3,5—二羟基苯乙酮的合成

３,５——二羟基苯乙酮（１）是合成平喘药如非诺特罗、班布特罗等药物的原料,目前国内尚无商品出售。本文作者参考有关文献［１］［２］［３］,设计出了如下的合成路线：ＣＯＯＨＨＮＯ３Ｈ２ＳＯ４→（２）Ｏ２ＮＣＯＯＨＮＯ２ＳＯＣｌ２→（３）Ｏ２ＮＣＯＣｌＮＯ...     

铁、锰与尿素配合物微量元素肥料的合成

本文用硝酸铁和硝酸锰与尿素反应，合成了组成为［Ｆｅ（Ｎ２Ｈ４ＣＯ）６］（ＮＯ３）３和［Ｍｎ（Ｎ２Ｈ４（ＣＯ）６）］（ＮＯ３）２·２Ｈ２Ｏ固体配合物。它们均易溶于水，在空气中稳定，吸湿性较小。红外光谱提示，铁（Ⅲ）、锰（Ⅱ）与尿素中的氮原子发生了配合，使金属更易被植物吸收，使氮缓释，因而合成的配合物不仅是优良的配合型微量元素肥料，而且也是长效氮肥。     

Na2O—Al2O3—B2O3—SiO2系统溶胶,凝胶涂层的振动光谱研究

本文用振动光谱分析了Ｎａ２Ｏ－Ａｌ２Ｏ３－Ｂ２Ｏ３－ＳｉＯ２系统溶胶中的化学反应和用浸渍法制备的凝胶涂层结构。结果表明：部分硼、铝在溶胶陈化初期就与Ｓｉ（ＯＣ２Ｈ５）４的水解或缩聚产物反应形成线性聚合物，宜于浸涂。热处理时涂层中继续形成Ｓｉ－Ｏ－Ｓｉ、Ｓｉ－Ｏ－Ａｌ和Ｓｉ－Ｏ－Ｂ键；基本结构单元为［ＳｉＯ４］、［ＢＯ４］、［ＢＯ３］和［ＡｌＯ４］。     

1，5－二（2－硝基苯氧基）－3－氮杂戊烷及其N－取代物的合成

报道了９个新型二硝基化合物的合成。将１，５－二（２－硝基苯氧基）－Ｎ－对甲苯磺酞基－３－氮杂戊烷用３３％ＨＢｒ－ＨＡｃ脱磺酰基得到１，５－二（２－硝基苯氧基）－３－氮杂戊烷。Ｎ－取代氮芥与邻硝基苯酚在碳酸钾存在下，在ＤＭＦ中，于８０℃缩合反应６ｈ得到Ｎ－取代－１，５－二（２－硝基苯氧基）－３－氮杂戊烷，取代基为：ＣＨ＿２ＣＨ＝ＣＨ＿２，Ｃ＿４Ｈ＿（９－ｎ），Ｃ＿５Ｈ＿（１１－ｎ），ＣＨ＿２ＣＨ＿２ＯＣＨ＿３，ＣＨ＿２ＣＨ＿２ＯＣ＿２Ｈ＿５，ＣＨ＿２ＣＨ＿２ＯＣ＿４Ｈ＿（９－ｎ），（ＣＨ＿２ＣＨ＿２Ｏ）＿２ＣＨ＿３，（ＣＨ＿２ＣＨ＿２Ｏ）＿２Ｃ＿４Ｈ＿（９－ｎ）。     

肥料级磷铵与工业级磷铵联产工艺

肥料级磷铵与工业级磷铵联产工艺王鹤楼，黄大雄（四川省化工设计院）正磷酸铵盐是磷酸盐产品中一个重要的系列产品，主要有磷酸二氢铵［ＮＨ＿４Ｎ＿２ＰＯ＿４］磷酸氢二铵［（ＮＨ＿４）＿２ＨＰＯ＿４］和磷酸铵［（ＮＨ＿４）＿３ＰＯ＿４·３Ｈ＿２Ｏ］，它们在肥料...     

