HPO法制备己内酰胺的羟胺化过程研究  

Study on hydroxylamine process in HPO caprolactam production

作　　者：毛伟[1] 蒋利萍[2] 张庆祥[1] 

机构地区：[1]中国石油化工股份有限公司巴陵分公司己内酰胺事业部,湖南岳阳414000 [2]巴陵石化公司职工培训学校,湖南岳阳414014

出　　处：《合成纤维工业》2014年第4期26-30,共5页China Synthetic Fiber Industry

摘　　要：在70 kt/a磷酸羟胺（HPO）法制备己内酰胺工业装置上,对硝酸盐催化还原制备磷酸羟胺的反应影响因素进行探讨.结果表明：羟胺化过程反应温度控制58～62 ℃,反应压力为2 500～2 550 kPa,氢分压为38％ ～40％,催化剂浓度为6.5～9.6 kg/m3,气体循环量体积分数为46.0～ 48.0 km3/h,羟胺反应器出口pH值为1.80 ～2.00,控制羟胺反应进料组分中H＋浓度为2.90～3.10 mol/kg、H2 PO4-浓度2.30 ～2.45mo1/kg、NH4＋浓度为2.50～3.00 mol/kg时,羟胺钯/碳（Pd/C）催化剂的活性和选择性能达到最佳值,磷酸羟胺的收率达0.98 ～ 1.03 mol/kg.The influential factors on nitrate catalytic reduction into hydroxylamine phosphate were discussed on a 70 kt/a capro- lactam commercial experimental unit of hydroxylamine phosphate （HPO） process. The results showed that the activity and selec- tivity of hydroxylamine Pd/C catalyst could be optimized, and the yield of hydroxylamine phosphate could be 0.98 - 1.03 mol/kg by controlling the hydroxylamine reaction temperature of 58 -62 ℃, hydroxylamine reaction pressure 2 500 -2 550 kPa, hydro- gen partial pressure 38% -40%, catalyst concentration 6.5 -9.6 kg/m3 , gas circulation volume 46.0 -48.0 km3/h, pH value of 1.80 - 2.00 at the exit of hydroxylamine reactor, H ＋ concentration of 2.90 - 3.10 mol/kg, H2PO4 concentration 2.30 - 2.45 mol/kg, and NH＋4 2.50 - 3.00 mol/kg in the feedstocks of hydroxylamine reaction.

关 键 词：磷酸羟胺 己内酰胺 催化 影响因素 优化 

分 类 号：TQ225.261[化学工程—有机化工]