Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- ben...Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- benzoic aicd) with CH 2 Cl 2 and triethylamine in 1∶1 molar ratio and characterized by elemental analysis, IR and 1 H NMR . Their crystal structures were determined by X-ray single crystal diffractometry, the crystal(Ⅰ) belongs to orthorhombic with a=0 699 43(14) nm, b=1 348 9(3 ) nm, c=1 668 9(3) nm, V= 1 574 5(6) nm 3 , Z=4, D c =1 336 Mg/m 3 , μ=0 259 mm -1 , R 1 =0 033 4, wR 2 =0 080 6, F(000)=672. The crystal(Ⅱ) belongs to triclinic with a=0 788(12) nm, b=1 239(19) nm, c=2 18(3) nm, α= 89 2°, β =89 6°, γ=76 9°, V=2 078(55) nm 3 , Z=4, D c=1 457 Mg/m 3 , μ=0 414 mm -1 , R 1 =0 062 0, wR 2 =0 151 6, F(000)=960.展开更多
The industrialization of electrochemical synthesis of 3,6-dichloropicolinic acid(3,6-DCP) from 3,4,5,6-tetrachloropicolinic acid(3,4,5,6-TCP) in a tank-type undivided electrolytic cell with silver cathode was investig...The industrialization of electrochemical synthesis of 3,6-dichloropicolinic acid(3,6-DCP) from 3,4,5,6-tetrachloropicolinic acid(3,4,5,6-TCP) in a tank-type undivided electrolytic cell with silver cathode was investigated.The experimental results showed that the electrolytic performance greatly depended on the operation parameters,such as flow rate of electrolyte,temperature,and concentration of NaOH.The reduction of 3,4,5,6-TCP to 3,6-DCP was favored by increasing temperature and flow rate of electrolyte.Industrialization tests of electrochemical synthesis of 3,6-DCP were conducted under the following conditions: silver cathode,temperature 313 K,flow rate 6 cm·s-1,concentration of NaOH 8%(mass),concentration of 3,4,5,6-TCP 5%(mass),cathode current density 600 A·m-2.The current efficiency and conversion ratio of 3,4,5,6-TCP were more than 76% and 99%,respectively.The yield of 3,6-DCP was up to 90% and DC power consumption was 2.939 kW·h·(kg 3,6-DCP)-1.The purity of the product was higher than 95%,and its melting point was 151—153℃.展开更多
文摘Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- benzoic aicd) with CH 2 Cl 2 and triethylamine in 1∶1 molar ratio and characterized by elemental analysis, IR and 1 H NMR . Their crystal structures were determined by X-ray single crystal diffractometry, the crystal(Ⅰ) belongs to orthorhombic with a=0 699 43(14) nm, b=1 348 9(3 ) nm, c=1 668 9(3) nm, V= 1 574 5(6) nm 3 , Z=4, D c =1 336 Mg/m 3 , μ=0 259 mm -1 , R 1 =0 033 4, wR 2 =0 080 6, F(000)=672. The crystal(Ⅱ) belongs to triclinic with a=0 788(12) nm, b=1 239(19) nm, c=2 18(3) nm, α= 89 2°, β =89 6°, γ=76 9°, V=2 078(55) nm 3 , Z=4, D c=1 457 Mg/m 3 , μ=0 414 mm -1 , R 1 =0 062 0, wR 2 =0 151 6, F(000)=960.
文摘The industrialization of electrochemical synthesis of 3,6-dichloropicolinic acid(3,6-DCP) from 3,4,5,6-tetrachloropicolinic acid(3,4,5,6-TCP) in a tank-type undivided electrolytic cell with silver cathode was investigated.The experimental results showed that the electrolytic performance greatly depended on the operation parameters,such as flow rate of electrolyte,temperature,and concentration of NaOH.The reduction of 3,4,5,6-TCP to 3,6-DCP was favored by increasing temperature and flow rate of electrolyte.Industrialization tests of electrochemical synthesis of 3,6-DCP were conducted under the following conditions: silver cathode,temperature 313 K,flow rate 6 cm·s-1,concentration of NaOH 8%(mass),concentration of 3,4,5,6-TCP 5%(mass),cathode current density 600 A·m-2.The current efficiency and conversion ratio of 3,4,5,6-TCP were more than 76% and 99%,respectively.The yield of 3,6-DCP was up to 90% and DC power consumption was 2.939 kW·h·(kg 3,6-DCP)-1.The purity of the product was higher than 95%,and its melting point was 151—153℃.
