超临界一步法合成聚醚胺的工艺

One-pot synthesis of polyether amine by supercritical method

采用超临界流体技术,一步反应合成了聚醚胺,旨在解决羟基胺化的技术瓶颈。主要研究了催化剂用量、物料配比、反应时间、反应温度、临氢压力对转化率的影响。确立了较佳反应条件为:催化剂用量7.5%,液氨对聚醚质量比1.5∶1,反应时间7.5 h,反应温度160℃,临氢压力1.0 MPa。最后,利用了核磁共振波谱技术对产品结构进行了表征。此工艺路线的成功开发,将为替代聚醚胺传统釜式间歇生产工艺,实现连续生产提供强有力的依据。

In order to overcome technical bottleneck of hydroamination, the influences of catalyst dosage, m（NH3）/m（polyether）, reaction time, temperature and pressure on the conversion of one-pot synthesis of polyether amine by the supercritical method were investigated. The results showed the suitable reaction conditions： catalyst dosage 7.5%, m（NH3）/m（polyether）=l.5, 7.5 h, 160 ℃, 1.0 MPa. The products was characterized with NMR. The development of this technology will provide strong basis for continuous production instead of traditional batch production.