杂质对氯苯胺在对位酯生产中的控制研究

Study on control of p-chloroaniline in the production of para-ester

对位酯[对-(β-羟乙基砜硫酸酯)苯胺]是活性染料最重要的中间体之一,以乙酰苯胺为原料合成工艺中应严格控制对位酯成品中对氯苯氨含量。对乙酰苯胺法合成对位酯工艺中磺化工段进行了优化实验研究,探讨了氯磺酸质量、氯化亚砜与氯磺酸配比对成品对位酯中对氯苯胺的影响。实验结果表明,对位酯磺化工序使用高三氧化氯磺酸(SO3含量>68.7%)、氯化亚砜与氯磺酸质量为0.25∶1时,能够有效减少对位酯中对氯苯胺含量。

Para-ester[para-(beta-hydroxyethyl sulfone sulphate)aniline]is one of the most important intermediates of reactive dyes.The content of chloraniline in para-ester should be strictly controlled in the synthesis process using acetaniline as raw material.The sulfonation process in the synthesis of para-ester by acetanilide was optimized.The effects of the quality of chlorosulfonic acid and the ratio of thionyl chloride to chlorosulfonic acid on p-chloroaniline in para-ester were discussed.When chloro sulfonic acid trioxide(SO3>68.7%)is used in the sulfonation process and the ratio of thionyl chloride to chloronic sulfonic acid is 0.25∶1,the content of p-chloroaniline in para-ester could be effectively reduced.