燃油清净分散剂壬基酚聚氧丙烯醚胺的合成

在间歇釜式反应器中,以壬基酚聚氧丙烯醚(NPP)为原料、Raney Ni为催化剂,采用脱氢-胺化加氢两步法合成了壬基酚聚氧丙烯醚胺(NPPA),考察了脱氢-胺化加氢两步反应的影响因素。实验结果表明,在脱氢反应中,NPP的端羟基脱氢转化为含有羰基的聚醚(简称脱氢产物),生成的氢与正十四烯发生加成反应,提高脱氢转化率;在NPP0.32 mol、240℃、Raney Ni催化剂质量分数5%(基于反应物)、反应时间25 h的条件下,NPP的转化率为61%。在脱氢产物胺化加氢反应中,用氧化钙除去反应中生成的水,提高脱氢产物的转化率;在220～230℃、14～20 MPa、Raney Ni催化剂质量分数(基于脱氢产物)3%、脱氢产物0.32 mol、氢气0.3 mol、氨4.7 mol、搅拌转速500 r/min、氧化钙0.3 mol、反应时间8 h的条件下,NPPA的收率达到80%以上。

Synthesis of Nonylphenoxypolyoxypropylene Amine as Fuel Oil Detergent-Dispersant

Nonylphenoxypolyoxypropylene amine(NPPA) used as detergent-dispersant of fuel oil was synthesized by a two-step process of dehydrogenation and amination-hydrogenation from nonylphenol polyoxypropylene ether (NPP) on Raney Ni catalyst in a batch reactor. In step of dehydrogenation, the end hydroxyl group of NPP was dehydrogenated to carbonyl-terminated polyether(simplified as "dehydrogenation product"). The hydrogen from the dehydrogenation joined addition reaction with 1-tetradecene and improved conversion of NPP to 61% at reaction temperature 240 ℃, NPP 0.32 mol,Raney Ni catalyst mass fraction 5%(based on NPP) and reaction time 25 h. In amination-hydrogenation step of the dehydrogenation product, for the sake to enhance the conversion of dehydrogenation product, CaO was added to take away water from the reaction. The yield of NPPA was above 80% at reaction temperature of 220-230 ℃, reaction pressure 14-20 MPa, mass fraction of Raney Ni catalyst 3%(based on dehydrogenation product),dehydrogenation product 0.32 mol,hydrogen 0.3 mol,ammonia 4.7 mol,stirring speed 500 r/min,CaO 0.3 mol and reaction time 8 h.