A new energetic complex, Ni（3,4＇-Hbpt）2（Hoba）2（H20）2 （3,4＇-Hbpt = 3-（3-pyridyl）- 5-（4＇-pyridyl）-l-H-l,2,4-triazole and H2oba = 4,4＇-oxybis（benzoic acid））, has been synthesized by hydrothermal reactio...A new energetic complex, Ni（3,4＇-Hbpt）2（Hoba）2（H20）2 （3,4＇-Hbpt = 3-（3-pyridyl）- 5-（4＇-pyridyl）-l-H-l,2,4-triazole and H2oba = 4,4＇-oxybis（benzoic acid））, has been synthesized by hydrothermal reaction and characterized by elemental analysis, IR spectroscopy, single-crystal X-ray diffraction, thermogravimetric analyses and X-ray powder diffraction. Single-crystal X-ray diffraction analysis indicates that the complex belongs to the monoclinic system, space group P2j/c with a = 10.2357（9）, b = 24.594（2）, c = 10.4225（9）/k, β = 114.0110（10）°, V = 2396.7（4） A3, Dc = 1.460 g/cm3,μ = 0.482 mm-1, Mr = 1053.63, F（000） = 1088, Z = 2, the final R = 0.0358 and wR = 0.0973 with I 〉 2σ（I）. Both 3,4＇-Hbpt and H2oba ligands adopt monodentate modes linking one Ni（II） ion to form a 0D motif. Furthermore, the 0D motifs are linked into a 3D supramolecular architecture with hydrogen bonds. In addition, the catalytic performance for thermal decomposition of the efficacy of ammonium perchlorate （AP） is explored by differential scanning calorimetry （DSC）, which indicates that the complex is a good candidate for a promoter of the thermal decomposition of ammonium perchlorate.展开更多
A modified Dakin-West one-pot, four-component condensation of an aryl aldehyde, aryl ketone, acetyl chloride and acetonitrile in the presence of silica supported perchloric acid as an active, inexpensive, recoverable ...A modified Dakin-West one-pot, four-component condensation of an aryl aldehyde, aryl ketone, acetyl chloride and acetonitrile in the presence of silica supported perchloric acid as an active, inexpensive, recoverable and recyclable catalyst is reported for the synthesis of β-acetamido ketones under mechanical stirring and ultrasonic irradiation conditions. This system has advantages of short reaction times, good to excellent yields and the ability to carry out the large scale reactions. The use of ultrasound increases the rate of reactions compared with reactions at reflux conditions.展开更多
An environmentally friendly and highly efficient procedure for the preparation of 1,4-dihydropyridines by the reaction between a,β-unsaturated aldehydes, aromatic amines and β-keto esters in the presence of silica s...An environmentally friendly and highly efficient procedure for the preparation of 1,4-dihydropyridines by the reaction between a,β-unsaturated aldehydes, aromatic amines and β-keto esters in the presence of silica supported perchloric acid is described.展开更多
目的本文旨在研究直接除碳重量法测定碳复合磷酸铁锂中总磷含量。方法采用高氯酸分解试样并同时除去样品中的碳后,在酸性介质中,正磷酸根与喹钼柠酮沉淀剂反应生成黄色磷钼酸喹啉沉淀,经过滤、洗涤、干燥、称量,即可求出磷含量。结果高...目的本文旨在研究直接除碳重量法测定碳复合磷酸铁锂中总磷含量。方法采用高氯酸分解试样并同时除去样品中的碳后,在酸性介质中,正磷酸根与喹钼柠酮沉淀剂反应生成黄色磷钼酸喹啉沉淀,经过滤、洗涤、干燥、称量,即可求出磷含量。结果高氯酸消解除碳,样品消解完全且清亮,减少了过滤除碳步骤,通过优化条件试验、对该方法进行了精密度和准确度试验,其相对标准偏差(Relative Standard Deviation,RSD)小于0.2%,加标回收率为98.4%~101.1%。该方法最大的优点在于碳在消解过程中直接除去,消除了碳包裹对磷测定的影响,不需要过滤除碳,缩短了操作流程,分析时间短,高含量磷用经典重量法测定,其精密度和准确度高,能为生产提供快速准确的结果。结论本法适用于快速准确测定碳复合磷酸铁锂中总磷含量的。展开更多
Chemical or electrochemical oxidation of N-benzylaniline in perehloric acid solution yields a highly colored polymer——poly-N-benzylaniline (PBAn).The polymer has good solubility in a num- ber of organic solvents in ...Chemical or electrochemical oxidation of N-benzylaniline in perehloric acid solution yields a highly colored polymer——poly-N-benzylaniline (PBAn).The polymer has good solubility in a num- ber of organic solvents in either acid or base form.At room temperature,conductivity measurements on pressed pellets of the acid form PBAn give a conductivity of 9.3×10^(-6) S·cm^(-1).The soluble polymer was analyzed using a variety of common experimental techniques including UV-vis,IR,NMR,ESR spectroscopy,elemental analysis and electrochemieal analysis.All experimental results showed that PBAn has a structure similar to polyaniline with the elimination of some benzyl groups.展开更多
