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作 者:侯月平[1] 陈志明[2] 褚洪雨[2] 邵利[2]
机构地区:[1]镇江机电高等职业技术学校,江苏镇江212000 [2]东南大学化学化工学院,江苏南京210096
出 处:《应用化工》2007年第11期1087-1089,共3页Applied Chemical Industry
基 金:江苏省高技术资助项目(BG2006038);东南大学校基金项目
摘 要:用铁氰化钾溶液氧化二硫代苯甲酸钠,得双二硫代苯甲酰,采用正交实验探讨了4,4’-偶氮双(4-氰基戊酸)与双二硫代苯甲酰反应的投料比、搅拌方式、反应时间对反应收率的影响。结果表明,4,4’-偶氮双(4-氰基戊酸)与双二硫代苯甲酰的最佳摩尔比为1.1∶1,在反应瓶中加入少许玻璃珠磁力搅拌,反应时间为16 h时,收率最高达到78%,两步总收率最高达到60%,远高于文献报道的44%。用IR和1H NMR表征了产物结构,证明获得所需的目的产物。The sodium dithiobenzoic acid was oxidized with potassium ferricyanide to obtain di (thiobenzoyl) disulfide(DTBDS). The influences of raw materials mole ratio, stirring method and reaction time on the yield were studied with orthogonal test. The experimental results showed that the mole ratio of elemental to DTBDS is 1 : 1, magnetic stirring with some beadings and react 16 h, with the best yield of 78%. The experimental results showed that the best overall yield of two steps is as high as 60% ,which is much higher than that (44%) reported in literature. The structure of the product was characterized by IR and ^1H NMR analysis.
关 键 词:4-氰基戊酸二硫代苯甲酸 合成 新工艺
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