2,5二甲基哌嗪合成工艺的研究讲解.pdf

南京理工大学硕士学位论文 2,5-二甲基哌嗪合成工艺的研究姓名:郭一斐申请学位级别:硕士专业:化学工艺指导教师:罗军 20080601 硕嫩论文 2, 2,,可用来合成医药、农药、染料和表匿活性剂等多种精缨化学品。2,,,5·二酮哌嗪、2,、~异丙醇胺制得。本文介绍了以一异丙醇胺为原料,催化脱氢加氢催化剂为催化剂合成2,,重点对以Raney-Ni 力催化荆的反应进行了研究。对反应中催化剂用量、反疲温度、压力、时间等因素进行研究,确定了反应的最佳条件:"--,反应温度150"-170℃,反应时间4~6h、Ran,ey-"-~,在此工艺条件下,原料一异丙醇胺的转化率为 100%,2,%,与文献相比反应条件要温和很多,。0MPa,降幅达50%,反应温度也下降了50℃。、,产率与以Raney-Ni为催化剂相比还有较大的差距,转化率也不高。经过精馏可得纯度90%的2,,再进行重结晶可得到纯度99%的2,5一二甲基哌嚷。通过改变反应温度、氢气初压等反应条件,可以实现对反应产物2,5一二甲基哌嗪和2,5-二甲基毗嗪的比例的控制。当反应温度为240"C、、氢气初压为O盼条件下反应 6h,%产率的2,。关键词:2,5。二甲基哌嚷,一异蘑酵胺,2,,雷尼镍, Abstract 2,5-dimethylpiperazine is all important chemical material and pharmaceutical could beused in thesynthesis of anumber offinechemicals including pharmaceuticals,pesticides,dyestuffs,surfactants,.etc。2,5*dimethylpiperazine could be obtainedby reductionof3,6-dimethyl-2,5*diketopiperazine、2,5-dimethytpyrazine orcatalytic hydrogenation oflactamide thisthesis,isopropanolamine was used鑫s reactant toform 2,5一dimethylpiperazine in thepresence ofhydrogenation—dehydrogenation catalysts,+Raney-Ni。翻转reaction conditions were optimized,such astheamount of the catalyst、reactiontemperature、reaction pressure and processing conditions:2,0"-'3。0M溉original hydrogen、reaction temperature 150"-'170℃、"--'5。0 grams ofRaney-Ni catalyst per moleand areaction timeof4 to6 hours。Under these conditions,the conversion of isopropanolamine was 00% and the yield of 2。 was about 70%.The reactionconditions were much pared toreferences, reactionpressure drop from andthe reactiontemperature drop about50℃。Reaction withNi-Bamorphous alloycatalysts、Ni-13 amorphous alloycatalysts withadditionofMo andCu/Si02 were alsostudie