甲磺胺磺隆合成方法述评

总结了文献报道的甲磺胺磺隆及其中间体的合成工艺路线和具体的合成方法。甲磺胺磺隆是由4-氰基甲苯或关键中间体N-叔丁基-2-甲氧羰基-5-甲基苯磺酰胺为原料经多步反应得到产品,主要有2条工艺路线。     

麦田除草剂丙苯磺隆在美上市

拜耳公司新型磺酰脲类(磺酰胺基羰基三唑啉酮类)麦田除草剂丙苯磺隆(通用名称：propoxycarbazonesodium，商品名称：Olympus)2004年7月30日在美上市。丙苯磺隆主要用于防除禾本科杂草如看麦娘、雀麦等和一些重要的阔叶杂草。为了扩大杀草谱，丙苯磺隆还可与2，4-滴，2甲4氯混用。(LCL)     

非异氰酸酯法合成豆田除草剂氯嘧磺隆

报道了以氯甲酸甲酯为起始原料合成豆田除草剂氯嘧磺隆的方法。原料邻乙氧羰基苯磺酰胺先与氯甲酸甲酯生成邻乙氧羰基苯磺酰胺基甲酸甲酯 ,再与 2 -氨基 - 4-氯 - 6 -甲氧基嘧啶反应生成氯嘧磺隆。避免了异氰酸酯路线的种种缺点 ,具有收率高、含量高、成本低的特点。以邻乙氧羰基苯磺酰胺计 ,总收率为 76 .7%,原药纯度达 92 .1 2 %。     

阿斯特拉捷利康公司把目标对准墨西哥和中国

2004年9月，冬小麦秋种期间，拜耳将谷物除草剂Olympus(丙苯磺隆70％)引入美国。丙苯磺隆已于6月30日获得EPA批准，这是继年初甲磺胺磺隆获得批准后，拜耳2004年在美国登记的第二个谷物除草剂。     

苯磺隆生产工艺评述

苯磺隆是一种重要的磺酰脲类旱田除草剂,是我国麦田防除阔叶杂草的当家品种。综述了苯磺隆及其关键中间体的主要生产工艺,并对各生产工艺在收率、质量、成本、安全环保等方面进行了比较和评价,指出了以邻甲酸甲酯苯磺酰氯、乙腈和氰酸钠为原料的工艺是苯磺隆的最佳生产工艺。     

三光气法合成磺酰脲类除草剂的研究

利用三光气代替光气合成磺酰脲类除草剂的新方法，用该方法成功地合成了噻磺隆和苯磺隆，其中噻磺隆收率83．3％，苯磺隆为85．4％，均以对应的磺酰胺计。噻磺隆和苯磺隆的合成稳定性结果表明．效果明显优于光气法。     

环丙嘧磺隆的合成路线

环丙嘧磺隆(Cyclosulfamuron)是一种新型的磺酰脲类超高效除草剂,祥述了Cyclosulfamuron及中间体的合成路线和收率。     

碘甲磺隆合成方法述评

总结了文献报道的碘甲磺隆的工艺合成路线和具体的合成方法。已知的碘甲磺隆的工艺合成路线主要有3条,对其中涉及到的关键中间体的合成路线和合成方法进行了总结。     

磺酰磺隆的合成

[目的]寻找具有工业化前景的除草剂磺酰磺隆的合成工艺。[方法]以2-氯咪唑[1,2-a]吡啶-3-磺酰胺为起始原料,先与乙硫醇钠反应合成2-乙硫基咪唑[1,2-a]吡啶-3-磺酰胺,再与双氧水反应合成2-乙磺酰基咪唑[1,2-a]吡啶-3-磺酰胺,最后与N-(4,6-二甲氧基嘧啶基-2-基)氨基甲酸苯酯反应合成磺酰磺隆。[结果]通过实验,确定了最佳路线,3步反应总收率68.1%,含量98.2%(HPLC)。[结论]该合成工艺具有步骤少、收率高、安全可靠的特点,可为工业化生产提供参考。     

甲酰氨基嘧磺隆的合成

甲酰氨基嘧磺隆是一种高效、广谱、低毒、高选择性的磺酰脲类除草剂。综述了甲酰氨基嘧磺隆的合成方法,并对其中一种合成路线进行了详细的研究。以对硝基甲苯邻磺酸为起始原料,经过中间体N,N-二甲基-2-氨基磺酰基-4-甲酰氨基苯甲酰胺制备甲酰氨基嘧磺隆。在优化的反应条件下,以对硝基甲苯邻磺酸计总收率可达34.5%。此工艺路线具有反应条件温和、产品纯度高、易于实现工业化生产等特点。     

Color-emotion associations in interiors

Emotional reactions to red, green, blue, and gray colors in a living room were investigated using a self-report measure. Participants first watched a short video of a 3D model of a living room. Next, they were asked to match the living rooms with facial expressions of six basic emotions. The most stated emotions associated for the red room were disgust and happiness, while the least stated emotions were sadness, fear, anger, and surprise; for the green room, neutral and happiness were the most stated emotions, and anger, surprise, fear, and sadness were the least stated ones; for the blue room, neutral was the most stated emotion, while the least stated emotions were anger and surprise. Neutral, disgust, and sadness were the most stated emotions for the gray room. Gender differences were not found in human emotional reactions to living rooms with different wall colors.     

