Facile one-pot synthesis of novel dicyanoanilines fused to tetrahydro-4H-thiopyran-4-one ring via Et3N/H2O catalyzed pseudo four-component reaction

A facile procedure is developed for one-pot synthesis of a new group of dicyanoanilines. Tetrahydro-4H-thiopyran-4-one, 1, undergoes a pseudo four-component reaction with various aldehydes bearing different groups and two equivalents of malononitrile in aqueous media in the presence of triethylamine (Et₃N). As a result, novel thiopyran-fused dicyanoanilines 4 are formed efficiently in the reaction mixtures in 90–97% yield within 9–12?h mixing at 40°C. Due to the polarity of the medium, products precipitate in the mixture spontaneously allowing for easy purification by recrystallization avoiding cumbersome chromatographic separations. Characterization of the products was performed by spectroscopic methods and, in one case, was further supported by X-ray crystallographic experiments.     

锌-锡液态金属碳气化反应的实验研究

液态金属气化技术是一种清洁的气化技术。因其原料适应性广,反应系统架构简单,适用于以固体碳为基础的分布式能源供给。反应过程中空气中的氧元素与熔融态的金属床料反应生成金属氧化物,再由碳原料还原氧化物生产含CO的产品气。为提高产品气中CO的比例,系统中引入了氧化锌(ZnO)以促进CO的生成。程序控温气化反应测试结果表明,氧元素由氧化锌向碳的迁移过程是气化反应的控制步骤,拓展熔池内部氧元素迁移路径,强化氧元素由氧化锌向碳的迁移过程是提高液态金属气化速率的重要途径。碱金属碳酸盐(Na_2CO_3,K_2CO_3)在高温下形成熔融态的氧传导路径,使得由氧化锌到碳原料的氧传导得到增强,改善了煤气化的反应特性。对不同碱金属碳酸盐的实验结果表明,具有较高氧离子传导率的碳酸盐能够使得熔体具有更好的煤气化特性。采用两种碳酸盐混合物制成的低熔点碳酸盐体系能够在较低温度(约720℃)时发挥氧离子传导的作用,促进气化反应在低温状态下的发生。     

太阳能行业含氟废水处理工程实例

浙江某太阳能企业在生产过程中排放含氟废水,废水量为2 000 m3/d,F-浓度为300～500 mg/L。采用两级反应沉淀方法,第一级采用钙盐沉淀,第二级采用铝盐沉淀,出水F-浓度降至10 mg/L以下,达到《污水综合排放标准》(GB 8978—1996)的一级排放标准,为企业解决了环保问题。     

Prediction of interfacial reaction products between metals with same lattice structure through thermodynamic modeling

Interfacial reactions exert crucial effect on the performance of soldering joints. Prediction of the first phase formed at the interface between metals benefit the design of electronic packaging. Based on our previous work, a new scheme is developed in this paper, which aims at predicting phase formation of the interface reaction between metals with the same lattice structure. In the new scheme, the conventional principle considering both the thermodynamic and kinetic factors is employed. A criterion is introduced for the case where a spinodal decomposition exists in the starting solution when the local equilibrium assumption is still valid. Another new criterion involving only nucleation driving force and entropy change is proposed for the case where no spinodal decomposition occurs and the assumption of local equilibrium is no longer valid. The validity of these criteria has been confirmed when applied to predict the intermetallic compound (IMC) formed in the binary diffusion couples such as Al/Cu, Al/Pt, Al/Au, and Co/Zn.     

新型绿色Knoevenagel反应进展

Knoevenagel反应在有机化学中是很重要的一类缩合反应,能够在活泼亚甲基和羰基之间脱水形成碳碳双键,广泛应用于合成以及一锅法串联反应,在过去一直是有机化学家研究的热点。发展至今,很多关于Knoevenagel反应的研究都已经打破了传统有机化学的实验形式和反应条件。针对最近新发展的,符合绿色化学要求的新型Knoevenagel反应进行简单介绍。     

Influence of inoculum and climatic factors on the severity of Fusarium head blight in German spring and winter barley

Fusarium head blight (FHB) of small cereals is a disease of global importance with regard to economic losses and mycotoxin contamination harmful to human and animal health. In Germany, FHB is predominantly associated with wheat and F. graminearum is recognised as the major causal agent of the disease, but little is known about FHB of barley. Monitoring of the natural occurrence of FHB on Bavarian barley revealed differences for individual Fusarium spp. in incidence and severity of grain infection between years and between spring and winter barley. Parallel measurement of fungal DNA content in grain and mycotoxin content suggested the importance of F. graminearum in winter barley and of F. langsethiae in spring barley for FHB. The infection success of these two species was associated with certain weather conditions and barley flowering time. Inoculation experiments in the field revealed different effects of five Fusarium spp. on symptom formation, grain yield and mycotoxin production. A significant association between fungal infection of grain and mycotoxin content was observed following natural or artificial infection with the type B trichothecene producer F. culmorum, but not with the type A trichothecene-producing species F. langsethiae and F. sporotrichioides. Trichothecene type A toxin contamination also occurred in the absence of significant damage to grain and did not necessarily promote fungal colonisation.     

