化学镀法制备银壳聚苯乙烯微球

采用一种新的化学镀法合成银壳包覆聚苯乙烯微球, 通过三乙醇胺和银离子络合来减小反应的氧化还原电位差, 降低银在改性聚苯乙烯微球表面的沉积速率. 采用TEM、XRD、UV 等测试手段对样品进行了分析和表征, 并考察了不同反应条件对实验结果的影响.实验表明, 该方法可在改性聚苯乙烯微球上包覆均匀的银层.     

单核铁(Ⅲ)双卟啉配合物在溶液中的构象平衡及其对环己烷羟化反应的催化活性的影响

合成及表征了一系列以柔韧碳氢链相连不同长度的ｐ／ｐ型单核铁（Ⅲ）双卟啉配合物，以可见光谱首次观察到该系列配合物在氯仿溶液中开放式及闭合式构象的平衡，发现６８０ｎｍ处吸收峰强度与这种构象平衡有关，烷氧链越长，该吸收峰强度越大．利用该类配合物模拟了细胞色素Ｐ４５０单加氧酶对环己烷的羟化作用，催化结果表明，在以分子氧为氧源及还原剂存在的温和条件下，该类配合物的催化活性显著高于单核铁卟啉（ＦｅＴＰＰＣｌ），随着柔韧碳氢链长度的增加，双卟啉的催化活性依次增加．高的催化活性与双卟啉配合物在溶液中的构象平衡，即闭合式构象引起的立体位阻及电子转移有关．     

Schiff碱双核Mn配合物的合成、结构和性能研究

Five manganese complexes of Schiff base were synthesized： [Mn^Ⅳ，Ⅳ(μ-O)(Salen)]₂·DMF·H₂O (1)， [Mn^Ⅳ，Ⅳ(μ-O)(5-BrSalen)]₂·DMF·0.5H₂O (2)， {Mn^Ⅳ，Ⅳ(μ-O)[Sal(1，2-pn)]}₂·H₂O (3)， {Mn^Ⅳ，Ⅳ(μ-O)[5-Br-Sal(1，2-pn)]}₂·H₂O (4)， {Mn^Ⅳ，Ⅳ(μ-O)[5-CH₃-Sal(1，2-pn)]}₂·2H₂O (5)， and were characterized by element analysis， IR and UV-Vis spectra. The results of cyclic voltammogram show that Schiff base ligands can drop the potential of manganese and steady high oxide state of manganese. The magnetic properties of 1 and 3 have also been studied. The results show that there is a weak ferromagnetically coupling of Mn^Ⅳ₂ pair at room and low temperature， and the interactions of complex 3 are weaker than complex 1.     

微交联聚合物降滤失剂的合成与性能

针对深井、超深井钻井液体系中的降滤失剂受长时间高温、高矿化度作用易降解的问题，以氮丙啶与3-氯丙烯反应制得-N-烯丙基氮丙啶（ALAI）； ALAI与乙二胺反应制得四烯基交联剂单体（EAAD）； EAAD与丙烯酰胺（AM）和2 丙烯酰胺基-2-甲基丙磺酸（AMPS）发生水溶液自由基共聚反应，合成了微交联共聚物降滤失剂(PAAT)，其结构和性能经¹H NMR, IR和TG-DTG表征。结果表明：PAAT可抗220 ℃高温，在高温、高矿化度条件下可维持钻井液的滤失量与流变性能，API滤失量均低于4.0 mL，高温高压滤失量均小于13.0 mL。     

Synthesis and properties of niobia films derived from niobium pentaethoxide

The hydrolysis of niobium pentaethoxide precursor in the presence of triethylamine (TEA) is discussed. Three precursors with TEA/Nb(OEt)₅ mole ratios of 0.25, 0.4 and 0.8 were prepared. Niobia colloids with different appearance were obtained after autoclaving the above precursors at 250°C during 12 h. The surface roughness and microstructure of niobia films prepared with the colloids by spread coating method are strongly dependent on the TEA/Nb(OEt)₅ mole ratio. At a value of 0.4 TEA/Nb(OEt)₅ mole ratio, a niobia film with large surface roughness can be achieved. It is opaque and mechanically stable and has differently ordered needle microstructure. The crystalline structure and photoelectrochemical property of niobia film with the largest surface roughness were examined. The effect of CO₂ gas bubbling, reflux and addition of 2-methoxyethanol on the hydrolysis of Nb(OEt)₅ and the nature of the Nb₂O₅ films is also discussed.     

自制苯乙烯-丙烯酸乙酯共聚物与PEG20M复合萃取涂层用于洗涤制品中1,4-氧杂环己烷的测定

采用顶空固相微萃取-毛细管气相色谱联用技术测定了洗涤制品中的1,4-二氧杂环己烷.使用自制的萃取头(苯乙烯-丙烯酸乙酯共聚物与PEG20M复合)于顶空平衡温度80℃下萃取样品40 min.萃取物用内壁涂有SE-30固定液的石英毛细管柱分离,外标法定量.1,4-二氧杂环己烷含量为0.35～120 μg/g时,其峰面积与含量呈良好的线性关系(r=0.999 8);回收率为98.7%～102%;相对标准偏差(n=5)为9.33%.     

煤加氢液化残渣的流变特性研究

采用从煤直接液化实验装置取得的液化残渣，研究了它的流变性及温度和油、沥青质、固体含量对其流变性的影响。液化残渣是剪切变稀的非牛顿型假塑性流体，非牛顿指数随温度升高而不断减小，温度越高越接近牛顿流体行为。液化残渣对温度非常敏感，在升温过程中其表观黏度下降很快，且没有出现黏度峰。在液化残渣中加入少量的循环油后其表观黏度大幅下降；而在加入少量沥青质后则表现出低温下黏度变大，高温下黏度变小的现象；固体含量则始终是黏度增大的因素，表明其黏度与油、沥青质和固体含量关系密切。液化残渣的黏度－温度关系符合Arrhenius关系式，但在升温过程中出现了拐点，低温段的黏流活化能比高温段的要大。     

Rasch模型在“化学键”概念教学评价中的应用研究

运用Rasch模型探查高二学生对"化学键"概念的认知情况，运用Conquest软件和Winsteps软件对测试结果进行分析。结果表明：基于Rasch模型编制的测试卷能客观有效地检测学生对"化学键"概念的理解，为一线教师的有效教学提供学情基础。     

Isolation of a new member of the ecdysteroid glycoside family: 2-deoxy-20-hydroxyecdysone 22-O-beta-D-glucopyranoside

A new ecdysteroid glycoside, 2-deoxy-20-hydroxyecdysone 22-O-beta-D-glucopyranoside, is isolated from the herb Silene italica ssp. nemoralis (Waldst. and Kit.) Nyman. The compound is purified with multistep chromatography, such as classical column chromatography on alumina and droplet countercurrent distribution. Also, it is expanded using twice low-pressure reversed-phase liquid column chromatography. Chromatography in four steps results in the purified 2-deoxy-20-hydroxyecdysone 22-O-beta-D-glucopyranoside. Two other ecdysteroids have also been separated, including the formerly identified integristerone A and 24(28)-dehydromakisterone A.     

THE SYNTHESIS OF MODIFIED DIPHENYL OXIDE RESIN

1. INTRODUCTION Poly (diphenyl oxide) (DPO) resins are a series of heat-resisting thermosetting resins. In 1960s, the West House Company applied them to make H class insulting materials and got an extensive use successfully [1]. But due to the three main…