Study on antimony oxide self-assembled inside HZSM-5

Sb/ZSM-5 was obtained by solid-state reaction with the mixture of Sb₂O₃ and zeolite HZSM-5 under a dry nitrogen flow at 773 K. Characterization of the treated zeolite was undertaken with XRD, ²⁷Al MAS NMR, BET, TGA and FT-IR. The results revealed that part of the antimony oxides migrated into the channels of zeolite, and decreased the Brönsted acid sites in Sb/ZSM-5 remarkably. The other part of antimony oxides together with the amorphous alumino-silicate in the products distributed on the external surface of zeolite ZSM-5 and modified it, while the framework of ZSM-5 in crystal phase was retained. The structure of occluded antimony oxide inside the channels of ZSM-5 was studied by XRD Rietveld method. The result showed that their structure can be described as a chain of non-perfect [Sb₅O₅(H₂O)₂]_n⁵ⁿ⁺, which is parallel to the straight channel of ZSM-5. There is about 0.6 [Sb₅O₅(H₂O)₂]⁵⁺ unit in every cell of the ZSM-5 on an average.     

复合蛋白锌在儿科疾患方面的应用

儿童缺锌是较普遍的社会现象，济南泉城微量元素生命研究所研制的复合蛋白锌系采用生物技术转化而得到的一种蛋白复合物，属生物合成的有机微量元素，经急性和长期毒性试验均未发现毒副作用，经检测不含兴奋剂，用于临床后，对纠正偏食厌食，反复呼吸道感染和智力低下等近千例儿童疾患，显示了可喜的临床效果，证明是优质有机补锌剂。     

氮杂冠醚与碱金属离子配位反应的研究

滴定量效法是研究反应热化学和热力学的重要手段之一．用这种方法对冠醚与金属离子的配位反应热力学性质进行研究一直受到很大关注【且S习．但是对氨杂冠林，尤其是一系列结构相似的氨杂冠醚体系进行系统的热力学性质研究的报导不多．前文K则曾报导了用自组装的消定量热计对银（I）－a吹体系和铜（11）·N，N’一问位取代革基乙二胺体系的配位反应热化学研究结果·本文报导从（对位取代革基）k杂15冠5卜RPW15CS，R＝CIZH；CHa；CHso）与碘化钠和碘化钾在25T、无水乙过溶液中进行配位反应的消定量效研究结果．讨论了配体上取代基的电…     

Highly Effective Phenol Hydroxylation over Ti-ZSM-5 Catalyst Prepared Using B-ZSM-5 as Precursor 以B-ZSM-5为母体合成Ti-ZSM-5高效苯酚羟基化催化剂

 以改进方法合成的B-ZSM-5为母体,采用气固相同晶取代法合成了较小晶粒的Ti-ZSM-5分子筛. 考察了样品的物化性能和催化苯酚羟基化性能. 结果表明: 所合成的小晶粒Ti-ZSM-5具有较高的结晶度,尺寸为100~200 nm,且不含锐钛矿型TiO2,对苯酚羟基化反应的催化性能优异.     

[2+2]-Photocycloaddition von Cyclohexen an 2-Acetyl-5,5-dimethyl-1,3-cyclohexandion und 3-Acetyl-1,5,5-trimethyl-2,4-pyrrolidindion

Summary Irradiation of solutions of excess cyclohexene and 2-acetyl-5,5-dimethyl-1,3-cyclohexanedione (1), and 3-acetyl-1,5,5-trimethyl-2,4-pyrrolidinedione (4) results mainly in the formation of 1,5-diones2 and5. These originate from intermediate cycloadducts of cyclohexene and theexo-enols of the cyclic 1,3-diketones. The yields decrease with increasing polarity of the solvent. In solution2 and5 are in equilibrium with the cyclic hemiacetales3 and6.

     

Efficient synthesis of CCR5 antagonist, 2,3-dihydro-1-benzothiepine derivatives by improved intramolecular Claisen type reaction using dialkylcarbonate

The efficient synthesis of 2,3-dihydro-1-benzothiepine derivatives 4 has been developed. The intramolecular Claisen type reaction of the new products, 4-(o-formylphenylthio)butyrate 9, with alcoholate in dialkylcarbonate as a solvent afforded 4 in good yields. According to this new procedure, we have accomplished the practical preparation of CCR5 antagonist 1 as a candidate for oral HIV-1 therapy.     

Catalytic Para‐Xylene Maximization. V. Toluene Methylation with Methanol and Disproportionation of Toluene Using Pt/ZSM‐5 and Pt/Mordenite Catalysts

Toluene was methylated with methanol and disproportionated using catalysts containing different Pt contents (0.2, 0.4 and 0.6%) supported on H‐ZSM‐5 or H‐mordenite (H‐M) zeolites in a fixed‐bed flow‐reactor operated atmospherically at temperatures of 300–500 °C in a flow of hydrogen. Platinum dispersion in the zeolite supports and acid sites strength distribution were evaluated using hydrogen chemisorption (1:1 stoichiometry) and ammonia temperature programmed desorption (TPD) in a differential scanning calorimeter (DSC). Toluene methylation was much faster on all catalysts than toluene disproportionation (DISP). Both reactions were more accelerated using H‐ZSM‐5 containing catalysts than H‐M containing catalysts. The yield of xylenes, and in particular para‐xylene, was significantly influenced by the yield of trimethylbenzenes (TMBs) in product. The selectivities for para‐, ortho‐ and meta‐xylenes production were found largely dependent on the Pt content in the catalysts, particularly when supported on H‐ZSM5‐zeolite. However, using Pt/H‐M catalysts, these selectivities were not strictly controlled by Pt content in the catalysts.     

氧氟沙星荷移络合物的荧光特性和应用

研究了电子受体氯冉酸(CL)和2,3 二氰5,6 二氯1,4 对苯醌(DDQ)与电子给体氧氟沙星之间的荷移反应。实验发现,氧氟沙星与以上两种电子受体在氯仿中可生成稳定的n π络合物,其荧光强度较之氧氟沙星分别增强了22和54倍。据此建立了两种基于荷移反应简便可靠地测定氧氟沙星的荧光光谱新方法。CL法和DDQ法测定氧氟沙星的质量浓度分别为0 06～2.4μg/mL和0 16～2.0μg/mL时,荧光强度与质量浓度呈良好的线性关系。该方法已用于药物制剂中氧氟沙星的测定,其回收率分别为98.4%～100.9%和98.5%～100.4%。     

细胞色素b5Glu44,Glu56的定点突变和蛋白质结构比较

用寡聚核苷酸定点突变的方法将牛肝细胞色素ｂ５基因上第４４位和５６位谷氨酸的密码子ＧＡＡ变成氨酸的密码子ＧＣＴ，获得突变体Ｅ４４Ａ，Ｅ５６Ａ和Ｅ４４／５６Ａ的基因。 它们分别克隆于ＰＵＣ１９上，转化大肠杆菌ＪＭ８３后，突变基因得到成功的表达。     

A column packing for isothermal gas chromatographic analysis of C1−C5 paraffins and monoolefins and dimethyl ether

Summary An analytical GC method was developed which uses a single packed column consisting of three packings in series prepared with the following liquid phases: dimethyl sulfolane, propylene carbonate, and silver nitrate. This system provides satisfactory resolution of mixtures of C₁–C₅ hydrocarbons and dimethyl ether obtained when converting methanol to gasoline. Due to the high capacity of the column it is possible to inject larger sample amounts permitting trace analysis.