硅胶负载钯催化剂对丙烯酸甲酯的催化加氢性能研究

本文报导一种新法制备的硅胶负载钯催化剂,其活性组份大部分负载于载体的表面。该催化剂在常温常压下对丙烯酸甲酯的液相加氢反应,即有很高的活性和良好的重复使用性能。 催化剂按下法制备:在圆底烧瓶中加入1.00g硅胶和20mL甲醇,抽真空置换出硅胶孔内的空气,在搅拌下加入一定浓度的吸附质(聚乙烯亚胺、正丙胺、正丁胺等),在25℃反应3—4小时,过滤,固体经甲醇充分洗涤后和一定浓度的氯化钯甲醇溶液反应6小时。过     

Flow injection spectrofluorimetric determination of reserpine in tablets by on-line acetone sensitized photochemical reaction

On-line photochemical reaction of reserpine in the presence of acetone was investigated. Acetone was found to speed up the on-line photochemical conversion of reserpine into an intensively fluorescent compound. Not only reaction acidity but also the acetate buffer concentration affected the on-line photochemical induced fluorescence signal. Based on the observation an automated flow injection photochemical fluorimetric approach was developed. An injected sample zone was carried by a water stream to be merged with a acetate buffer (pH 3.4) solution containing 0.02% acetone in a knotted PTFE reactor (KR), which was freely coiled around a 6-W low pressure mercury lamp. While passing the KR, reserpine was transformed into an intensively fluorescent compound. It was on-line detected in a flow-through cell at the emission wavelength of 490 nm and excitation wavelength of 386 nm. At optimized conditions, a detection limit 0.45 mug l(-1) was achieved at a sampling rate of 90 h(-1). Eleven determinations of a 0.5 mg l(-1) reserpine standard solution gave a R.S.D. of 0.3%. The linear dynamic range of reserpine calibration curve was 0.01-0.75 mg l(-1). The proposed method was applied to assay the reserpine content in tablets and to monitor the dissolution profile of reserpine tablets. Satisfactory results were obtained for both the assays and dissolution studies.     

磷化氢与环烯烃反应的原位^3^1P NMR研究

本文应用加压原位核磁共振波谱技术, 在反应温度50-70℃、反应压力1.0-2.0MPa, 氘代苯为溶剂, 偶氮二异丁腈为引发剂的条件下, 考察了磷化氢与环烯烃1, 5-环辛二烯、双环戊二烯、1, 3-环己二烯、1, 4-环己二烯及1, 5, 9-环十二三烯的反应。实验结果表明, 磷化氢与1, 5-环辛二烯反应主要生成双环膦杂环壬烷; 与其它环烯烃均不生成膦杂环化合物, 仅为一取代伯膦或二取代仲膦产物。磷化氢与环烯烃反应仍为串行机理。     

Interaction between netropsin and double-stranded DNA in capillary zone electrophoresis and affinity capillary electrophoresis

Poor sensitivity and low phase ratio are the main drawbacks of open tubular capillary electrochromatography (OTCEC). The poor sensitivity results from the use of narrow bore size capillary, whereas the low phase ratio, which limits the separation capability, is caused by the limited surface area of conventional capillary. Two strategies may be useful to overcome these disadvantages. First, an extended light path (ELP) capillary, which has a bubble cell at the detection point, is used to improve the sensitivity. Secondly, an etched capillary of a 1,000-fold increased surface area is used to enhance the phase ratio. In this work, use of an ELP capillary and an etched capillary in OTCEC was evaluated with a chiral stationary phase of avidin prepared with the physical adsorption method. With a 20 microm I.D. ELP capillary with a 150 microm bubble cell, the peak height was enhanced by 4-10-fold and the corrected peak area was increased by 12-fold relative to a 20 microm I.D. conventional capillary. However, the peak efficiency and resolution decreased noticeably. The phase ratio on the etched capillary was slightly enhanced, by a factor of 1.64 relative to an unetched capillary. Consequently, the separation capability was slightly improved. The increase in the phase ratio was much lower than that expected from the increase in surface area, the reason for which is probably the reduced density of surface silanol group and the generation of nitrogen-containing groups due to the etching process.     

Organosoluble and transparent polyimides derived from alicyclic dianhydride and aromatic diamines

Organosoluble polyimides were synthesized with the alicyclic dianhydride 1,8‐dimethylbicyclo[2,2,2]oct‐7‐ene‐2,3,5,6‐tetracarboxylic dianhydride and aromatic diamines. The polyimides possessed good solubility both in strong dipolar solvents and in common solvents; the thermal decomposition temperature of the polyimides exceeded 420 °C. Strong and flexible films of the polyimides, with the cutoff of ultraviolet–visible absorption lower than 310–320 nm, exhibited good features as the alignment layers for nematic liquid crystals with pretilt angles of 1.5–2.9°. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 40: 110–119, 2002     

Use of α‐diketones as visible photoinitiators for the photocrosslinking of waterborne latex paints

The efficiency of several α‐diketones as visible light photoinitiators for the crosslinking of waterborne latex dispersions in the presence of acrylic monomers was evaluated. Among the eight α‐diketones studied, camphorquinone allows the fastest curing speed, and the curing of the acrylic waterborne coating is not affected by the presence of oxygen. The properties of the sunlight‐cured volatile organic compound (VOC)‐free pigmented paints prepared from the waterborne latex are as good or better than the equivalent conventional paint containing VOCs. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 3171–3181, 2002     

神经毒品解毒和戒瘾的新疗法──血液灌流疗法

贩毒吸毒是当今世界最严重的社会公害之一，对社会安定和人们的身心健康构成极大威胁。至今，解毒和戒瘾还一直沿用传统医疗手段。本文介绍了毒品的药理学和成瘾机制以及有关解毒戒瘾的治疗方法，着重探讨了血液灌流疗法在治疗毒品滥用上的应用前景。     

R-(—)-1-氯甲基-4-乙基-2,8,9-三氧杂-5-氮杂-1-硅杂三环[3,3,3,0~(1.5)]十一碳烷的晶体结构

杂氮硅三环是一类具有特殊生理活性的新型有机硅化合物,有关其合成及性质在近20年中已有大量报道。特别是当R为氯甲基时,该化合物的生理活性很高,用它制成的药膏已用来治疗脱发及伤口愈合。因此,1-氯甲基杂氮硅三环(Ⅰ)的分子结构引起了人们的关注,先后有人报道了(Ⅰ)及1-氯甲基-3,7-二甲基,1-氯甲基-3,7,10-三甲基     

碱金属沸石上乙醇双分子缩合反应及其机理

首次发现在碱金属Ｘ沸石上乙醇能够发生以正丁醇为主产物的双分子缩合反应，在所研究的催化剂中，含Ｒｂ的ＬｉＸ沸石表现出较高的反应活性和选择性。反应机理的研究表明，反应不经过ａｌｄｏｌ缩合步骤。在此基础上，对反应机理提出了新建议：在碱性沸石作用下，乙醇的β－位Ｃ－Ｈ键被活化，双分子脱水导致缩合。碳链的增长按此模式进行。