石油炼制与化工

• 分析与评定 • 上一篇    下一篇

己内酰胺成品中挥发性碱杂质的研究

胡合新,孙斌,王恩泉   

  1. 石油化工科学研究院
  • 收稿日期:2010-12-16 修回日期:2011-01-06 出版日期:2011-06-12 发布日期:2011-06-12
  • 通讯作者: 胡合新

AN ANALYSIS OF IMPURITIES AFFECTING THE VOLATILE BASE CONTENT IN CAPROLACTAM

bin sun   

  • Received:2010-12-16 Revised:2011-01-06 Online:2011-06-12 Published:2011-06-12

摘要: 通过GC-MS定性分析己内酰胺成品重结晶后的杂质浓缩液,比较不同质量等级己内酰胺的杂质差异,特别是影响挥发性碱含量的杂质。结果表明,己内酰胺成品中主要含有C3 C7直链酰胺、肟、苯胺和己二酰亚胺等杂质,其中C3 C7直链酰胺和己二酰亚胺对挥发性碱含量影响最大,其含量增加0.1 mmol/kg,挥发性碱含量约上升0.1 mmol/kg;苯胺对挥发性碱含量影响较小,肟及环状内酰胺基本无影响。与优级品相比,己内酰胺合格品中主要含有较多C3 C7直链酰胺及己二酰亚胺、一级品含有微量的正戊酰胺和正己酰胺而使挥发性碱含量超标。

关键词: 己内酰胺, 挥发性碱, 重结晶, 产品质量

Abstract: The compositions of impurities in the concentrated mother liquids after the recrystallizations of three various quality grades caprolactam products were analyzed by GC-MS to compare the impurities that affect the volatile base contents in these products. Results showed that the impurities were mainly composed of C3-C7 amides with straight chain, C6 imides, oximes and aniline, in which C3-C7 amides with straight chain and C6 imides had significant effect on the volatile base content: with the increase of 0.1 mmol/kg these impurities, the volatile base content could increase 0.1 mmol/kg. Aniline had less effect on the volatile base content; oximes and lactams had little effect. As compared with the superior caprolactam product, in the qualified product impurities were mainly composed of C3-C7 amides with straight chain and C6 imides, in the first-class product minor impurities were n-valeramide and n-caproamide, however, the existence of these impurities in products leads to a higher volatile base content, which degrades the product class.

Key words: caprolactam, volatile base, re-crystallization, Product quality