一锅法合成二硝基五亚甲基四胺工艺研究  

Reaction Process of Synthesizing Dinitro Pentamethylene Tetramine by One-Pot Method

作　　者：王鹏[1] 宋红燕[1] 孟子晖[1] 李清霞[1] 

机构地区：[1]北京理工大学化工与环境学院,北京100081

出　　处：《北京理工大学学报》2011年第5期603-605,617,共4页Transactions of Beijing Institute of Technology

摘　　要：通过研究一锅法合成DPT工艺为DPT法制备HMX工艺改进提供依据．以尿素为起始原料，中间体不分离，经硝化、水解、Mannich缩合等反应得到DPT．考察硝酸用量、硝化时间、水解时间、甲醛用量和介质pH值等因素对DPT收率的影响，确立了较佳工艺．当发烟硝酸用量11．5mL，硝硫混酸体积比1．1，硝化60min，水解90min，体积分数37％～40％的甲醛溶液40．8mL加热至40℃反应40min，氨水中和溶液至pH=7．5，DPT产率65．2％．Dinitro pentamethylene tetramine （DPT） is an important precursor of octogen （cyclotetramethylene tetramine, HMX）. This article explores the process of synthesizing DPT by one-pot method to provide a practical basis for improving HMX production through DPT. The urea was used as the original material. Without isolation from intermediates, DPT was obtained by the chemical reaction of nitration, hydrolysis and Mannich condensation. Some factors to affect yield of DPT were investigated, such as dosage of nitric acid, nitration time, hydrolyzation time, dosage of formaldehyde, pH of solution and so on. The optimum conditions of process were determined. With this process, the yield of DPT was advanced up to 65.2~/oo.

关 键 词：二硝基五亚甲基四胺 二硝基脲 一锅法 

分 类 号：O621.3[理学—有机化学]