邻苯二甲酰亚胺在K2CO3—Al2O3负载型碱试剂作用下的苄基化反应

邻苯二甲酰亚胺在Ｋ＿２ＣＯ＿３－Ａｌ＿２Ｏ＿３负载型碱试剂作用下的苄基化反应陆文兴，颜朝国（扬州大学师范学院化学化工系，扬州２２５００２）Ｎ－烃基邻苯二甲酰亚胺类化合物是合成脂肪族伯胺和－氨基酸的重要中间体。Ｎ－烃基化反应可使用催化剂或在强碱条件下进...     

Keggin结构稀土硅钨钒杂多配合物的合成与性质研究

报道了通式为Ｋ１３Ｈ２［Ｌｎ（ＳｉＷ１０ＶＯ３９）２］·ｘＨ２Ｏ（Ｌｎ＝Ｌａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｎ）［简记为Ｌｎ（ＳｉＷ１０Ｖ）２］６种配合物的合成方法。并利用顺磁共振光谱、磁化率、Ｘ射线粉末衍射、差热热重分析和循环伏安－极谱方法研究了它们的性质。     

Keggin结构稀土硅钨钒杂多配合物的合成与性质研究

报道了通式为Ｋ１３Ｈ２［Ｌｎ（ＳｉＷ１０ＶＯ３９）２］·ｘＨ２Ｏ（Ｌｎ＝Ｌａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｎ）［简记为Ｌｎ（ＳｉＷ１０Ｖ）２］６种配合物的合成方法。并利用顺磁共振光谱、磁化率、Ｘ射线粉末衍射、差热热重分析和循环伏安－极谱方法研究了它们的性质。     

含有弱金属-氮键的磷钼酸有机衍生物的研究

［（ＥＤＴＢ）Ｍ］（ＣＨ３ＣＯＯ）２和Ｈ３ＰＭｏ１２Ｏ４０在无水乙醇中反应得到［（ＥＤＴＢ）Ｍ］（ＨＰＭｏ１２Ｏ４０）,Ｍ为Ｃｕ、Ｃｏ,ＥＤＴＢ为Ｎ,Ｎ,Ｎ′,Ｎ′－四［（２－苯并咪唑）甲基］－１,２－乙二胺。测定了它们的ＩＲ、ＨＮＭＲ、紫外－可见光谱和元素分析以及对酯化和乙酸环己酯热消除反应的催化活性。     

一种有用的锌配合物的制备研究及其可能机理

二（１,３－二硫杂环戊烯－２－硫酮－４,５－二硫）合锌酸的四级铵盐（以下简写为［Ｚｎ］）是合成有机超导材料ＢＥＤＴ－ＴＴＦ［１］的原料,它是合成含硫取代基ＴＴＦ的重要试剂。其合成文献［２～５］报道较多,但产率均不高,且操作要在惰性气氛或无溶剂下进行。本文对［Ｚｎ］制备工艺进行了研究,取得了满意结果,并提出了可能机理。合成路线如下：ＣＳ２＋ＮａＤＭＦＳＳＳＮａＳＳＮａＺｎＣｌ２,Ｅｔ４ＮＢｒＣＨ３ＯＨ,ＮＨ３·Ｈ２Ｏ（Ｅｔ４Ｎ）２ＳＳＳＳＳＺｎＳＳＳＳＳ　［Ｚｎ］１　实验将ＤＭＦ滴加到１８ｍＬ二硫…     

四元混配配合物[Ln(x-MBA)2(NO3)(Phen)]2的合成及表征

在酸性介质,乙醇／水混合溶剂中合成得到了三个系列的四元混配配合物[Ln(x-MBA)2(NO3)(Phen)]2(Ln=La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Er;MBA=CH3C6H4COO^-）。用元素分析、IR、UV、DTA－TG和^1H NMR等方法对配合物进行了表征,测量了三个Eu配合物的荧光光谱和三个Gd配合物的ESR谱。     

Relationship Between Structure and Coordination Strength of N and N,O-Hybrid Donor Ligands with Trivalent Lanthanides

ABSTRACT

To effectively separate lanthanides (Ln(III)) from actinides (An(III)), symmetrical 2,2′-bipyridyl (Bpy), 1,10-phenanthroline (Phen), and unsymmetrical N-methyl-N-tolyl-1,10-phenanthroline-2-carboxamide (MeTol-PTA) were investigated. According to the crystal structures and EXAFS experiments, the decreasing ionic radius from light to heavy Ln led to decreases in the Ln–N (Bpy) and Ln–N (Phen) distances, while log β simply increased due to the electrostatic interaction and the order of Ln–O (MeTol-PTA) < Ln–N (Bpy, Phen) < Ln–N (MeTol-PTA) was obtained. This indicated that the bulky phenanthroline moiety of MeTol-PTA may not allow N (MeTol-PTA) to come close to Ln. Consequently, the log β of MeTol-PTA exhibited a local maximum (around Nd).     

