted-hexa-2,4,5-trienoates. A plausible explanation for the regioselectivity was discussed. The double bonds in 6-phenylhex-5-yn- 2-enoates were prone to migrate to the position conjugated with the carbon-carbon triple bonds to form 6-phenylhex-5-yn-3-enoates at higher temperature. The migration did not occur in absence of an excess amount of allenic/propargylic zinc reagent or at low temperature.     

氧化锌薄膜的电化学沉积和表征

以透明导电玻璃(TCO)为衬底，用硝酸锌水溶液作为电解液，研究了阴极还原沉积ZnO薄膜的反应机理和电化学行为. 通过改变工艺条件来控制ZnO的生长速率， 得到了粒径为10～15 nm的纳米ZnO薄膜. XRD分析显示纳米ZnO薄膜纯度高， 呈纤锌矿结构. 光学测试结果表明，在可见光区其透光度高达90%，禁带宽度为3.37 eV.     

高频燃烧红外吸收光谱法测定钨钛合金中碳含量

建立高频燃烧红外吸收光谱法测定钨钛合金中碳含量的分析方法。在1980 W分析功率下,称取0.3 g样品,以2.0 g钨锡及0.5 g纯铁混合助熔,用高频红外分析仪测定碳。碳的含量在0.013%~0.050%范围内与红外吸收峰面积线性相关,相关系数为0.9993。碳的测定下限为3.6μg/g,方法检出限为1.08μg/g。该法测定结果的相对标准偏差为2.97%~4.11%(n=8),碳的加标回收率为96.2%~103.1%。该方法能够满足合金中碳含量的分析要求。     

Et2NH2[Nd(S2CNEt2)4]的晶体结构和生成反应焓变

在干燥氮气气氛下,以无水乙醇为溶剂,制备了低水合氯化钕与二乙氨基荒酸二乙铵(D-DDC)配合物,确定其组成为Et2NH2[Nd(S2CNEt2)4].单晶结构分析表明,配合物中4个二乙氨基荒酸根各通过2个硫原子与钕离子成键形成八配位十二面体阴离子,并与二乙铵阳离子形成缔合型分子.晶体属单斜晶系,空间群P21/n,a=1.37517(14)nm,b=2.1146(2)nm,c=1.44641(15)nm,β=102.028(2)°,Z=4.用微量热法测定了298.15K下水合氯化钕和D-DDC在无水乙醇中的溶解焓及二乙氨基荒酸钕液相生成反应焓变分别为(-17.89±0.096),(50.280±0.151)和(-10.116±0.065)kJ/mol,求得固相生成反应焓变.     

TiO2-SiO2光催化纸业废水有色有机物的降解

研究了TiO2-SiO2混合氧化物对纸业废水中有色有机物的吸附与光催化降解效率．常温下．TiO2对纸业废水中有色有机物的吸附符合Freundlich模型，Qe=0．239Ce^0.791。TiO2-SiO2混合氧化物对纸业废水中有色有机物的吸附与光催化降解效率与催化剂样品的组成有关，光催化降解效率也与TiO2-SiO2表面总酸量有关．     

A Novel Synthesis of Two-dimensional Nanopatterned TiO2 Thin Film

Recently the research on structures with an ordered two-dimensional(2D) pattern has attracted great attention due to its versatile applications in the fields of microelectronic and optoelectronic devices, displays, biochips and sensors, enzymatic immobilization, drug carriers, and photonic band gap materials. Various well-arrayed 2D structures have been made by the modern technique such as laser writing pattern fabrication, photoetching technique, micro-electromechanical systems based on scann…     

Dienone—phenol Rearrangement of C—9 Oxygenated Decalinic Dienone and Analogs through B—Ring Cleavage

Dehydrogenation of 9-hydroxy decalinic enones and analogs with DDQ resulted in a formal dienone-phenol type rearrangement via B-ring cleavage, while the corresponding dienone acetates underwent base-catalyzed formal dienone-phenol type rearrangement analogously.     

B2O3/TiO2-ZrO2催化环己酮肟气相Beckmann重排反应研究 Ⅰ.B2O3含量的影响

 制备了不同B2O3含量（0～20％）的B2O3／TiO2－ZrO2固体酸催\r\n化剂，用XRD，FT－IR，N2吸附及NH3－TPD等方法测定了其结构、比表\r\n面积、孔分布和表面酸性．结果表明，当B2O3含量较低（≤5％）时，\r\n催化剂呈无定形态，样品中的B2O3主要以BO4结构存在．当B2O3含量较\r\n高（≥8％）时，催化剂中的TiO2－ZrO2以ZrTiO4晶相存在，分散于Ti\r\nO2－ZrO2表面的B2O3主要以玻璃体形式和BO3结构存在．随着B2O3含量\r\n的增加，催化剂的比表面积减小，孔径增大．300℃下的环己酮肟气相\r\nBeck－mann重排反应结果表明，随着B2O3含量的增加，己内酰胺的选择\r\n性逐渐增大，而己内酰胺的收率在B2O3含量为12％时达到最大值．讨论\r\n了B2O3／TiO2－ZrO2的催化性能与其表面酸性及孔径大小的关系．