媒体头条概览

<正>《化学建材》06/20093,5-二叔丁基羟苯甲酸正丁酯的合成及其对HDPE的热氧老化性能研究以3,5-二叔丁基-4-羟基苯甲酸和正丁醇为原料,采用酯化反应,合成了抗氧剂3,5-二叔丁基-4-羟基苯甲酸正丁酯,并通过测定熔点、红外光谱和核磁共振谱对其结构进行表征。制备了抗氧剂3,5-二叔丁基-4一羟基苯甲     

3,4-二羟基苯甲酸乙酯合成工艺研究

以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影响,以及酯化反应中催化剂TsOH用量、乙醇用量、反应时间和反应温度对3,4-二羟基苯甲酸乙酯产率的影响。在最优合成条件下,3,4-二羟基苯甲酸乙酯的产率可达90.5%。实验证明本合成方法提高了产率,降低了成本,具有较好的工业应用前景。     

含4-取代苯基4-羟基-丁-2-酮类衍生物对映异构体的HPLC手性分离研究

7个含4-取代苯基4-羟基-丁-2-酮类衍生物对映异构体首次在Chiralpak IA[淀粉-三(3,5-二甲基苯基氨基甲酸酯)]手性固定相上进行了拆分,通过考察不同流动相体系(正己烷/乙醇、正己烷/异丙醇、正己烷/二氯甲烷),以样品的分离度为重要依据(Rs>2)。分别以正己烷/二氯甲烷=70/30(V/V)和正己烷/异丙醇=97/3(V/V)为流动相体系统下,实现对样品外消旋体的分离,并对其催化产物的光学活性进行测定,ee值最高为79.5%。     

鹿心雪茶化学成分研究

采用硅胶柱色谱及HPLC等分离方法对鹿心雪茶正己烷提取物进行分离纯化,得到7个化合物,依据波谱数据分析鉴定它们的结构分别为:3,6-二甲基-2,4-二羟基苯甲酸甲酯(1)、2,4-二羟基-3-醛基-6-甲基苯甲酸甲酯(2)、羊角衣酸(3)、3β-羟基-5α,8α-过氧桥麦角甾-6,22(E)-二烯(4)、3β-羟基-5α,8α-过氧桥麦角甾-6,9,22(E)-三烯(5)、3β-羟基-5α-豆甾烷-4-烯-3-酮(6)、8α,11-elemodiol(7)。其中化合物6和7为首次从该植物中分离的到。     

2,6-二甲基-3,5-吡啶二甲酰腙衍生物的合成及与DNA的作用

本文以2,6-二甲基-1,4-二氢吡啶-3,5-二甲酸二乙酯为原料,通过氧化、肼解得到2,6-二甲基-3,5-吡啶二甲酰肼,该甲酰肼和芳香醛反应合成了4个2,6-二甲基-3,5-吡啶二甲酰腙衍生物,合成路线设计合理,反应条件温和,产率高,目标化合物的结构用氢谱和质谱进行了表征,通过EB竞争实验测定了它们与DNA的结合常数约为104左右,表明该类酰腙化合物可以与DNA发生作用。     

1,10-邻菲啰啉衍生物配体和对苯二甲酸构筑的镉配位聚合物

以3,5-二溴对羟基苯甲醛和1,10-邻菲啰啉-5,6-二酮反应生成(L)配体。以L为主配体,对苯二甲酸为辅配体采用混合溶剂热法合成了过渡金属有机化合物,[L.(1,4-bdc).Cd]n,对该配位聚合物进行了红外光谱分析,元素分析,X-射线单晶衍射分析,热失重分析。X-单晶衍射分析表明,配合物为三维网状超分子结构。     

基于液质联用技术的蒙药扑勒蒙化学成分分析与鉴定

针对蒙药扑勒蒙化学成分的快速分离与鉴定,采用液质联用技术对其乙醇提取物进行了研究,从中分离鉴定了11个化合物,其化学结构分别为咖啡酸、5,7,2’,4’-四羟基-6,5’-二甲氧基黄酮、槲皮万寿菊素、4’-羟基汉黄芩素、槲皮万寿菊素-4’-甲醚、5,6,3’-三羟基-7,4’-二甲氧基黄烷酮、圣草酚-7-甲醚、槲皮素-7-甲醚、樱花素、异樱花素和3,5-二羟基-7,4’-二甲氧基黄烷酮。     

