4-甲氧基-N-苯基-N-(4-(2,2-二苯乙烯基)苯基)苯胺的合成

在氮气保护下,以二苯胺、对碘苯甲醚和二苯基氯甲烷为原料,经过Ullmann反应、Vilsmeier-Haack反应和Wittig反应,合成了电荷传输材料4-甲氧基-N-苯基-N-(4-(2,2-二苯乙烯基)苯基)苯胺,收率达到20.1%,通过熔点、红外光谱、核磁共振谱等手段确证了所合成化合物的结构。该合成工艺具有反应温度低,反应时间短,制备简单的优点,并优化了反应条件。并用紫外光谱、荧光光谱测试了其光谱性质。     

N-苯基-3-氯-6-(3,5-二甲基-1-吡唑基)吡啶-2-甲酰胺及3-氯-6-(3,5-二甲基-1-吡唑基)吡啶-2-甲酸的合成和表征

以3,6-二氯吡啶-2-甲酸为原料经过酰胺化、肼取代、环合、水解等反应合成了标题化合物,并通过红外光谱、核磁共振谱和质谱对其结构进行了表征.     

2,2′-联吡啶-4-甲酸甲酯的合成

以2-乙酰基吡啶为起始原料,经过烃化、 Krhnke反应得到目标化合物,总收率为62.2%。由核磁共振氢谱和质谱对产物进行了结构表征。该方法具有反应条件温和、收率高、易于纯化的特点,为2,2′-联吡啶-4-甲酸甲酯的合成提供了新途径。     

固体光气法合成2-氧-5-甲基-3-氢-1,3,4-噁二唑

研究了以乙酸乙酯为原料,用固体光气代替光气合成2-氧-5-甲基-3-氢-1,3,4-噁二唑,为该中间体的合成提供了一条环境友好的新途径。考察了反应温度、反应物配比、反应溶剂等因素对收率的影响,在最佳条件下,合成总收率为81．8％。目标化合物经红外光谱、核磁共振谱、质谱验证。     

2-甲基-5-取代苯硫基-1,3,4-噻二唑的合成研究

以取代碘苯和2-巯基-5-甲基-1,3,4-噻二唑为原料,合成了一系列2-甲基-5-取代苯硫基-1,3,4-噻二唑类化合物,确定最佳合成条件为:以碘化亚铜作催化剂、2-吡啶甲酸作配体,于70～80℃在二甲基亚砜中反应24～36h。目标化合物结构经核磁共振氢谱、核磁共振碳谱、红外光谱、质谱分析确证。     

固体光气法合成2-氧-5-甲基-3-氢-1,3,4一噁二唑

研究了以乙酸乙酯为原料,用固体光气代替光气合成2-氧-5-甲基-3-氢-1,3,4-(口恶)二唑,为该中间体的合成提供了一条环境友好的新途径。考察了反应温度、反应物配比、反应溶剂等因素对收率的影响,在最佳条件下,合成总收率为81.8%。目标化合物经红外光谱、核磁共振谱、质谱验证。     

N-丙基-4-哌啶酮的合成研究

以丙烯酸甲酯和丙胺为原料，经过Michael加成，Dieckmann缩合和水解脱羧反应，简便、高效地合成了N-丙基-4-哌啶酮。分别对原料配比、合成过程等方面进行了改进，简化了合成工艺，节省了原料和成本，更适合于大规模生产。产品经过核磁氢谱检测表征，而且也经过气相色谱检测，具有很高的纯度。     

环境荷尔蒙类物质2,4-二氯酚人工抗原的合成与表征

以环境荷尔蒙类物质2,4-二氯酚、对氨基苯甲酸等为起始原料,经重氮化反应合成了2,4-二氯酚半抗原。再经过混合酸酐法与载体蛋白BSA,成功合成了2,4-二氯酚人工抗原,为其免疫分析方法的建立提供了条件。产物经红外光谱、紫外光谱和核磁共振鉴定分析确定。     

1-苄基-5-苯基吡咯烷-2,3-二酮的高效合成研究

在浓硫酸作用下,不饱和酮酰胺发生分子内的氮杂Michael反应,高效地合成了1-苄基-5-苯基吡咯烷-2,3-二酮。考察了反应发生的条件,确定了反应的最佳条件。该化合物的结构已经通过氢谱,碳谱和质谱确定。     

3,3′-二羟基-4,4′-联苯二甲酸的合成和表征

联苯二甲酸类化合物是很好的刚性桥联配体,可用于制备纳米多孔材料.设计了一条制备联苯二甲酸类新配体的合成路线,以4-氨基水杨酸为原料,经过4步反应最终合成了新配体3,3′-二羟基-4,4′-联苯二甲酸,并通过红外光谱、核磁共振氢谱和元素分析进行了表征.     

Effect of coupon geometry and preload on flexural properties of oxide ceramic matrix composites

Oxide ceramic matrix composites (O-CMCs) have a high potential for usage in thermal protection systems or combustion chambers because of their low weight, temperature- and corrosion stability as well as non-brittle failure behavior. Mechanical property changes over their lifetime due to operational loads are not well understood. Moreover, mechanical properties from planar samples under laboratory conditions often differ substantially from upscaled components with complex geometries. In this work, the influences of curvature and preloading conditions were investigated experimentally using modeling to determine boundary conditions. Effects of curvature and trends among preload conditions were determined, with high-cycle-fatigue-preload (HCF) reducing strength and Young’s Modulus by 15% compared to their original values where low-cycle-fatigue-preload (LCF) had smaller effect. The low impacts of high temperatures and small-to-medium loads on the properties of O-CMCs makes them an interesting choice for high-temperature combustive environments.     

