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％。     

甲基葡萄糖甙（MeG）水溶液工艺改进试验

介绍了用５次以上的母液生产ＭｅＧ水溶液工艺的改进试验。     

熔块釉中三氧化二硼的测定

用NaOH熔融样品，向标准溶液中加入同样量的KOH基体，建立工作曲线，试样酸化后，直接用ICP－AES法测定。     

Nucleation of isolated PO4 units on CeO2 driven by high temperatures and the effect on its oxygen storage and release properties

The chemical nature of P-containing species of varying concentration present in CeO₂ after impregnation with (NH₄)₂HPO₄ and calcination at 1273 K, and their effects on the oxygen storage and release (OSR) properties of ceria are reported for the first time. The samples were characterized by different techniques and the results were compared with those recently reported on the same samples but calcined at 873 K. When P-containing ceria solids were calcined at 1273 K, CePO₄ (monazite) was the predominant P-containing species on the surface of ceria, confirming previous studies that showed that monazite exists for those samples in which the surface P loading (P atoms per nm⁻²) is larger than 5.5. For lower surface P concentrations, isolated orthophosphate units are present at the surface and within the subsurface region of the solid. Severe sintering of CeO₂ after calcination at 1273 K resulted in P concentrations >5.5 P atoms·nm⁻² in all samples. Isolated PO₄ units that could initially be present in the samples calcined at 873 K nucleated and CePO₄ was formed when samples were calcined at 1273 K. OSR properties of CeO₂ deteriorated progressively when P loading increased due to the presence of larger crystals of the very stable Ce(III) phase of CePO₄ at the surface of the P-containing ceria solids.     

Effect of Pt Incorporation into Ni/ZrO2–SO 4 = /Al2O3 Catalyst for n-Butane Isomerization

Three Ni/ZrO₂–SO₄⁼/Al₂O₃ catalysts with different concentrations of platinum (0.2, 0.3 and 0.4 wt%) were prepare and tested for n-butane isomerization reaction at 338 K, in absence and in presence of hydrogen. The results shown that, at low temperature, platinum contributes to the olefin or butyl ion formation and the reaction follows a bimolecular pathway. However, when the reaction occurs in the presence of hydrogen, the formation of butyl ions is inhibited. The main feature of platinum addition is the stabilization of the catalytic activity, which is indicated by the slow deactivation constants compared to that of the unpromoted catalyst.     

聚己二酸1,2-环己二醇酯的合成

采用正交实验方法,分别以钛酸四丁酯和对甲苯磺酸为催化剂,合成了聚己二酸1,2 环己二醇酯,对其合成工艺条件进行了研究,得出了最佳工艺条件。并以所得聚酯合成了具有透明度高、硬度大、耐磨、玻璃化温度高等优异性能的聚氨酯材料。     

反相高效液相色谱法测定meso-四苯基卟啉钴的纯度

采用反相高效液相色谱法测定合成meso-四苯基卟啉钴的纯度;以甲醇乙腈二氯甲烷(体积比为55∶35∶10)为流动相,ShimpackCLCODS柱(150mm×6.0mmi.d,5μm)为分离柱,流速为1.5mL/min,检测波长420nm;meso四苯基卟啉钴的测定在1.0～10μg/mL时线性关系良好(相关系数r=0.9993),加标回收率为97.03%～101.42%,重复进样的相对标准偏差RSD为0.64%～2.92%(n=5)。方法的准确度高,精密度好,实际应用效果好。     

添加物对ZrO2系快离子导体烧结性能的影响

本文介绍了１３２０℃下，ＣａＯ，Ｙ２Ｏ３等稳定剂，低融物组成及１－６价阳离子化合物对ＺｒＯ２烧结性能的影响并列举出材料的晶型及某些主要性能。     

莫达非尼的绿色化学合成

采用[bm im]BF4离子液体作为反应溶剂,以二苯甲硫醇为原料,经醚化、氨解、氧化得到新型提神醒脑药物莫达非尼。讨论了不同的氯乙酸酯和反应温度对醚化反应收率的影响,讨论了不同的二苯甲硫乙酸酯对氨解反应收率的影响,及离子液体的回收使用。研究表明,采用氯乙酸甲酯作为醚化试剂,反应时间4 h,反应温度100℃,二苯甲硫醇∶氯乙酸甲酯=1∶1.5(摩尔比),室温下氨解反应20 h,二苯甲硫乙酰胺收率76%;采用过氧化氢作为氧化试剂,反应时间3 h,反应温度60℃,过氧化氢∶二苯甲硫乙酰胺=1∶1(摩尔比),莫达非尼收率79%,反应总收率可达48%。     

The influence of F doping on the activity of PbO2 film electrodes in oxygen evolution reaction

The PbO₂ and F⁻-doped PbO₂ (F-PbO₂) film electrodes have been prepared by an electrodeposition process onto platinum substrate. The changes of their electrochemical activity for oxygen evolution (OE) reaction with accelerated electrolysis time have been studied. The results show that the activity of the electrodes decreases with increasing electrolysis time. This can be attributed to the conductivity variations, which are caused by the decrease of the oxygen vacancy concentration in PbO₂ films during OE. The mechanism of the decrease of the oxygen vacancies has been investigated. For F-PbO₂ film electrodes, though its electrochemical activity is somewhat lower than that of undoped one, its activity stability is much higher in comparison with that of PbO₂. The influence of F⁻ doping on the activity of PbO₂ film electrodes has been also discussed.