采用单变量试验方法,研究了己内酰胺工业生产中发烟硫酸浓度对环己酮肟贝克曼重排反应的影响.在固定其他工艺条件不变,发烟硫酸质量分数为8%~22%的条件下,对重排反应的重排液滴定值、汽提塔底液的化学耗氧量(COD)及己内酰胺产品的碱度、挥发性碱含量、消光值进行了分析.结果表明:适当提高发烟硫酸的浓度可明显改善环己酮肟贝克曼重排反应状况,提高己内酰胺的收率,降低生产过程中物料消耗,有效提高己内酰胺的产品质量;在己内酰胺生产过程中,将发烟硫酸质量分数提高至20%时,重排反应工序重排液滴定值为0.832,汽提塔釜液COD为1.05×105 mg/L,己内酰胺产品的消光值降至0.017,碱度降至0.05 mmol/kg,挥发性碱降至0.259 mmol/kg.%The effect of oleum concentration on Beckmann rearrangement reaction of cyclohexanone oxime was studied by single variable experiment during caprolactam production.The titration value of rearrangement solution,COD of extraction base solution and the alkalinity,volatile base content,extinction value of caprolactam were analyzed at the mass fraction of oleum 8%-22% under other fixed process conditions.The results showed that the Beckmann rearrangement reaction could be profoundly improved by properly increasing the oleum concentration,hence the yield of caprolactam could be increased,the material consumption be decreased,and the caprolactam quality be efficiently improved;and the titration value of the rearrangement solution was 0.832,the COD of extraction base solution was 1.05×105 mg/L,the extinction value,the alkalinity and volatile base content of caproplactam was decreased to 0.017,0.05 mmol/kg and 0.259 mmol/kg,respectively,as the mass fraction of oleum was increased to 20% during the caprolactam production.
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