连续法合成间甲酚的工艺研究  

Study on continuous synthesis process of m-cresol

作　　者：邵徽旺[1] 蔡剑波[1] 郑志花[1] 崔建兰[1] 曹端林[1] 

机构地区：[1]中北大学化工与环境学院,山西太原030051

出　　处：《应用化工》2007年第10期1011-1013,1016,共4页Applied Chemical Industry

摘　　要：主要研究了将重氮盐合成的传统釜式反应器改为管式反应器和重氮盐合成、水解的间歇式反应工艺改为连续的反应工艺,考察了亚硝酸钠和硫酸的用量、亚硝酸钠溶液、硫酸铵盐溶液、尿素的进料速率对间甲酚得率的影响,得出较佳工艺条件为：重氮化温度维持在0～5℃,亚硝酸钠溶液和硫酸溶液的浓度分别为35%和30%,亚硝酸钠与硫酸与间甲苯胺的物质的量比为1.02∶3.6∶1;亚硝酸钠溶液、硫酸铵盐溶液、尿素的进料速率分别为20 mL/min、120 mL/min、0.100 g/min。所得的重氮盐以130 mL/min滴加到水解反应釜,在110～120℃进行水解反应制备间甲酚,间甲酚得率为86.5%,纯度为99.5%。The traditional reactor by which the diazonium salt was synthesized and switched a tubular reactor and the batch process of synthesis and hydrolysis of the diazonium salt was transformed a continuous reaction process. The influence of the consumption of sodium nitrate and the feeding rate of sodium nitrite solution, ammonium sulfate salt solution and urea on the m-cresol yield were investigated. The results showes that the better condition of process that diazotization temperature maintained at 0 ～ 5 ℃, sodium nitrite concentration was 35% and sulfate solution was concentration 30%, the mole ratio of sodium nitrite, sulfuric acid and m-toluidine was 1.02 ： 3.6 ： 1, the feeding rate of sodium nitrite solution, ammonium sulfate salt solution and urea respectively was 20 mL/min, 120 mL/min ,0. 100 g/min. The diazonium salt , which was synthesized under the above better conditions, added to the hydrolysis reactor at the feed- ing rate of 130 mL/min and reacted at 110 ～ 120 ℃. The m-cresol was attained, its yield and purity were 86.5% ,99.5%.

关 键 词：间甲酚 间歇式反应釜 连续工艺 管式反应器 

分 类 号：TQ923[轻工技术与工程—发酵工程]