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
3,6-二硝基吡唑[4,3-c]并吡唑(D N PP),是一种新型氮杂环含能材料。以乙酰丙酮为原料,经环化、重氮化、双环构建、硝化、氧化、脱羧硝化等反应合成了D N PP,得率为13.3%,比文献值提高了4%。考察了一锅法制备中间体4-氨基-3,5-二甲基吡...3,6-二硝基吡唑[4,3-c]并吡唑(D N PP),是一种新型氮杂环含能材料。以乙酰丙酮为原料,经环化、重氮化、双环构建、硝化、氧化、脱羧硝化等反应合成了D N PP,得率为13.3%,比文献值提高了4%。考察了一锅法制备中间体4-氨基-3,5-二甲基吡唑的合成工艺、硝化工艺和脱羧硝化工艺。展开更多
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℃.