Ln(Ⅲ)与糠醛缩-L-酪氨酸席夫碱配合物的合成

合成了Ln(Ⅲ)(Ln=Gd、Dy、Nd、Er、La、Sm)与糠醛缩 L 酪氨酸席夫碱的6种配合物,通过元素分析、红外光谱、紫外光谱、摩尔电导和热重分析,得到了配合物的组成为[Ln(C14H12NO4)(NO3)(H2O)2](NO3)(H2O)x(x=0～2)。得到了Er配合物的热分解反应动力学机理。     

Preparation of Tb(Pht)3Phen/rubber composites and characterization of their fluorescent properties

A rare‐earth ternary complex compound, Tris‐(terbium‐phthalate)‐1, 10‐phenanthroline Terbium (III) [Tb(Pht)₃Phen], was synthesized through the reaction among a rare‐earth oxide (Tb4O7), potassium hydrogen phthalate and phenanthroline, and its structure was characterized with scanning electron microscopy (SEM), laser particle size (LPS), IR, and X‐ray diffraction. This was the first time that Tb(Pht)₃Phen/rubber [nitrile butadiene rubber (NBR) or methyl vinyl silicone rubber (SiR)] composites had been prepared through mechanical mixing processing. SEM revealed that the dimensions of Tb(Pht)₃Phen dispersed in matrix rubber were much smaller than those of the original particles of the complex compound. The Tb(Pht)₃Phen/rubber composites showed much better luminescent performance than the Tb(Pht)₃Phen complex compound. The fluorescent intensities of the Tb(Pht)₃Phen/rubber composites were strongly dependant on the concentration of Tb(Pht)₃Phen, and 30 phr was the optimal concentration for both the Tb(Pht)₃Phen/NBR and Tb(Pht)₃Phen/SiR composites. Within the concentration range of Tb(Pht)₃Phen used in this work, the fluorescent intensions of the SiR composites were stronger than those of their NBR counterparts. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 20–28, 2005     

镝(Ⅲ)-BDPPPD配合物的合成及其荧光性质

以二氧六环为溶剂 ,在 pH约为 7的条件下 ,分别以n (Dy3+ )∶n (BDPPPD) =2∶3和n (Dy3+ )∶n(BDPPPD)∶n(Phen ) =2∶3∶2的量比 (Phen为邻菲罗啉 ) ,合成了Dy(Ⅲ)的 1,5 双 (1′,3′ 二苯基 5′ 氧代吡唑 4′ 基 ) 1,5 戊二酮 (BDPPPD)的二元配合物Dy2 (BDPPPD) 3·6H2 O和三元配合物Dy2(BDPPPD) 3(Phen) 2 ·2H2 O ,收率为 91 2 %和 89 6 %。通过化学分析、元素分析和热分析确定了配合物的组成 ,通过FT -IR谱对配合物进行了表征。测定了配合物的荧光光谱 ,配合物的荧光发射峰位于 481和 5 76nm附近 ,分别相应于Dy3+ 的 4 F9/2 → 6H15/2 和 4 F9/2 → 6H13/2 跃迁 ,说明配合物发射Dy(Ⅲ)的特征荧光。第二配体Phen具有荧光增强作用 ,三元配合物Dy2 (BDPPPD) 3(Phen) 2 ·2H2 O最大发射峰 (5 76nm)的荧光强度是二元配合物Dy2 (BDPPPD) 3·6H2 O的 1 6 8倍。配合物具有较强荧光 ,说明BDPPPD的三重态能级与Dy3+ 最低激发态 (4 F9/2 )能级具有良好匹配 ,且其吸光系数较高 ,BDPPPD是Dy(Ⅲ)发光配合物的适宜配体     

