Kinetics for benzoylation of sodium 4-acetylphenoxide via third-liquid phase in the phase-transfer catalysis

In this research, the kinetics for synthesizing 4-acetylphenyl benzoate (R^*COOR) from benzoylation of sodium 4-acetylphenoxide via third-liquid phase-transfer catalysis was investigated. The reaction rate was observed to be strongly dependent on agitation speeds in the third-phase catalytic reaction. By forming the third-liquid phase, the observed reaction can be greatly enhanced to give a product yield of 100% in a duration of 3 min at 20 °C and 200 rpm. If a third-liquid phase was not formed in the liquid–liquid system, the reaction rate is very slow and the product yield is only 2% in 3 min at 20 °C. The reaction conducted in third-liquid phase-transfer catalytic system is faster than that in LLPTC system by 25–28 times. The amount of catalytic intermediate (QOR) in the third-liquid phase was about 50% of the catalyst initially added and kept about 30% of it remained after 1 min, and only small amounts of a catalytic intermediate residing in the organic phase were observed during the reaction using methyl t-butyl ether as the solvent. The concentration of catalytic intermediate slightly decreased with increasing reaction time, while the molar ratio of QOR to benzyl tri-n-butylammonium cation in the third-liquid phase remained almost constant after 1 min and increased with increasing agitation speeds. The experimental results were well described by the pseudo-first-order kinetics. The present work shows an effective method to synthesize 4-acetylphenyl benzoate.     

SiC晶须对Si3N4陶瓷基复合材料机械强度的影响

制备了含10vol％,20vol％及30vol％SiC晶须的Si_3N_4基复合材料,对其室温及高温机械强度的测试研究表明,SiC晶须对基体的高温机械性能有明显的增强作用。含20vol％SiC晶须的复合材料1200℃下强度达780MPa,比基体材料提高50％。通过SEM和TEM研究,讨论了SiC晶须增强的原因。     

洗涤剂用4A沸石工业的回顾及展望

4A沸石具有软化水质的作用，是全球公认的优良的代磷助剂。介绍了洗涤剂用4A沸石在世界各地的发展历程和现状，指出了国际洗涤剂用4A沸石的发展趋势，并就国内洗涤剂用4A沸石提出了发展建议。     

CaSO_4晶须对聚氨酯胶粘剂性能影响的研究

用实验室自制的相对分子质量为2500的聚己二酸-1,4-丁二醇酯二醇和甲苯二异氰酸酯、混合扩链剂配制聚氨酯胶粘剂,并使用实验室自制的改性和未改性200nm硫酸钙晶须对聚氨酯胶粘剂进行改性,考察不同硫酸钙晶须及其加入量、加入方式对聚氨酯胶粘剂综合力学性能的影响。根据实验结果,200nm改性硫酸钙晶须当加入量为3％时,聚氨酯胶粘剂的拉伸强度、初粘性和最终剥离强度均有明显提高。     

[Cu_2(Gly—GlyO)_2(OH)_2(4,4—bpy)]·9H_2O配合物合成、晶体结构研究

采用Gly—GlyOH,4,4＇—联吡啶与Cu(NO_3)_2·H_2O在二次水溶液中反应,合成出以4,4＇—bpy为中继基,Gly—Glyo为螯环新型双核铜配合物。经X射线单晶结构分析确定该配合物品体的化学结构式:[(H_2NCH_2CONHCH_2COO) Cu(OH) (C_(10)H_8N_2)Cu(OH) (H_2NCH_2CONHCH_2COO)]·9H_2O.晶体属于三斜晶系,P_空间群,晶胞参数a=1.1412nm,b=1.2298nm,C=1.4269nm,α=113.82°,β=101.91°,y=103.64°,V=1.6747nm~3,Z=2。衍射数据是在Nicolet XRD R3型四圆衍射仪上收集,结构参数经块矩阵最小二乘法精修后,最终一致性因子R值为0.068,RW值为0.057。     

Electrochemical performance of nanocrystalline Li3V2(PO4)3/carbon composite material synthesized by a novel sol–gel method

A novel sol–gel method based on V₂O₅·nH₂O hydro-gel was developed to synthesize nanocrystalline Li₃V₂(PO₄)₃/carbon composite material. In this route, V₂O₅·nH₂O hydro-gel, NH₄H₂PO₄, Li₂CO₃ and high-surface-area carbon were used as starting materials to prepare precursor, and the Li₃V₂(PO₄)₃/carbon was obtained by sintering precursor at 750 °C for 4 h in flowing argon. The sol–gel synthesis ensures homogeneity of the precursors and improved reactivity. The sample was characterized by XRD, SEM and TEM. X-ray diffraction results show Li₃V₂(PO₄)₃ sample is monoclinic structure with the space group of P2₁/n. The TEM image indicates that the Li₃V₂(PO₄)₃ particles modified by conductive carbon are about 70 nm in diameter. The Li₃V₂(PO₄)₃/carbon system showed that the discharge capacities in the first and 50th cycle are about 155.3 and 143.6 mAh/g, respectively, in the range of 3.0–4.8 V. The sol–gel method is fit for the preparation of Li₃V₂(PO₄)₃/carbon composite material which may offer some favorable properties for commercial application.     

Electrochemical and surface-enhanced Raman spectroscopy studies of 4-phenylpyridine adsorption at the gold/solution interface

The adsorption of 4-phenylpyridine (4-PhPy) on the Au electrode was examined using conventional electrochemical techniques: cyclic voltammetry and impedance measurements and also by surface enhanced Raman spectroscopy (SERS) in a wide range of electrode potentials. Electrochemical results indicate the strong adsorption of 4-Phpy molecules, particularly at the positively charged Au electrode. The wide shoulder of capacity close to the pzc suggests that the composition and/or the structure of 4-Phpy monolayer change with the sign of the surface charge on the electrode. Investigation of integrity of adsorbed layer, however, indicates that adsorbed molecules do not form tight, compact monolayer even in the case of adsorption from saturated solution. SERS spectra provided evidence for gradual, potential-induced reorientation of the molecular plane with respect to the surface, from nearly vertical in the negatively charged electrode, to more flat at the positively charged metal surface.