In process monitoring of polymer batch to batch variation in injection moulding

Abstract

Injection moulding studies are reported, during which in process measurements have been used to monitor batch to batch variation of several production grade polymers. Three materials were studied: a polyamide 6, a polyacetal, and a flexible poly(vinyl chloride), all of which were commercial injection moulding polymers supplied by industrial collaborators. Instrumented high precision electric and servohydraulic moulding machines were used to mould parts in house from a number of different material batches. Moulding conditions were kept constant throughout and several process variables were monitored during injection, including melt pressure, melt temperature, and viscosity index –a specific pressure integral calculated from primary injection. Part weights were measured to provide an indication of part quality. Results showed that in each case, variations between batches produced a measurable effect on part quality. These variations were detected by in process measurements, particularly by viscosity index, which tracked significant changes in part weight. Several ‘problem’batches not identified by the compounder's internal quality checks were detected, and the influence of regrind and a development compound were also clearly identified. No simple relationship between viscosity index and part quality was observed for the limited processing range covered. Overall, the studies show the potential of in process measurements to provide a real time, sensitive indication of process variation.     

噻唑型偶氮分散染料合成研究

本文以2-氨基-4-氯-5-醛基噻唑为重氮组分合成了一系列含醛基分散染料,进而与合活泼亚甲基的化合物缩合得到一系列含氰乙烯基的分散染料.对染料结构进行了表征,并测试了染料的吸收光谱.结果表明氰乙烯基的引入使得λmax和εmax都有所增大.     

Changes in fatty acids and volatile components in mackerel by broiling

Mackerel is known to be a rich source of omega‐3 family PUFAs. The acid value and conjugated dienoic acid value of mackerel, known as indices of oxidation, were determined. Fatty acids in both raw and broiled mackerels were analyzed by GC. PUFAs and saturated fatty acids were observed at a low level in broiled mackerel, possibly as a result of thermal degradation of the lipids. In addition, volatile components in mackerel extracted by solvent‐assisted flavor evaporation were analyzed by GC‐MS. In total, 38 volatile components were detected in raw mackerel, whereas 53 volatiles were found in broiled mackerel. Hydrocarbons and methyl‐ and/or ethyl‐substituted benzenes were quantitatively dominant. Levels of aldehydes and alcohols were significantly enhanced in broiled mackerel, as was the level of benzothiazole, which possibly forms as a result of the condensation of thermal degradation products from amino acids and/or proteins, and lipids.     

喷动流化床流动形态变化的试验研究国家

在一个可视化的半圆柱喷动流化床试验台上研究了喷动流化床的流形变化规律。研究表明：随着喷动气量和流化气量的改变,床内会呈现不同的流动形态：固定床、带射流的流化床、喷动床、充气喷动床和喷动流化床。同时研究了量小喷动速度和最小喷动流化速度随喷动管内径、颗粒粒径、静止床高的变化规律,归纳了预测量小喷动速度和最小喷动流化速度的试验关联式,绘制了喷动流化床的流形划分相图。     

Transport property measurements in sheared granular flows

Experiments were performed in a shear cell device under four different solid fractions. The glass spheres with a mean diameter of 3 mm were used as granular materials. The motions of the granular materials were recorded by a high-speed camera. By using image processing technology and a particle tracking method, the average and fluctuation velocities in the streamwise and the transverse directions could be successfully measured and analyzed. Three bi-directional stress gages were used to measure the normal and shear stresses along the upper boundary. The effective viscosity of the granular material flow can be calculated. By tracking the movements of particles continually, the curves of the mean-square diffusive displacements versus time were plotted and were used to determine the self-diffusion coefficients from the slopes of the curves. The fluctuations and the self-diffusion coefficients in the streamwise direction were much higher than those in the transverse direction. The fluctuations were found to increase with the solid fraction, but the diffusion coefficients were greater in a more dilute flow system.     