Multi stimuli-responsive HPC-PAA/Eu(AA)3Phen complex nanogels and their decoration with 3-APBA for detecting glucose

In this paper, novel multi stimuli-responsive complex nanogels of hydroxypropylcellulose (HPC)-PAA/Eu(acrylic acid [AA])₃Phen were synthesized by radical polymerization method with HPC, rare earth complex (Eu(AA)₃Phen) and AA as raw materials, and the 3-aminophenylboronic acid (3-APBA) decorated nanogels (HPC-PAAPBA/Eu(AA)₃Phen) were fabricated via condensation of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride with 3-APBA. The microstructure, morphology and diameter of the nanogel were characterized by Fourier transform infrared spectrometer, UV–Visible spectrophotometer, transmission electron microscope, dynamic light scattering. Moreover, the fluorescence responsive performance of complex nanogels to temperature, pH value and glucose concentration was investigated by photoluminescence spectroscopy. The results showed that both of the as-prepared nanogels were uniform in size and had good monodispersity. The temperature and pH value had significant effects on the particle size and the fluorescence emission intensity of the HPC-PAA/Eu(AA)₃Phen complex nanogels; after decoration with 3-APBA, the obtained HPC-PAAPBA/Eu(AA)₃Phen nanogels showed excellent stimulus-response to glucose concentration.     

稀土配合物[Ln(C_3H_7NO_2)_x(C_3H_4N_2)(H_2O)](ClO_4)_3(Ln=La,x=3;Ln=Pr,Nd,Sm,x=2)的合成、表征与热分析

合成了稀土高氯酸盐与咪唑、DL α 丙氨酸的4种配合物晶体。经傅里叶变换红外光谱(FTIR)、元素分析和化学分析测定后确定其组成为[Ln(C3H7NO2)x(C3H4N2)(H2O)](ClO4)3(Ln=La,x=3;Ln=Pr,Nd,Sm,x=2)。用差示扫描量热法(DSC)测定了4种配合物的热分解数据,4个配合物开始熔化分解的温度分别为502 5K,532 4K,495 7K,516 7K,配合物有较高的热稳定性。     

高氯酸化三邻菲啰啉合锌(Ⅱ)的合成及晶体结构

合成了过渡金属元素Zn与1,10-邻菲啉的配合物,并进行了元素分析、红外光谱等表征,测定了配合物的晶体结构。配合物组成为[Zn(Phen)3](ClO4)2,属于单斜晶系,P2(1)/n空间群。配合物中金属离子Zn2 处于N6的配位环境,配位构型为六配位的扭曲八面体。     

YAG：Ce,Ln体系中Ce~（3＋）的荧光寿命的研究

采用高温固相法合成了一系列的（Y0.95Ln0.01Ce0.04）3Al5O12（简称YAG∶Ce,Ln）,系统地研究了此体系中Ln3＋对Ce3＋的荧光寿命的影响。结果表明,荧光寿命数值能够较好地说明双掺杂晶体中除Ce3＋以外的其它三价稀土离子（Ln3＋）对Ce3＋的发光强度的增强或者猝灭现象。     

Dense ceramics of lanthanide-doped Lu2O3 prepared by spark plasma sintering

Dense ceramics of Ln:Lu₂O₃ (Ln = Pr, Eu, Tb, Dy) were obtained using spark plasma sintering (SPS) from co-precipitated nanocrystalline powders. X-ray diffraction, scanning and transmission electron microscopies were used for the characterization of Ln:Lu₂O₃ powders obtained by various annealing regimes. Transparency of the sintered ceramics was achieved when powders with highly developed crystallinity were used for sintering. Sintered ceramics exhibited luminescence with a characteristic emission based on the element doped into the Lu₂O₃ host. The light yield of the sintered ceramics improved when the sintered ceramics was further annealed. The annealing of the sintered ceramics also improved the transmittance in the visible region; however, the transparency was lost when the annealing temperature was too high. To our best knowledge, the SPS fabrication of dense ceramics of Pr³⁺, Tb³⁺ and Dy³⁺-doped Lu₂O₃ is reported here for the first time.