【作者】 王金砖；

【导师】 程广斌；

【作者基本信息】 南京理工大学 ， 应用化学， 2009， 硕士

【摘要】 本论文研究以异丙醇胺为原料经催化氨化合成1,2-丙二胺的方法,考察了Raney Ni催化剂用量、原料配比、反应温度、反应时间和氢气加入量对实验结果的影响。确定了合成1,2-丙二胺的最佳反应条件:Raney Ni催化剂用量为异丙醇胺质量的4%,异丙醇胺与氨气的物质的量比为1:3.5,反应温度为160℃,氢气加入量与原料异丙醇胺的物质的量之比为1:5,反应时间为5h。1,2-丙二胺收率在90.3%以上,纯度99.5%以上。大大减少了工业三废的排放量,探索出了一条绿色的合成工艺。以1,2-丙二胺和2,3-丁二酮为原料经缩合氧化合成了2,3,5-三甲基吡嗪,分别考察了影响缩合反应和氧化反应的各种因素,确定了缩合反应的最佳条件为:将原料2,3-丁二酮溶于乙醇(2,3-丁二酮与乙醇的质量比为1:5),匀速滴加到1,2-丙二胺的乙醇溶液(1,2-丙二胺与乙醇质量比为1:6)中,滴加时间3h,反应温度为-5℃,1,2-丙二胺与2,3-丁二酮的物质的量比为1.1:1。最佳的脱氢氧化反应条件为:以空气做氧化剂,氢氧化钾与2,3,5-三甲基-5,6-二氢吡嗪的物质的量比为3:1,乙醇与2,3,5-三甲基-5,6-二氢吡嗪的质量比10:1,反应温度68℃,反应时间7h,两步反应的总收率为83.0%,产物2,3,5-三甲基吡嗪的纯度可达99.5%。更多还原

【Abstract】 1,2-Diaminopropane was synthesized by amination of isopropanolamine in the presence of ammonia and a hydrogenation catalyst Raney Ni.The effect of the amount of Raney Ni catalyst,the molar ratio of materials,reaction temperature and reaction time on the experiment were studied.The optimum conditions were as follows:the amount of catalyst used was 4%by weight of the amount of isopropanolamine used,the molar ratio of isopropanolamine to ammomia was 1:3.5,the reaction temperature was 160℃,the reaction was 5h,the molar ratio of hydrogen to isopropanolamine was 1:5.Yield of 1,2-diaminopropane as high as 89%was obtainable and the purity is above 99.5%.The green synthesis technology with very little emission was developed.Synthesis of 2,3,5-trimethylpyrazine from 2,3-butanedione and 1,2-diaminopropane through 2,3,5-trimethyl-5,6-dihydropyrazine was studied.The reaction was comprised of synthesis of 2,3,5-trimethyl-5,6-dihydropyrazine and 2,3,5-trimethylpyrazine.(1) The optimum conditions of 2,3,5-trimethyl-5,6-dihydropyrazine synthesis were established: 2,3-butanedione which was mixed with anhydrous ethyl alcohol(the mass ratio of anhydrous ethyl alcohol to 2,3-butanedione was 5:1) was droped to the mixture of anhydrous ethyl alcohol and 1,2-diaminopropane(the mass ratio of anhydrous ethyl alcohol to 1,2-diaminopropane was 6:1) at the even pace for 3h,the molar ratio of 2,3-butanedione to 1,2-diaminopropane was 1:1.1,the condensation reaction temperature was -5℃.(2) The best dehydrogen oxidation conditions were as follows:air was used as oxidant,the molar ratio of potassium hydroxide and 2,3,5-Trimethyl-5,6-dihydro-pyrazine was 3:1,the mass ratio of ethanol to 2,3,5-trimethyl-5,6-dihydro-pyrazine 10:1,reaction temperature 68℃,reaction time 7h,the total yield of this two-step reaction was 83.0%.更多还原