A novel one-dimensional chain complex [Zn(dafo)2(H2O)2](NO3)2 was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 s...A novel one-dimensional chain complex [Zn(dafo)2(H2O)2](NO3)2 was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a = 0.702 7(14) nm, b = 0.828 95(17) nm, c = 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.展开更多
The new room-temperature molten salt was prepared based on LiTFSI[LiNC(SO 2CF 3) 2] with OZO(C 3H 5NO 2) which were not reported in literature. Its thermal and electrochemical properties were studied by differential s...The new room-temperature molten salt was prepared based on LiTFSI[LiNC(SO 2CF 3) 2] with OZO(C 3H 5NO 2) which were not reported in literature. Its thermal and electrochemical properties were studied by differential scanning calorimetry, ac impedance spectroscopy and cyclic voltammertry respectively. The results indicated that the structure symmetry of the molecule was depressed and the extent of charges delocalization was expanded, because of introducing oxygen atom of differential electronegativity in OZO molecule. DSC analysis showed that the LiTFSI-OZO molten salt has the excellent thermal stability and its eutectic temperature is below about 223.15 K. Meanwhile, the conductivity of LiTFSI-OZO molten salt at a molar ratio of 1∶4.5 is 0.75×10 -3 S/cm at 298.15 K and 3.50×10 -3 S/cm at 333.15 K. CV analysis showed that the electrochemical window of the sample is about 4 V.展开更多
研究了以3-氯-邻苯二甲酸酐为原料,经甲胺化、偶联、水解和脱水反应制备2,2,′3,3′-联苯四酸二酐(i-BPDA)的工艺过程,偶联反应以三苯基膦(PPh3)为配位体的镍络合物为催化剂、锌粉为还原剂、碘化钠为促进剂。采用红外光谱、氢核磁共振对...研究了以3-氯-邻苯二甲酸酐为原料,经甲胺化、偶联、水解和脱水反应制备2,2,′3,3′-联苯四酸二酐(i-BPDA)的工艺过程,偶联反应以三苯基膦(PPh3)为配位体的镍络合物为催化剂、锌粉为还原剂、碘化钠为促进剂。采用红外光谱、氢核磁共振对i-BPDA及反应中间产物的结构进行了表征,并用高效液相色谱测定了i-BPDA的纯度。实验结果表明,中间产物N-甲基-3-氯-邻苯酰亚胺(C8H6NO2C l)偶联反应的收率受催化剂的种类、催化剂配比、反应时间和反应温度的影响,其中当催化剂中的镍化合物为无水N iC l2时,催化剂的活性最高;最佳偶联条件为:n(C8H6NO2C l)∶n(N iC l2)∶n(PPh3)∶n(Zn)=1∶1∶4∶1.1,反应时间5h,反应温度110℃。在此条件下,偶联产物的收率为69.0%。i-BPDA的平均纯度大于98%。展开更多
文摘A novel one-dimensional chain complex [Zn(dafo)2(H2O)2](NO3)2 was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a = 0.702 7(14) nm, b = 0.828 95(17) nm, c = 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.
文摘The new room-temperature molten salt was prepared based on LiTFSI[LiNC(SO 2CF 3) 2] with OZO(C 3H 5NO 2) which were not reported in literature. Its thermal and electrochemical properties were studied by differential scanning calorimetry, ac impedance spectroscopy and cyclic voltammertry respectively. The results indicated that the structure symmetry of the molecule was depressed and the extent of charges delocalization was expanded, because of introducing oxygen atom of differential electronegativity in OZO molecule. DSC analysis showed that the LiTFSI-OZO molten salt has the excellent thermal stability and its eutectic temperature is below about 223.15 K. Meanwhile, the conductivity of LiTFSI-OZO molten salt at a molar ratio of 1∶4.5 is 0.75×10 -3 S/cm at 298.15 K and 3.50×10 -3 S/cm at 333.15 K. CV analysis showed that the electrochemical window of the sample is about 4 V.
文摘研究了以3-氯-邻苯二甲酸酐为原料,经甲胺化、偶联、水解和脱水反应制备2,2,′3,3′-联苯四酸二酐(i-BPDA)的工艺过程,偶联反应以三苯基膦(PPh3)为配位体的镍络合物为催化剂、锌粉为还原剂、碘化钠为促进剂。采用红外光谱、氢核磁共振对i-BPDA及反应中间产物的结构进行了表征,并用高效液相色谱测定了i-BPDA的纯度。实验结果表明,中间产物N-甲基-3-氯-邻苯酰亚胺(C8H6NO2C l)偶联反应的收率受催化剂的种类、催化剂配比、反应时间和反应温度的影响,其中当催化剂中的镍化合物为无水N iC l2时,催化剂的活性最高;最佳偶联条件为:n(C8H6NO2C l)∶n(N iC l2)∶n(PPh3)∶n(Zn)=1∶1∶4∶1.1,反应时间5h,反应温度110℃。在此条件下,偶联产物的收率为69.0%。i-BPDA的平均纯度大于98%。
