双氧水对环己酮氨肟化反应的影响及优化措施

Effect of hydrogen peroxide on cyclohexanone ammoximation reaction and optimization measures thereof

针对300 kt/a氨肟化装置双氧水(H_(2)O_(2))消耗高、己内酰胺产品色度及挥发性碱含量高的现状,探讨了H_(2)O_(2)对氨肟化反应的影响,并提出了优化措施。结果表明:氨肟化反应过程中,控制H_(2)O_(2)/环己酮摩尔比在1.12~1.14,H_(2)O_(2)质量分数在29.5%~32.0%,不仅可提高装置的生产能力,而且H_(2)O_(2)、环己酮消耗也明显降低;H_(2)O_(2)总碳含量对环己酮肟色度、环己酮肟二段重排反应滴定值有较大影响,通过将吸附树脂床运行工艺由并联优化为串联,可控制H_(2)O_(2)总碳含量在100 mg/kg以下;将H_(2)O_(2)由反应釜顶部进料调整为底部进料,H_(2)O_(2)与环己酮、氨的共混效果提高,环己酮的转化率达到99.95%。

In response to the high consumption of hydrogen peroxide(H_(2)O_(2))and the high chromaticity and volatile alkali content of caprolactam products on a 300 kt/a ammoximation unit,the effect of H_(2)O_(2) on the ammoximation reaction was discussed,and the optimization measures were proposed.The results showed that the production capacity of the unit can be improved and the consumption of H_(2)O_(2) and cyclohexanone can be significantly reduced by controlling the molar ratio of H_(2)O_(2)/cyclohexanone between 1.12 and 1.14 and the mass fraction of H_(2)O_(2) between 29.5%and 32.0%during the ammoximation reaction process;the total carbon content of H_(2)O_(2) had a significant impact on the chromaticity of cyclohexanone oxime and the titration value of the two-stage rearrangement reaction of cyclohexanone oxime,and the total carbon content of H_(2)O_(2) can be controlled below 100 mg/kg by optimizing the operation process of the adsorption resin bed from parallel to series;and the blending effect of H_(2)O_(2) with cyclohexanone and ammonia was improved and the conversion rate of cyclohexanone reached 99.95%when the feeding method of H_(2)O_(2) was optimized from top feeding to bottom feeding.