聚2,6-二甲基苯醚树脂分子量分布及其与冲击强度关系的研究

本工作建立了室温下用凝胶色谱法(GPC)测定聚2,6-二甲基苯醚(PPO)树脂分子量、分子量分布的方法。淋洗剂不采用文献申报道的毒性较大者,也不在较高柱温下进行,而采用甲苯(或氯仿)在室温下测定。对样品在甲苯中溶解温度、浓度和稳定性等都进行了系统研究,找到了最优化条件。GPC数据结合改性PPO(MPPO)产品性能测定结果,经仔细分析找到了影响MPPO产品质量的一个重要因素是PPO树脂中低分子量部分含量。它与产品冲击强度有明显的依赖关系。提出了一个从CPC谱图确定低分子量部分含量的方法。     

N-[5-(1-邻(对)氯苯氧乙基)-1,3,4-噻二唑-2-基]-N'-芳酰基硫脲的合成与生物活性

为了寻找高活性的杂环农药,通过2-氨基-5-(1-邻氯苯氧乙基)-1,3,4-噻二唑和2-氨基-5-(1-对氯苯氧乙基)-1,3,4-噻二唑与芳酰基异硫氰酸酯反应,合成了26种新的芳酰基硫脲.采用核磁共振氢谱、红外光谱及元素分析确证了它们的结构.初步的生物活性测定试验表明,部分目标化合物表现出良好的植物生长调节活性,其中3c,3d,3e,4b和4c具有优良的生长素活性.     

KF－Al2O3催化下3，4－二氢－2H－吡喃[3,2-h]喹啉衍生物的合成

芳醛、8－羟基喹啉与丙二腈或氰乙酸乙酯KF－Al2O3催化下反应生成一系列新 的3，4－二氢－2H－吡喃[3,2-h]喹淋衍生物，产物的结构通过单晶X射线确证。     

机械球磨与反应烧结合成Sr2CeO4发光体的研究

Sr₂CeO₄ phosphor was synthesized by mechanical milling and reactive sintering in this work. The solid state reaction of SrCO₃and CeO₂ (2∶1) started at about 850 ℃ and completed at 1 000 ℃ for about 4 h. Two types of formation mechanism of Sr₂CeO₄ were proposed. When the starting powder mixture was fired above 1 000 ℃, the unstable intermediate phase SrCeO₃was developed, which then reacted with SrCO₃to form the final product Sr₂CeO₄, however, SrCO₃and CeO₂ converted directly to Sr₂CeO₄ at a lower temperature. The XRD results showed the crystal structure of Sr₂CeO₄ was orthorhombic. The emission spectra displayed a broad band with maximum at about 465 nm. The mechanical milling of starting power mixture and the sintering temperature had no effect on this emission spectra.     

电子俘获材料Zn_4B_6O_(13)∶Dy~(3+)的热释光特性研究

通过高温固相扩散反应合成了稀土元素镝掺杂的 Zn4 - x B6 O1 3∶ x Dy3+ 磷光体 .测定了该化合物在高能6 0 Co伽玛射线辐照下的热释发光曲线和三维热释光谱 .三维热释光谱表明 ,位于大约 480 nm和 5 80 nm的发光谱带来自于 Dy3+ 离子的 f-f 跃迁 .基质中掺杂的 Dy3+ 离子浓度的变化能够改变陷阱的相对分布 ,随着Dy3+浓度的增加 ,发光峰温向高温方向移动 ,这可提高剂量器的热稳定性 .当辐照剂量增加时 ,发光峰温亦向高温方向移动 ,即陷阱加深 .确定了 Zn3.86 B6 O1 3∶ 0 .1 6Dy3+样品主峰的陷阱深度 E=0 .73 e V,频率因子S=2 .43× 1 0 9s- 1 .在 1～ 1 0 0 Gy治疗级范围内 ,Zn3.86 B6 O1 3∶ 0 .1 6Dy3+ 对 6 0 Co伽玛射线辐照的热释光剂量响应呈良好的线性关系 .实验结果表明 ,Zn3.86 B6 O1 3∶ 0 .1 6Dy3+是一个潜在的应用于临床医疗的伽玛射线电离辐射热释光剂量计材料 .     

4－（2－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Fe、Co、Ni

４－（２－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Ｆｅ、Ｃｏ、Ｎｉ格日勒，李惠梅，李南强，汪尔康（中国科学院长春应用化学研究所电分析化学开放实验室，北京大学化学系，长春，１３００２２）关键词液相色谱，Ｆｅ，Ｃｏ，Ｎｉ，４－（２－氨基噻唑）...     

A Facile Synthesis of Ethyl 2,4-Dimethoxy-6-perfluoroalkyl-benzoates via Acyclic Precursors

Introduction Polysubstituted arenes are important intermediates in synthetic medicines and dyestuffs, and the fluorinated analogues are more attractive as a result of their lipo-philicity and the increment of activity.1,2 Therefore, to study the convenient and efficient synthesis of polysub-stituted arenes is valuable in organic synthetic method-ology. We have designed a simple synthesis of fluori-nated polysubstituted arenes through the intramolecular Wittig reaction of a new phosphorous ylid…     

3,4,5-三甲氧基苯甲酰甲壳素的制备与表征

在甲磺酸体系中，将具有较好紫外吸收性能的3，4，5—三甲氧基苯甲酸分子键接到甲壳素的分子链上，制得了3，4，5—三甲氧基苯甲酰甲壳素。采用红外光谱、^1H-NMR、广角X—射线衍射、紫外光谱等表征方法对改性产物进行了结构表征。通过对改性产物的紫外光谱表征发现产物具有一定的吸收紫外线能力。产物在有机溶剂中有一定的溶解性能。     

反相高效液相色谱法半制备分离[T(4-MOP)PS4]卟啉的研究

本文研究了新水溶性５，１０，１５，２０－四（４－甲氧基－３－磺酸苯基）卟啉［Ｔ（４－ＭＯＰ）ＰＳ４］的反相高效液相色谱（ＨＰＬＣ）分离条件。采用ＳｈｉｍｐａｃｋＰＲＥＰ－ＯＤＳ半制备色谱柱，用含有１０ｍｍｏｌ／Ｌ四乙基碘化铵的乙腈－水（体积比２５：７５）为流动相，流速１８ｍＬ／ｍｉｎ，于４１８ｎｍ波长下检测。［Ｔ（４－ＭＯＰ）ＰＳ４］与合成中生成的杂质组分完全分离。经此制备的卟啉纯度高，已成功地应用于自来水样中微量钴、锌、铜离子的ＨＰＬＣ测定中。     

Synthesis and crystal structure of 4-acetoxy-5,6-dihydro-5,5-dinitro-2H-1,3-oxazineN-oxide

A novel heterocyclic compound, 4-acetoxy-5,6-dihydro-5,5-dinitro-2H-1,3-oxazineN-oxide, has been synthesized by the reaction of the dipotassium salt of 1,1,5,5-tetranitro-3-oxapentane with aqueous acetic acid. The synthesized compound has been studied by X-ray diffraction analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2207–2210, December, 1994.We would like to thank G. V. Lagodzinskaya (Institute of Chemical Physics in Chernogolovka, Russian Academy of Sciences) for recording and interpreting¹H NMR spectra, A. M. Korolev (Institute of Chemical Physics in Chernogolovka, Russian Academy of Sciences) for helpful discussion, and V. I. Fetisov (Institute of Physiologically Active Compounds, Russian Academy of Sciences) for performing quantum-chemical calculations by the AM1 SCF MO LCAO method.