固体酸SO_4~(2-)/TiO_2催化合成尼泊金庚酯工艺研究

以固体酸SO_4~(2-)/TiO_2作催化剂,不加有毒带水剂,利用过量正庚醇与水共沸,高温回流直接制备长链泥泊金正庚酯,反应时间短,后处理简单,是绿色环保的制备方法。并通过正交实验确定了最优合成条件:对羟基苯甲酸与正庚醇的摩尔比为1∶1.2,反应温度160℃,反应时间3 h,催化剂用量为对羟基苯甲酸的10%,产率可达92%以上。     

4-羟基邻苯二甲酸二甲酯的合成研究

4-羟基邻苯二甲酸二甲酯是合成N-羟基邻苯二甲酰亚胺的重要中间体,在有机合成中应用越来越广泛.该论文设计了4-羟基邻苯二甲酸二甲酯的合成新路线,该路线以邻苯二甲酸酐为原料,重氮化为关键步骤,经硝化、酯化、还原、重氮化和水解合成了4-羟基邻苯二甲酸二甲酯.此外,对其关键步骤的反应条件进行了探索,在优化的条件下总收率达34.4%.     

N-(4-羟基苯基)-乙酰胺的合成及表征

以4-甲氧基苯胺为原料,经乙酰化、去甲基化两步反应合成得到了目标产物N-(4-羟基苯基)-乙酰胺,并采用IR、1H NMR和13C NMR对产物结构进行了表征.探讨了乙酰化反应时催化剂Al Cl3用量、反应温度及反应时间对N-(4-甲氧基苯基)-乙酰胺产率的影响,以及去甲基化反应中催化剂TBAB用量、溴化氢用量、反应温度及反应时间对产物N-(4-羟基苯基)-乙酰胺产率的影响.在最佳合成条件下,N-(4-羟基苯基)-乙酰胺的产率可达94.1%.     

Analysis of the antioxidant butylated hydroxytoluene (BHT) in water by means of solid phase extraction combined with GC/MS

The antioxidant 3,5-di-tert-butyl-4-hydroxy-toluene (BHT) is widely used as an additive to increase the tenability of food and plastics. BHT is degraded to 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO) in mammals, as well as in the natural environment such as in water and soils. BHT-CHO has been studied extensively in terms of their potential toxicities. The present investigation was carried out to quantify BHT and BHT-CHO in river, ground, rain and drinking water obtained from several locations in Germany. Apart from the compounds mentioned above, 1,2-bis-(3,5-di-tert-butyl-4-hydroxyphenyl)ethane (2-BHT), which is a dimer of BHT, was also detected in the extracts of some ground water samples. The applied analytical method is based on solid phase extraction (SPE) to concentrate trace compounds from water samples followed by gas chromatography/mass spectrometry (GC/MS) of the extracts. A total of 51 of the respective water samples were used for extraction purposes and analyte recoveries were all > or = 80%. The determination limit for BHT was 5 ng l(-1) and for BHT-CHO 16 ng l(-1). The standard deviations for the analytical procedure were 6% for BHT and 10% for BHT-CHO. The use of the antioxidant BHT in Germany has resulted in water concentrations of 7-791 ng l(-1) in the rivers Rhine, Elbe, Main, Oder, Nidda and Schwarzbach. The degradation product BHT-CHO was also detected in the river water samples at concentrations between 29 and 223 ng l(-1). The concentrations of BHT measured in German rivers are lower compared to values measured in the USA and Japan 20 years ago. In ground water, levels for BHT varied from non-detectable up to 2156 ng l(-1) and for BHT-CHO from non-detectable up to 674 ng l(-1). Both compounds were also detected in rain water in Frankfurt/Main at a concentration of 1797 ng l(-1) for BHT and 59 ng l(-1) for BHT-CHO.     

