Using 30 percent hydrogen peroxide as the oxidant,the oxidation reaction of cyclohexanone to adipic acid catalyzed by Na2WO4·2H2O in the presence of acid ligands was investigated.The reaction follows the coordina...Using 30 percent hydrogen peroxide as the oxidant,the oxidation reaction of cyclohexanone to adipic acid catalyzed by Na2WO4·2H2O in the presence of acid ligands was investigated.The reaction follows the coordination catalysis mechanism.Both the acidity and the structure of the acid ligand had a notable effect on the catalytic ability of the catalytic system.By using sulfosalicylic acid as acidic ligand and the mole ratio of sulfosalicylic acid to Na2WSO4·2H2O was 1/1,the intermediate products of the catalytic oxidation reaction were analyzed by the GC-FTIR technique.the result showed that ε-caprolactone was the important stable intermediate product of the reaction.The possible mechanism was proposed.The cyclohexanone was oxidized by hydrogen peroxide to ε-caprolactone in the first step based on the Baeyer-Villiger oxidation mechanism,then the product from the rapid hydrolization of ε-caprolactone is oxidized to adipic acid.展开更多
江西南昌西汉海昏侯墓是近年来汉代考古的重要发现,其出土的大量珍贵文物为研究西汉列侯葬制、复原汉代社会生活提供了难能可贵的实物资料。其中墓园M1和M5棺内各出土了玻璃席,作为玉敛葬中的一种葬具,是西汉手工业水平的重要见证,也是...江西南昌西汉海昏侯墓是近年来汉代考古的重要发现,其出土的大量珍贵文物为研究西汉列侯葬制、复原汉代社会生活提供了难能可贵的实物资料。其中墓园M1和M5棺内各出土了玻璃席,作为玉敛葬中的一种葬具,是西汉手工业水平的重要见证,也是列侯丧葬等级和汉代法赙制度的具体表征。本研究使用傅里叶变换显微红外光谱(micro-FTIR)、热裂解气相色谱-质谱分析(Py-GC/MS)以及基于质谱的动物考古学技术(zooarchaeology by mass spectrometry,ZooMS)等多种手段,对海昏侯墓出土玻璃席包边及疑似胶结材料进行了科学分析。首先利用傅里叶变换显微红外光谱确定样品中均含有蛋白质成分,再利用热裂解气相色谱质谱技术检测包边残留物和疑似胶结材料的主要成分,判断包边样品应为动物性来源,最后使用基于质谱的动物考古学技术,确定了M1刘贺墓玻璃席包边残留物的生物来源为普通牛,推测包边残留物材料为牛皮。包边样品中检测到的少量酚类物质,表明牛皮在鞣制过程中可能使用了植物鞣剂。样品中含量较高的脂肪酸类物质可能来源于皮革鞣制中的加脂处理。此外,两件胶结材料样品中含有吲哚类、脯氨酸类化合物以及磷酸三甲脂,但未发现胆固醇类化合物,判断胶结材料应为蛋清。本研究明确了玻璃席包边制作材料,为了解古代制席工艺、制作技法提供了科学认知,两张玻璃席制作精美、工艺复杂,展现了西汉中期高超的制席工艺,为后续针对玻璃席开展的保护修复工作提供了重要参考依据。展开更多
文摘Using 30 percent hydrogen peroxide as the oxidant,the oxidation reaction of cyclohexanone to adipic acid catalyzed by Na2WO4·2H2O in the presence of acid ligands was investigated.The reaction follows the coordination catalysis mechanism.Both the acidity and the structure of the acid ligand had a notable effect on the catalytic ability of the catalytic system.By using sulfosalicylic acid as acidic ligand and the mole ratio of sulfosalicylic acid to Na2WSO4·2H2O was 1/1,the intermediate products of the catalytic oxidation reaction were analyzed by the GC-FTIR technique.the result showed that ε-caprolactone was the important stable intermediate product of the reaction.The possible mechanism was proposed.The cyclohexanone was oxidized by hydrogen peroxide to ε-caprolactone in the first step based on the Baeyer-Villiger oxidation mechanism,then the product from the rapid hydrolization of ε-caprolactone is oxidized to adipic acid.
文摘江西南昌西汉海昏侯墓是近年来汉代考古的重要发现,其出土的大量珍贵文物为研究西汉列侯葬制、复原汉代社会生活提供了难能可贵的实物资料。其中墓园M1和M5棺内各出土了玻璃席,作为玉敛葬中的一种葬具,是西汉手工业水平的重要见证,也是列侯丧葬等级和汉代法赙制度的具体表征。本研究使用傅里叶变换显微红外光谱(micro-FTIR)、热裂解气相色谱-质谱分析(Py-GC/MS)以及基于质谱的动物考古学技术(zooarchaeology by mass spectrometry,ZooMS)等多种手段,对海昏侯墓出土玻璃席包边及疑似胶结材料进行了科学分析。首先利用傅里叶变换显微红外光谱确定样品中均含有蛋白质成分,再利用热裂解气相色谱质谱技术检测包边残留物和疑似胶结材料的主要成分,判断包边样品应为动物性来源,最后使用基于质谱的动物考古学技术,确定了M1刘贺墓玻璃席包边残留物的生物来源为普通牛,推测包边残留物材料为牛皮。包边样品中检测到的少量酚类物质,表明牛皮在鞣制过程中可能使用了植物鞣剂。样品中含量较高的脂肪酸类物质可能来源于皮革鞣制中的加脂处理。此外,两件胶结材料样品中含有吲哚类、脯氨酸类化合物以及磷酸三甲脂,但未发现胆固醇类化合物,判断胶结材料应为蛋清。本研究明确了玻璃席包边制作材料,为了解古代制席工艺、制作技法提供了科学认知,两张玻璃席制作精美、工艺复杂,展现了西汉中期高超的制席工艺,为后续针对玻璃席开展的保护修复工作提供了重要参考依据。
