华东理工大学学报(自然科学版)
華東理工大學學報(自然科學版)
화동리공대학학보(자연과학판)
JOURNAL OF EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
2001年
1期
30-33,37
,共5页
N-羟乙基乙二胺%哌嗪%杂多酸%Raney Ni%脱水
N-羥乙基乙二胺%哌嗪%雜多痠%Raney Ni%脫水
N-간을기을이알%고진%잡다산%Raney Ni%탈수
研究了以N-羟乙基乙二胺(HDEA)为原料，经催化脱水环化合成哌嗪(PIP)的过程；考察了不同的催化剂，催化剂用量，反应时间、温度、压力，溶剂配比等对转化率和哌嗪选择性的影响。结果表明，较好的催化剂为Raney Ni(C),在180°C，3MPa,溶剂与原料配比6∶1(mol∶mol)，催化剂用量w=0.10,反应时间3h时，得到的转化率为89.2%，选择性85.0%，收率75.8%。小试数据能在放大试验中重复，精馏分离得到的产品哌嗪纯度>98.0%。
研究瞭以N-羥乙基乙二胺(HDEA)為原料，經催化脫水環化閤成哌嗪(PIP)的過程；攷察瞭不同的催化劑，催化劑用量，反應時間、溫度、壓力，溶劑配比等對轉化率和哌嗪選擇性的影響。結果錶明，較好的催化劑為Raney Ni(C),在180°C，3MPa,溶劑與原料配比6∶1(mol∶mol)，催化劑用量w=0.10,反應時間3h時，得到的轉化率為89.2%，選擇性85.0%，收率75.8%。小試數據能在放大試驗中重複，精餾分離得到的產品哌嗪純度>98.0%。
연구료이N-간을기을이알(HDEA)위원료，경최화탈수배화합성고진(PIP)적과정；고찰료불동적최화제，최화제용량，반응시간、온도、압력，용제배비등대전화솔화고진선택성적영향。결과표명，교호적최화제위Raney Ni(C),재180°C，3MPa,용제여원료배비6∶1(mol∶mol)，최화제용량w=0.10,반응시간3h시，득도적전화솔위89.2%，선택성85.0%，수솔75.8%。소시수거능재방대시험중중복，정류분리득도적산품고진순도>98.0%。
A catalytic dehydrolysis process for synthesis of piperazine (PIP) from N-hydroxyethylethylenediamine (HDEA) has been studied. Various kinds of catalysts, such as acid catalysts, metal oxide supported on γ-Al2O3 and Raney Ni have shown certain activities on this reaction. In this case, the suitable catalyst is Raney Ni, especially the Raney Ni (C) which is prepared by adding some copper. The effect of content of metal copper on the reaction results has also been observed, it shows that the optinum wCu is 0.07～0.10. The optimal reaction conditions for Raney Ni (C) are 180°C， 3MPa, H2O∶HDEA=6∶1(mol∶mol), catalyst amount wcat=0.10 and reaction time 3h. Under these conditions the conversion and selectivity are 89.2% and 75.8% respectively. The results of scale-up experiment are comparable to these of the laboratory test. The SEM micrographs of fresh and used catalyst showed that the used catalyst has been covered by some substance, and the skeleton structure can not be distinguished clearly. So the conversion and selectivity of the product decrease with the used times. After fractional distillation, the purity of the product PIP is higher than 95%.
