精细与专用化学品
精細與專用化學品
정세여전용화학품
FINE AND SPECIALTY CHEMICALS
2012年
12期
21-24
,共4页
王留成%张磊%赵建宏%宋成盈%王建设
王留成%張磊%趙建宏%宋成盈%王建設
왕류성%장뢰%조건굉%송성영%왕건설
邻甲苯胺%重氮化%邻氨基偶氮甲苯
鄰甲苯胺%重氮化%鄰氨基偶氮甲苯
린갑분알%중담화%린안기우담갑분
o-toluidine%diazotization%o-aminoazotoluene
以邻甲苯胺、硫酸、亚硝酸钠为原料,采用重氮化一偶合反应方法制备邻氨基偶氮甲苯。分别考察了硫酸浓度、亚硝酸钠浓度、以及亚硝酸钠与邻甲苯胺的量比等因素对邻氨基偶氮甲苯收率的影响,同时考察了采用一定量回收邻甲苯胺对邻氨基偶氮甲苯收率的影响。结果表明:浓度为36%硫酸溶液、36%亚硝酸钠溶液以及亚硝酸钠与邻甲苯胺的量比为1.1:1条件下,邻氨基偶氮甲苯的收率达到87%的最高值,纯度为95%;在偶合反应中添加30%~50%的回收邻甲苯胺,产物收率在77%左右。
以鄰甲苯胺、硫痠、亞硝痠鈉為原料,採用重氮化一偶閤反應方法製備鄰氨基偶氮甲苯。分彆攷察瞭硫痠濃度、亞硝痠鈉濃度、以及亞硝痠鈉與鄰甲苯胺的量比等因素對鄰氨基偶氮甲苯收率的影響,同時攷察瞭採用一定量迴收鄰甲苯胺對鄰氨基偶氮甲苯收率的影響。結果錶明:濃度為36%硫痠溶液、36%亞硝痠鈉溶液以及亞硝痠鈉與鄰甲苯胺的量比為1.1:1條件下,鄰氨基偶氮甲苯的收率達到87%的最高值,純度為95%;在偶閤反應中添加30%~50%的迴收鄰甲苯胺,產物收率在77%左右。
이린갑분알、류산、아초산납위원료,채용중담화일우합반응방법제비린안기우담갑분。분별고찰료류산농도、아초산납농도、이급아초산납여린갑분알적량비등인소대린안기우담갑분수솔적영향,동시고찰료채용일정량회수린갑분알대린안기우담갑분수솔적영향。결과표명:농도위36%류산용액、36%아초산납용액이급아초산납여린갑분알적량비위1.1:1조건하,린안기우담갑분적수솔체도87%적최고치,순도위95%;재우합반응중첨가30%~50%적회수린갑분알,산물수솔재77%좌우。
The o-aminoazotoluene was preparated using o-toluidine, sulfuric acid, and sodium nitrate as raw materials by diazotization and coupling. The influwence of sulfuric acid concentration, sodium nitrate concentrations, and the mole ratio of sodium nitrate and o-toluidine on the reaction was examined. At the same time, the influence of a amount of recovery o-toluldine in the coupling on the reaction was examined. The results showed that the yield of o-aminoazotoluene is 87% , and the purity of o-aminoazotoluene is 95% , when the concentration of the solution of sulfuric acid is 36% , the concentration of the solution of sodium nitrate is 36% , and the mole ratio of sodium nitrate and o-toluidine is 1.1 : 1. The yield of o-aminoazotoluene is about 77% with addition of 30% - 50% o-toluldine after through recovery and purification in the coupling reaction.