Chemoattraction ofBiomphalaria glabrata (Gastropoda: Planorbidae) to lipid standards and lipophilic factors in leaf lettuce and Tetramin

Chemoattraction of individualBiomphalaria glabrata snails for lipid standards and lipophilic fractions of leaf lettuce and Tetramin were studied in a Petri dish bioassay. Snails were more significantly attracted to a whole Tetramin lipophilic fraction than that of leaf lettuce. Thin-layer chromatography showed that major neutral lipid fractions in Tetramin were triacylglycerols, free fatty acids, and free sterols, and in leaf lettuce were free fatty acids and a mixed free sterol-chlorophyll fraction. Snails were significantly attracted to both the free fatty acid and free sterol fractions from Tetramin, but only to the free fatty acid fraction from leaf lettuce. Snails were significantly attracted to a mixed lipid standard containing equal amounts of phosphatidylcholine, cholesterol, oleic acid, triolein, and cholesteryl oleate. Of four individual neutral lipid standards tested, i.e., cholesterol, oleic acid, triolein, and cholesteryl oleate, snails were only attracted to cholesteryl oleate.     

Synthesis,characterization, and application of hetarylazo disperse colorants: Preparation and properties of ink-jet inks with active agents for polyester printing

The synthesis and characterization of two hetarylazo disperse colorants are described. These compounds were used for the preparation of ink-jet inks with and without active agents for polyester printing. The viscosity, conductivity, surface tension, and pH of these inks were studied over a period of time and discussed with respect to their structure and the active agent content. The particle size and particle size distribution of a representative ink containing a new synthesized hetarylazo compound were measured. All the prepared inks were proved to be suitable for ink-jet printing in terms of their particle size. Viscosity , surface tension, conductivity, and pH values of all inks, with and without active agent, were monitored over a period of 90 days and were related to the ink stability. The same properties were measured for an ink preparation with a commercial dye for comparison. The inks containing the new synthesized dyes were found to be more advantageous regarding most of the above properties, i.e., surface tension, viscosity, and conductivity. Contrarily pH values of all the preparations were unacceptable for ink-jet inks. The ink compositions containing the new synthesized compounds were applied by exhaustion (dyed) on polyester fabric. Fastness properties of the dyed polyester samples were excellent to very good in most cases. Color measurements of the dyed fabric were also performed. A qualitative determination of the aroma-active agent adsorbed on the fiber by the exhaustion method was achieved by the GC-MS method. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Dispersion polymerization of vinyl acetate in a mixture of ethanol and water

Dispersion polymerization of vinyl acetate (VAc) was studied in a mixed solvent of ethanol and water using poly(vinyl alcohol) (PVA) with a low degree of hydrolysis as a steric stabilizer. Six compositions were chosen from a homogeneous phase before the polymerization. In a composition with the highest solubility parameter, 450 nm particles with a size distribution close to monodispersity were obtained. With decreasing solubility parameters of the compositions, the particles became polydisperse. In the compositions with solubility parameter lower than 17.1, particles were not formed even at 100 % conversion. Degrees of polymerization obtained in this homogeneous phase were less than 100 and close to calculated values. With increasing solubility parameters of the system, degrees of polymerization increased but were still less than 200. Grafting of VAc onto PVA and grafted PVA were very small, indicating the presence of a competing reaction to the grafting. Copyright © 2004 Society of Chemical Industry     

FoxO3a基因缺失致小鼠脾脏进行性慢性炎性反应的观察

目的观察FoxO3a基因缺失致小鼠脾脏进行性慢性炎性反应。方法分别于16周、24周和12个月称取FoxO3a基因敲除小鼠和对照小鼠体重;于16、24和38周处死各组小鼠,取脾脏,肉眼观察脾脏变化,并制备脾细胞悬液,进行细胞计数,同时取各组小鼠卵巢、肺及皮下等组织,观察其炎性变化。流式细胞术检测24周的FoxO3a基因敲除小鼠和对照小鼠脾细胞中T、B淋巴细胞和Mac-1+细胞数量及百分率;Real-time PCR检测脾细胞中炎性细胞因子S100A8和S100A9基因mRNA的表达水平。结果与对照小鼠相比,FoxO3a基因敲除小鼠脾脏明显肥大,且随年龄增加更加显著,卵巢、肺及皮下等组织内可见大量炎性细胞浸润,脾细胞数明显升高;基因敲除组老年小鼠的体重明显低于对照小鼠;FoxO3a基因敲除小鼠的脾细胞中T、B淋巴细胞数增加明显,但所占脾细胞的百分率无明显增加,Mac-1+细胞数和百分率均明显增加;S100A8和S100A9基因mRNA的表达水平明显高于对照小鼠。结论 FoxO3a基因缺失致小鼠脾脏进行性慢性炎性反应。