甲硫基乙醛肟的合成工艺研究

本文研究了以乙醛肟为原料合成甲硫基乙醛肟的工艺。对各种因素对产品收率的影响进行了试验，找出了最佳工艺条件。经过工业性试验，证明本工艺安全可靠，收率稳定，产品质量好，经济效益高。     

IR Spectroscopic Study of the Organic Component of Ultrafine Diamond Produced by Detonation Synthesis

IR spectra of ultrafine diamonds produced by different teams of researchers are studied. The effects of heating and radiation on the properties of ultrafine diamonds are studied. Quantitative assumptions on the kinetics of formation of ultrafine diamonds are made from analysis of IR spectra.     

Degree of crosslinking and mechanical properties of crosslinked poly(vinyl alcohol) beads for use in solid-phase organic synthesis

The limited swellability in polar media of the commonly used polystyrene/divinylbenzene (PS-DVB) support materials for solid-phase organic synthesis has led to the development of novel, highly swellable hydrophilic gels designed for use in aqueous or polar media. Poly(vinyl alcohol) beads crosslinked with epichlorohydrin (PVA-EP) were prepared by a two-step inverse-suspension polymerization method. While it is known that the morphology of the resulting beads can be controlled by the ratio of EP versus PVA as well as by the pre-crosslinking time, the actual degree of crosslinking of the beads and their mechanical properties remain unknown. It is therefore the purpose of this study to evaluate the actual degree of crosslinking of beads prepared with different quantities of crosslinker in the feed by spectroscopic (Raman, nuclear magnetic resonance) and chemical (functional group loading) methods. The mechanical properties of these swollen PVA-EP beads will be evaluated by single-bead unconfined compression in solvents such as water, N,N-dimethylformamide (DMF), and tetrahydrofuran (THF) and compared to model PS-DVB beads commonly used for solid phase synthesis.     

5—烃基—2,3—二甲基吡嗪的合成

2,3-二基-5,6-二氢吡嗪与醛或酮在氢氧化钠的乙醇溶液中反应制得16种5-烃基-2,3-二甲基吡嗪。产率66%～90%。其中6种为新合成的化合物。产率17%～87.9%。     

Electrodeposition of catalytically active nickel for the oxygen evolution reaction — effects of anionic composition

Nickel electrodes were prepared by electrodeposition in electrolytes of various anionic compositions. The deposition conditions and bath types were evaluated with special emphasis on the electrocatalytic properties for the oxygen evolution reaction (OER). Electrochemical characterizations in a 5 mol/L KOH solution at 25°C showed that the electrode deposited from the chloride bath, having a low Tafel slope of 50 mV/dec and an overpotential of 396 mV at 100 mA/cm², is the most catalytically active among electrodes prepared in electrolytes of various anionic compositions. The electrode activity for the OER is related to the real surface areas, which depend on the anion compositions in the deposition bath and the deposition conditions.     

等离子体技术在化学合成中的应用

从等离子体的基本特性出发,综述了等离子体技术在氨气合成、有机物合成、高分子合成以及纳米碳管的合成等方面的应用和最新进展,并展望了等离子体技术在化学合成方面的应用前景.     

高岭土在碳热还原氮化过程中的相变

系统研究了苏州高岭土碳热还原氮化合成SiAlON过程在不同温度下的相变。对试样的XRD、SEM以及EDXA分析结果表明 ,1 30 0℃之前 ,试样中没有氮化物生成 ,物相为莫来石、石英和方石英 ;1 30 0℃时 ,高岭土开始发生氮化反应 ,生成过渡型SiAlON和β SiAlON。此时 ,石英和方石英相基本消失 ;1 4 0 0℃时 ,过渡型SiAlON、β SiAlON和X SiAlON三相共存 ,β SiAlON有所增多并有少量刚玉相生成 ;从 1 4 50℃到 1 550℃ ,Z值为 3的β SiAlON成为惟一的氮化产物 ,与少量SiC和刚玉相并存。莫来石在 1 50 0℃时完全消失     

Pt/C活性催化剂催化氢化合成6-氯-2-羟基喹喔啉

以对氯邻硝基乙酰乙酰苯胺为原料，在碱性条件下经环合及催化氢化合成6-氯-2-羟基喹喔啉。采用自制的Pt／C催化剂，考察了反应条件对产品收率的影响，在85℃，1．0～1．3MPa氢气压力下进行加氢还原反应，总收率89．6％(以对氯邻硝基乙酰乙酰苯胺转化为6-氯-2-羟基喹喔啉)。     

2,6-二乙酰基吡啶合成方法的改进

优化了2，6—二乙酰基吡啶的合成工艺。以2，6—吡啶二羧酸为原料，经过醇化及克莱森酯缩合反应，合成了2，6—二乙酰基吡啶，2，6—吡啶二羧酸二乙醇和2，6—二乙酰基吡啶的分离收率分别为94．1％和88．9％，2，6—二乙酰基毗啶的质量分数大于99％。     

Aldol condensation in gaseous phase by zeolite catalysts

Vapour-phase reactions of, in situ, prepared formaldehyde with methyl propionate were studied using X, Y and ZSM-5 zeolite catalysts. Base properties of these zeolites were enhanced by KOH or NaN₃ treatment. The niobium and molybdenum ZSM-5 zeolite supported oxides were also tested for their catalytic activity. The results are discussed in terms of an ability of zeolite catalysts to synthesize methyl methacrylate.