丙烯酸酯-丙烯酸共聚物类聚羧酸高分子分散剂对聚丙烯中碳酸钙填料的分散效果研究

将丙烯酸丁酯-丙烯酸共聚物类分散剂处理过的碳酸钙添加到聚丙烯塑料中,通过电镜扫描观察到,碳酸钙均匀分布在树脂中.当丙烯酸丁酯与丙烯酸的摩尔比为1:1,添加量达3%时,可使含碳酸钙20%的聚丙烯塑料的拉伸强度由原来的18.20 MPa增加到25.2 MPa,缺u冲击强度由3.7kJ/m2增加到4.8 kJ/m2,断裂伸长率由8.7%增加到12.2%.     

高耐擦洗内墙涂料用苯丙乳液的研制

以甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸、丙烯酸乙酯、苯乙烯、多功能交联单体(LEG)、交联剂(LA28)及有机硅单体等为主要原料,通过特殊的乳液聚合工艺,制成高光、高硬、附着力强、耐候、耐水、耐洗刷性能极佳的内墙专用苯丙乳液。通过对其配制内墙乳胶漆后进行耐洗刷性能的检测,结果表明:该苯丙乳液配制的内墙涂料,耐洗刷次数是普通苯丙乳液的2～4倍。经过多次检测,当该乳液在涂料中含量为10%的时候,涂料耐擦洗次数可以达到2000次以上,最少的时候也要在1500次以上;当该乳液在涂料中含量为8%的时候,涂料的耐擦洗次数可以达到400次以上,有时甚至会超过600次。该苯丙乳液是做高PVC(颜料体积浓度)内墙乳胶漆的理想选择。     

Monitoring of the antioxidant BHT and its metabolite BHT-CHO in German river water and ground water

The behavior of anthropogenic polar organic compounds in ground water during infiltration of river water to ground water was studied at the Oderbruch area on the eastern border of Germany. Additionally, waste water sewage treatment works (STWs) discharging their treated waste water into the Oder River and rain water precipitation from the Oderbruch area were investigated. The study was carried out from March 2000 to July 2001 to investigate seasonal variations of the target analytes. Samples were collected from four sites along the Oder River, from 24 ground water monitoring wells located close to the Oder, from one rain water collection station, from two roof runoffs, and from four STWs upstream of the Oderbruch. Results of the investigations of the antioxidant 3,5-di-tert-butyl-4-hydroxy-toluene (BHT) and its degradation product 3,5-di-tert-butyl-4-hydroxy-benzaldehyde (BHT-CHO) are presented. BHT and BHT-CHO were detected in all samples of the Oder River with mean concentrations of 178 and 102 ngl(-1), respectively. BHT and BHT-CHO were also detected in effluent waste water samples from municipal STWs at mean concentrations of 132 and 70 ngl(-1), respectively. Both compounds are discharged into river water directly via treated waste water. In the rain water sample, 308 ngl(-1) of BHT and 155 ngl(-1) of BHT-CHO were measured. Both compounds were detected in roof runoff with mean concentrations of 92 ngl(-1) for BHT and 138 ngl(-1) for BHT-CHO. The median values of BHT and BHT-CHO in ground water samples were 132 and 84 ngl(-1), respectively. The chemical composition of ground water from parts of the aquifer located less than 4.5 m distant from the river are greatly influenced by bank filtration. However, wet deposition followed by seepage of rain water into the aquifer is also a source of BHT and BHT-CHO in ground water.     

An ATP luminescence method for direct toxicity assessment of pollutants impacting on the activated sewage sludge process

An ATP luminescence method was used to determine the toxicity of three reference toxicants to two sources of domestic activated sludge, and an activated sludge from a laboratory model plant. Repeatability in the ATP test was demonstrated for Cr (as K2Cr2O7), Zn (as ZnSO4 x 7H2O), and 3,5-dichlorophenol (3,5-DCP) using each source of activated sludge. The three sources of sludge showed sensitivity to Cr and 3,5-DCP, and insensitivity to Zn using the ATP luminescence method. Sludge source did not appear to effect test response. The toxic response to 3,5-DCP in model and domestic activated sludge was shown to be dependent on sludge solid concentration (measured as total suspended solids, gTSS(-1). It is recommended that a standard solids concentration is used during toxicity evaluation.     