树脂催化重汽油烷基化硫转移的动力学研究

采用树脂催化剂,研究重汽油中噻吩类硫化物的烷基化硫转移性能,分析反应前后硫分布的变化,并对反应动力学进行研究。结果表明,在反应温度110℃和反应时间60 min条件下,烷基化硫转移率大于90%,其反应动力学为一级反应速率方程,反应活化能为20.32 kJ·mol~(-1),指前因子为1 364 h~(-1),噻吩类硫化物烷基化反应的动力学方程可表示为:r=1364exp(-2.445×10~3/T)c_T。     

基于铜粉的室温气固反应自生长刺球状半导体Cu_2S纳米线阵列

本研究通过简单的气-固硫化反应对ITO玻璃上涂覆的铜颗粒膜进行硫化反应,得到了大面积的自生长刺球状结构的半导体Cu2S纳米阵列。采用SEM,TEM,EDS、XRD,以及UV-vis等方法对反应生长的半导体Cu2S纳米线阵列的微观结构及光吸收性能进行了系统研究。实验结果表明,合成的Cu2S为刺球状纳米线阵列,纳米刺球的直径分布在50~100μm之间;刺球上的纳米线为单斜晶系的Cu2S单晶,晶体生长方向为[-102];纳米线的平均直径为100nm,长度分布在20~50μm之间。合成的刺球状纳米线阵列具有良好的光吸收性能,反应20小时样品在可见光波长范围内(400~800nm)平均光吸收率达到了93%;反应30小时样品在可见光波长范围内(400~800nm)平均光吸收率达到了92%。同时两种刺球状纳米线阵列结构对于大的光线入射角仍然保持很高的光吸收性能,对光线入射角的变化不敏感。当入射光角度从0°增加到60°时,光吸收率仅下降3%,明显优于文献已报道的规则排列纳米线阵列的光吸收性能。本项研究合成方法简单,工艺可控,成本低,可以采用更广的基体材料。合成的纳米结构具有优良的综合光吸收性能,在光电领域有很好的应用潜力。     

Effect of Bicarbonate Salts and Sequential Using of Frying Oil on Acrylamide and 5-Hydroxymethylfurfural Contents in Coated Fried Chicken Meat

In this research, the effect of different bicarbonate salts (sodium and ammonium) and their doses (0, 1, 2, and 3 g/100 g raw material) in the coating batter formula use and the sequential use of frying oil (1st, 2nd, 3rd, and 4th) on 5-hydroxymethylfurfural and acrylamide contents in coated fried chicken meat. The addition of sodium bicarbonate was efficient for reducing acrylamide content, but it increased browning and 5-hydroxymethylfurfural content compared to the control. When increasing the doses of sodium and ammonium bicarbonate from 1 to 3 g/100 g of raw material, the acrylamide content of samples did not change significantly, although adding sodium bicarbonate significantly reduced the acrylamide content as a control. These research results showed that using about 1 g/100 g raw material sodium bicarbonate rather than ammonium bicarbonate and as little frying oil as possible use during the production of coated and fried meat results in lower contents of 5-hydroxymethylfurfural and acrylamide.     

Effect of Mo on microstructure and mechanical properties of bulk nanocrystalline Fe3Al materials prepared by aluminothermic reaction

Abstract

Bulk nanocrystalline Fe₃Al based materials with 5, 10 and 15 wt-%Mo were prepared by aluminothermic reaction. The microstructure and mechanical properties of the materials were investigated. It was shown that the materials consisted of a nanocrystalline matrix phase that was composed of Fe, Al and Mo and a little Al₂O₃ contamination phase. The nanocrystalline phase had a disordered bcc crystal structure. Average grain sizes of the nanocrystalline phase of the materials with 5, 10 and 15 wt-%Mo were 19, 31 and 24 nm respectively and that of the material with 5 wt-%Mo was the smallest. The materials with 10 and 15 wt-%Mo exhibited brittle behaviour in compression, whereas the material with 5 wt-%Mo had a large plastic deformation. The material with 5 wt-%Mo had the highest bending strength and the lowest compressive yield strength.