The influences of catalyst concentration, reaction temperature and pressure, feed rate, and water content on the liquid phase oxidation of 2,6-diisopropylnaphthalene to 2,6-naphthalenedicarboxylic acid (2,6-NDCA)were ...The influences of catalyst concentration, reaction temperature and pressure, feed rate, and water content on the liquid phase oxidation of 2,6-diisopropylnaphthalene to 2,6-naphthalenedicarboxylic acid (2,6-NDCA)were studied in a 1 L titanium reactor using air as oxidant, acetic acid as solvent, and a Co-Mn-Br mixture as catalyst, and the optimum operation conditions were obtained in the experimental range.Meanwhile, the promotor effects of individual CO2 and Ni 2+ and their combined use on the activity of Co-Mn-Br catalyst were discussed.Based on the results of the batch experiments, a continuous process for making 2,6-NDCA was developed.The yield of 2,6-NDCA increased from 69% to 73% and the purity of 2,6-NDCA could be up to 95% with the increasing of reaction time.展开更多
以联苯和乙酰氯为原料,通过傅克酰基化反应合成4-联苯乙酮,在醋酸体系中,4-联苯乙酮经Co-Mn-Br常压催化氧化,得目标产物联苯-4-甲酸。详细考察了催化剂用量、物料配比、氧气流速和反应温度对氧化反应的影响,确定较佳的工艺条件:n(Co)∶n...以联苯和乙酰氯为原料,通过傅克酰基化反应合成4-联苯乙酮,在醋酸体系中,4-联苯乙酮经Co-Mn-Br常压催化氧化,得目标产物联苯-4-甲酸。详细考察了催化剂用量、物料配比、氧气流速和反应温度对氧化反应的影响,确定较佳的工艺条件:n(Co)∶n(Mn)=1∶1,n(Co+Mn)∶n(Br)=1∶1,催化剂的用量为1.5%(原料的重量比),氧气流速为150 m L/min,反应温度80℃。在此条件下,联苯-4-甲酸产品收率为92.9%(以原料联苯计),纯度为99.5%(HPLC面积归一化法)。产物结构经过熔点、1H-NMR和MS表征。展开更多
文摘The influences of catalyst concentration, reaction temperature and pressure, feed rate, and water content on the liquid phase oxidation of 2,6-diisopropylnaphthalene to 2,6-naphthalenedicarboxylic acid (2,6-NDCA)were studied in a 1 L titanium reactor using air as oxidant, acetic acid as solvent, and a Co-Mn-Br mixture as catalyst, and the optimum operation conditions were obtained in the experimental range.Meanwhile, the promotor effects of individual CO2 and Ni 2+ and their combined use on the activity of Co-Mn-Br catalyst were discussed.Based on the results of the batch experiments, a continuous process for making 2,6-NDCA was developed.The yield of 2,6-NDCA increased from 69% to 73% and the purity of 2,6-NDCA could be up to 95% with the increasing of reaction time.
文摘以联苯和乙酰氯为原料,通过傅克酰基化反应合成4-联苯乙酮,在醋酸体系中,4-联苯乙酮经Co-Mn-Br常压催化氧化,得目标产物联苯-4-甲酸。详细考察了催化剂用量、物料配比、氧气流速和反应温度对氧化反应的影响,确定较佳的工艺条件:n(Co)∶n(Mn)=1∶1,n(Co+Mn)∶n(Br)=1∶1,催化剂的用量为1.5%(原料的重量比),氧气流速为150 m L/min,反应温度80℃。在此条件下,联苯-4-甲酸产品收率为92.9%(以原料联苯计),纯度为99.5%(HPLC面积归一化法)。产物结构经过熔点、1H-NMR和MS表征。
