摘要
以1-氨基-2-苯氧基-4-羟基蒽醌、氯磺酸、氯化亚砜、3-乙氧基丙胺为原料及Na2CO3为缚酸剂合成了C.I.分散红92.研究了氯磺酸、氯化亚砜用量及温度对氯磺化的影响,研究了3-乙氧基丙胺用量、pH值及温度对胺化缩合的影响.通过实验得到了较佳的反应条件,原料摩尔比是n（1-氨基-2-苯氧基-4-羟基蒽醌）∶n（氯磺酸）∶n（氯化亚砜）∶n（3-乙氧基丙胺）=1∶8∶0.6∶1;氯磺化温度为30～35℃;胺化缩合pH值为7～8,温度为15～20℃.并通过HPLC,^1H-NMR,IR和MS对目标产品进行了分析.以1-氨基-2-苯氧基-4-羟基蒽醌计,总收率大于91%,目标产品HPLC纯度大于99%,溶剂回收率为95%.
Taking 1-amino-2-phenoxy-4-hydranthraquinone, chlorosulfonic acid, thionyl chloride, and 3-ethoxypropylamine as raw materials, using sodium carbonate as an acid-bingding agent, C. I. disperse red 92 was synthesized. The effects of chlorosulfonic acid and thionyl chloride concentrations,as well as reaction temperature on the yield of C. I. disperse red 92 in the sulfonate and chlorination process were investigated. The effects of 3-ethoxypropylamine concentration, pH, and reaction temperature on the yield of C. I. disperse red 92 in the amidation and hydrysis process were studied. A better reaction condition was obtained. The raw materials molar ratio of 1-amino-2-phenoxy-4-hydranthraquinone chlorosulfonic acid, thionyl chloride and 3-ethoxypropylamine was found to be 1, 8, 0.6, and 1. In the sulfonate and chlorination process, reaction temperature was 30-35 ℃. In the amidation and hydrysis process, pH was 7-8, reaction temperature was 15-20 ℃, respectively. The destination product was identified with HPLC, ^1H-NMR, IR and MS. Its total yield was over 91% by 1-amino-2-phenoxy-4-hydranthraquinone, and over 99% purity was obtained . The recovery of solvent was 95%.
出处
《浙江工业大学学报》
CAS
2007年第4期399-403,共5页
Journal of Zhejiang University of Technology