用香草醛-高氯酸比色法测定苦瓜总皂苷。通过对比色条件进行优化得最佳条件:加热时间15 m in,加热温度60℃,显色剂用量0.7 mL 8%香草醛-冰乙酸。结果表明,该测定方法精密度高,在50 m in内显色稳定,加样回收率高,平均加样回收率为101.46%...用香草醛-高氯酸比色法测定苦瓜总皂苷。通过对比色条件进行优化得最佳条件:加热时间15 m in,加热温度60℃,显色剂用量0.7 mL 8%香草醛-冰乙酸。结果表明,该测定方法精密度高,在50 m in内显色稳定,加样回收率高,平均加样回收率为101.46%,RSD为1.19%(n=3),且操作简单,对设备要求不高,是一种快速测定苦瓜总皂苷的好方法。展开更多
基金Supported by the National Natural Science Foundation of China(No.21263019)
文摘A new energetic complex, Ni（3,4＇-Hbpt）2（Hoba）2（H20）2 （3,4＇-Hbpt = 3-（3-pyridyl）- 5-（4＇-pyridyl）-l-H-l,2,4-triazole and H2oba = 4,4＇-oxybis（benzoic acid））, has been synthesized by hydrothermal reaction and characterized by elemental analysis, IR spectroscopy, single-crystal X-ray diffraction, thermogravimetric analyses and X-ray powder diffraction. Single-crystal X-ray diffraction analysis indicates that the complex belongs to the monoclinic system, space group P2j/c with a = 10.2357（9）, b = 24.594（2）, c = 10.4225（9）/k, β = 114.0110（10）°, V = 2396.7（4） A3, Dc = 1.460 g/cm3,μ = 0.482 mm-1, Mr = 1053.63, F（000） = 1088, Z = 2, the final R = 0.0358 and wR = 0.0973 with I 〉 2σ（I）. Both 3,4＇-Hbpt and H2oba ligands adopt monodentate modes linking one Ni（II） ion to form a 0D motif. Furthermore, the 0D motifs are linked into a 3D supramolecular architecture with hydrogen bonds. In addition, the catalytic performance for thermal decomposition of the efficacy of ammonium perchlorate （AP） is explored by differential scanning calorimetry （DSC）, which indicates that the complex is a good candidate for a promoter of the thermal decomposition of ammonium perchlorate.
文摘A modified Dakin-West one-pot, four-component condensation of an aryl aldehyde, aryl ketone, acetyl chloride and acetonitrile in the presence of silica supported perchloric acid as an active, inexpensive, recoverable and recyclable catalyst is reported for the synthesis of β-acetamido ketones under mechanical stirring and ultrasonic irradiation conditions. This system has advantages of short reaction times, good to excellent yields and the ability to carry out the large scale reactions. The use of ultrasound increases the rate of reactions compared with reactions at reflux conditions.
文摘An environmentally friendly and highly efficient procedure for the preparation of 1,4-dihydropyridines by the reaction between a,β-unsaturated aldehydes, aromatic amines and β-keto esters in the presence of silica supported perchloric acid is described.
文摘目的本文旨在研究直接除碳重量法测定碳复合磷酸铁锂中总磷含量。方法采用高氯酸分解试样并同时除去样品中的碳后,在酸性介质中,正磷酸根与喹钼柠酮沉淀剂反应生成黄色磷钼酸喹啉沉淀,经过滤、洗涤、干燥、称量,即可求出磷含量。结果高氯酸消解除碳,样品消解完全且清亮,减少了过滤除碳步骤,通过优化条件试验、对该方法进行了精密度和准确度试验,其相对标准偏差(Relative Standard Deviation,RSD)小于0.2%,加标回收率为98.4%~101.1%。该方法最大的优点在于碳在消解过程中直接除去,消除了碳包裹对磷测定的影响,不需要过滤除碳,缩短了操作流程,分析时间短,高含量磷用经典重量法测定,其精密度和准确度高,能为生产提供快速准确的结果。结论本法适用于快速准确测定碳复合磷酸铁锂中总磷含量的。
基金the National Natural Science Foundation of China
文摘Chemical or electrochemical oxidation of N-benzylaniline in perehloric acid solution yields a highly colored polymer——poly-N-benzylaniline (PBAn).The polymer has good solubility in a num- ber of organic solvents in either acid or base form.At room temperature,conductivity measurements on pressed pellets of the acid form PBAn give a conductivity of 9.3×10^(-6) S·cm^(-1).The soluble polymer was analyzed using a variety of common experimental techniques including UV-vis,IR,NMR,ESR spectroscopy,elemental analysis and electrochemieal analysis.All experimental results showed that PBAn has a structure similar to polyaniline with the elimination of some benzyl groups.
文摘用香草醛-高氯酸比色法测定苦瓜总皂苷。通过对比色条件进行优化得最佳条件:加热时间15 m in,加热温度60℃,显色剂用量0.7 mL 8%香草醛-冰乙酸。结果表明,该测定方法精密度高,在50 m in内显色稳定,加样回收率高,平均加样回收率为101.46%,RSD为1.19%(n=3),且操作简单,对设备要求不高,是一种快速测定苦瓜总皂苷的好方法。