一种新型沥青防水材料改性剂

介绍环境气候、工艺思路对沥青防水材料的影响，通过内配法、外掺法、吹制（氧化）沥青及主财配沥青的原料，达到改善沥青性能的方法；掺加高分子聚合物改性石油沥青的方法及改性性能。较详细介绍一种新的沥青改性剂，它的主要成份为乙烯丙烯酸正丁脂和甲基丙烯酸缩水甘油脂共聚物，通过与沥青之间产生化学反应达到对沥青改性的目的。     

萃取法去除油页岩干馏污水中酚类物质的研究

采用乙酸丁酯萃取油页岩干馏污水中的酚类物质,考察了pH、油水比、温度、搅拌强度、搅拌时间、萃取剂的重复使用次数对除酚效果的影响.试验结果表明,采用乙酸丁酯对油页岩干馏污水进行处理是可行的,其最佳处理条件为:pH值为6.50、油水比为1:5、温度为30～40℃、搅拌强度为200～300 r/min、搅拌时间为10～20 min,在此条件下平均除酚率可达90%以上.用乙酸丁酯萃取油页岩干馏污水,不但萃取时间短、除酚效率高,还为后续生化处理创造了条件.     

有机相变蓄热复合材料导热性能的实验研究

以膨胀多孔石墨(EG)和硅藻土(DI)这2种多孔矿物介质与硬脂酸丁酯(BS)有机相变材料制备了有机相变蓄热复合材料,并采用调制差示扫描量热方法(MDSC)测试了复合材料的导热系数,借助层状复合材料热传导模型分析了多孔矿物介质内部结构特征对复合材料导热性能的影响.结果表明:采用EG和BS制备的有机相变蓄热复合材料具有明显的层状结构,其压制方向的导热系数更接近于层状复合材料热传导模型c轴方向的导热系数;采用DI和BS制备的有机相变蓄热复合材料的导热系数接近层状复合材料热传导模型a-b平面方向的导热系数,即该复合材料内部具有非常好的连通性.多孔矿物介质对有机相变复合材料导热性能的增强效果不仅受多孔矿物介质导热系数的作用,而且还受到复合材料内部结构特征的影响.当复合材料在热传导方向上形成连通性结构时有利于上述增强效果;而当复合材料形成与热传导方向垂直的层状结构时则不利于上述增强效果,即使多孔矿物介质具有很高的导热系数也是如此.     

丁基橡胶压敏胶粘带的制备及其性能研究

以丁基橡胶为主要原料研制出了丁基橡胶压敏胶粘带,讨论了丁基橡胶、增黏剂、增塑剂和填料用量等对胶粘带性能的影响,研究了其对三元乙丙橡胶防水卷材接缝的粘结作用。     

Toxicity assessment of common xenobiotic compounds on municipal activated sludge: comparison between respirometry and Microtox

The toxicity of four xenobiotic compounds 3,5-dichlorophenol, formaldehyde, 4-nitrophenol and dichloromethane, representative of industrial wastewater contaminants was evaluated by a simple respirometric procedure set up on the basis of OECD Method 209 and by the Microtox bioassay. Very good reproducibility was observed for both methods, the variation coefficients being in the range of 2-10% for the respirometric procedure and 6-15% for Microtox, values that can be considered very good for a biological method. Comparison of EC(50) data obtained with the two methods shows that in both cases 3,5-dichlorophenol is more toxic than other compounds investigated and dichloromethane has a very low toxicity value. Intermediate EC(50) values were found for the two other chemicals, formaldehyde and 4-nitrophenol. Moreover, the Microtox EC(50) values are generally lower (except for dichloromethane) than the respirometric ones: these differences could be explained by the fact that the Microtox method uses a pure culture of marine species and, therefore, should not necessarily be expected to behave like a community of activated sludge bacteria. In conclusion, both methods can be usefully applied for toxicity detection in wastewater treatment plants but it is advisable to take into account that Microtox is more sensitive than respirometry in estimating the acute toxicity effect on the biomass operating in the plant.