二乙酰二茂铁与氨基酸的Mannich反应

使用三氯甲烷做溶剂 ,三氯化铝做催化剂的条件下合成了 1 ,1′-二乙酰基二茂铁 ,并初步探讨了其与谷氨酸 ,苯丙氨酸的曼尼希反应 (Mannich)条件 ,制备了 2种二乙酰基二茂铁衍生物     

[bmim]PF_6增塑PVC糊树脂膜迁移规律研究

文章应用固相萃取、液相色谱联用技术,研究了[bmim]PF6增塑PVC糊树脂膜中的[bmim]PF6在水环境及低酒精含量模拟溶剂（15%乙醇-水溶液）中的迁移规律,同时研究了[bmim]PF6迁移对薄膜力学性能的影响。结果表明：时间和温度对[bmim]PF6向水环境中迁移均有加速效应,在中性条件下迁移量较小,在酸性和碱性条件下迁移量较大。[bmim]PF6在低酒精含量模拟溶剂中与浸泡在去离子水中的薄膜迁移量相比,迁移量明显降低。增塑剂迁出后PVC糊树脂膜的断裂伸长率降低,弹性模量、拉伸强度均升高,可望用于医疗制品的开。     

Developments in the deprotection of thioacetals

Dithioacetals are very important and commonly used protecting groups for carbonyl compounds. Among the advantages of their use are the ease of formation, stability under both acidic and basic conditions, and umpolung reactivity. Unfortunately, their deprotection into the corresponding carbonyls is quite often difficult and requires special conditions. Hence, numerous protocols for the dithiane deprotection have been devised. In this review, various methodologies that were developed for the hydrolysis of thioacetal protecting groups are summarised and the detailed reaction conditions are presented.     

金属铕配合物的合成及其晶体结构

合成了席夫碱N-亚水杨基-2-氨基吡啶,并以此为有机配体与过渡金属铕反应,得到了相应的配合物,且在一定的条件下培养得到配合物的单晶,解析出其晶体结构,并对其进行了荧光性质研究。     

不同条件下两种纤维增强MC聚酰胺复合材料摩擦磨损性能研究

制备了单体浇铸聚酰胺（MCPA）、纤维质量占比30 %的玻璃纤维增强MC聚酰胺（GFMCPA）及体积占比35 %的碳纤维增强MC聚酰胺（CFMCPA），分别将3种材料在干摩擦、洁净水、干砂、水砂4种不同摩擦条件下进行摩擦磨损性能实验，并对实验结果进行对比分析。结果表明，干摩擦及洁净水条件下，CFMCPA的摩擦因数（f_CF）f_GF）f_MC）；干砂及水砂条件下，f_MC<f_CF<f_GF；3种材料在不同摩擦条件下的摩擦因数排序均为：洁净水条件下的摩擦因数（f_W）<水砂条件下的摩擦因数（f_WS）<干摩擦条件下的摩擦因数（f_D）<干砂条件下的摩擦因数（f_DS）；不同材料在4种摩擦条件下的体积磨损率排序均为：干摩擦条件下的磨损率（W_D）<洁净水条件下的磨损率（W_W）<水砂条件下的磨损率（W_WS）<干砂条件下的磨损率（W_DS）；不同摩擦条件下3种材料的体积磨损率排序均为：GFMCPA的磨损率（W_GF）W_CF）W_MC）；4种条件下，各材料的摩擦磨损性能各有高低，可以根据具体的性能要求，选择使用。     

Characterization of zinc–nickel alloys obtained from an industrial chloride bath

Zinc–nickel electrocoatings obtained from an industrial bath containing two additives were characterized by analysing their morphology, structure, microhardness, residual stress and corrosion resistance. Changes in deposit characteristics following the addition of saccharin were also studied. All coating, with or without saccharin, presented a good appearance, good mechanical properties and a high corrosion resistance. Moreover, by varying certain plating conditions it was observed that the deposits maintained their properties over a wide interval of experimental conditions, which suggests their suitability for use in batch bath.     

Influence of Preparation Conditions of Alumina‐Based Refractory on the Morphological Parameters of Surface Defects

The surface defects on alumina‐based refractory arising from thermal shock were studied using image analysis and statistical tools. Alumina‐based refractory specimens were prepared by adding a different amount of fibers into their original composition and compacted on different pressures. Obtained specimens were subjected to thermal shock, and induced surface defects were characterized by their morphological parameters determined using the image analysis procedure. The influence of preparation conditions on the surface defects morphology was studied using principle component analysis. It was shown that morphological parameters of defects vary corresponding to the composition and preparation conditions of ceramic material.     

低温对化妆品及其包装的影响研究

化妆品通常会有两年以上的货架期,货架或仓储的温度环境因时而异,北方市场冬天的储存温度甚至会低至-30℃。为了考察化妆品在恶劣条件下可能发生的变化,抽取了市场上三个大众化的化妆品品牌,通过试验验证,得到低温下导致不同产品因膨胀造成包装瓶破裂的条件,为开发适应北方严寒气候的产品提供积极参考。     

Investigating the Commercial Microwave Vacuum Drying Conditions on Physicochemical Properties and Radical Scavenging Ability of Thai Green Tea

The effects of drying conditions using a commercial microwave vacuum dryer on the physicochemical properties and antioxidant activity of Thai green tea were investigated. Nine different drying conditions (power 3200, 3600, and 4000 Watts vs. radiation time 20, 25, and 30 min) were applied in this study. The results showed that individual catechins, their total quantities, radical scavenging ability, and moisture content were significantly affected; however, total polyphenol content and color parameters were not significantly affected by these drying conditions. Based on this data, to obtain optimal physicochemical properties of green tea, drying conditions at 3600 Watts for 30 min were recommended.