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我国吡虫啉工业化合成路线探讨 总被引:1,自引:0,他引:1
回顾了我国吡虫啉工业化的历史,阐述了我国吡虫啉工业化的现状。对3-甲基吡啶氧化法、苄胺-丙醛环合法和3-甲基吡啶直接氯化法3种吡虫啉合成工艺路线进行了探讨和比较,并提出了其中存在的问题。认为3-甲基吡啶氧化法和苄胺-丙醛环合法有希望替代传统环戊二烯环合法合成吡虫啉。 相似文献
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以廉价原料丙醛制备了标题化合物.以丙醛与2-溴丙烷格氏试剂反应,经水解生成2-甲基-3-戊醇,后经50%过氧化氧氧化得标题化合物,总收率73%. 相似文献
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3-甲基吡啶(3-MPD)与4-甲基吡啶(4-MPD)主要来源于吡啶、3-甲基吡啶合成的副产物以及煤焦油,但由于两者是沸点十分相近(分别为144.14℃、145℃)的同分异构体,依靠传统的分离方法,如精馏、普通的溶剂萃取,无法将其分离开来。3-甲基吡啶与4-甲基吡啶混合体系的分离技术主要有化学转化法、共沸精馏法、反应蒸馏法、吸附分离法、解离萃取法以及其他方法。其中铜盐法在常压或低压下操作,操作安全可靠。适用于工业化生产。 相似文献
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以活性炭、尿素和FeCl_3·6H_2O为原料得到Fe(OH)3,通过N2气氛还原得到磁核Fe_3O_4/C,随后将其置于CaCl_2与MgCl_2·6H2O溶液中超声分散,通过共沉淀法得到前驱体,焙烧制得磁性非均相固体碱催化剂(CaOMgO)@Fe_3O_4/C。对磁性非均相固体碱催化剂〔(CaO-MgO)@Fe_3O_4/C〕进行了磁滞回线、X射线衍射(XRD)、透射电镜(TEM)、CO_2-TPD及N_2的吸附-脱附(BET)测试。结果表明,CaO-MgO均匀地分散在磁核Fe_3O_4/C表面,催化剂在700℃有个强峰,具有较强的碱强度,磁化强度为23.8 emu/g,显示出较好的磁性。以碳酸二甲酯与甘油制备碳酸甘油酯作为探针反应,考察了(CaO-MgO)@Fe_3O_4/C催化剂的催化性能,得到在温度为85℃,n(碳酸二甲酯)∶n(甘油)=5∶1,催化剂用量为甘油质量的3%,反应时间为1 h的条件下,碳酸甘油酯的收率达到98.80%,甘油的转化率达到99.48%。催化剂重复使用6次后,碳酸甘油酯的收率为94.45%。 相似文献
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A new process, coupling reaction and azeotropic distillation was proposed for the synthesis of glycerol carbonate (GC) from glycerol (G) and dimethyl carbonate (DMC). The bench scale experimental investigation was systematically conducted for this new process. With calcium oxide (CaO) as the solid catalyst, the high yield of glycerol carbonate can be obtained at a low molar ratio of dimethyl carbonate to glycerol with the method of coupling reaction and azetropic distillation. The effect of azeotropic agents on glycerol carbonate yield was explored, and indicated that benzene was the most effective azeotropic agent. The effects of the process parameters, tower height, amount of added benzene, final temperature of tower bottom and reflux ratio were investigated. Glycerol carbonate yield can be as high as 98% under the conditions at molar ratio of dimethyl carbonate to glycerol 1:1, final temperature of tower bottom 85 °C, 1.5 mass ratio of added benzene to that in the azeotrope with methanol theoretically produced and reflux ratio 4. By continuously removing methanol from reaction system with the method of coupling reaction and azeotropic distillation, the yield of glycerol carbonate can be retained at high level using the recycled catalyst. 相似文献
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以苯甲醛和甘油为原料,通过活性炭负载磷钨酸(TPA)为催化剂,催化合成苯甲醛甘油缩醛。分别研究了催化剂磷钨酸负载量、反应时间、反应物配比及催化剂用量对合成反应的影响。结果表明,TPA负载量(质量分数)15%,催化剂用量(质量分数)4%,苯甲醛:甘油=1:1.1(摩尔比),反应时间2.0h,苯甲醛甘油缩醛的收率可达96.4%。 相似文献
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Biodiesel produced from crude Jatropha curcas L.oil with trace sulfuric acid catalyst(0.02%-0.08% oil) was investigated at 135-184 ℃.Both esterification and transesterification can be well carried out simultane-ously.Factors affecting the process were investigated,which included the reaction temperature,reaction time,the molar ratio of alcohol to oil,catalyst amount,water content,free fatty acid(FFA) and fatty acid methyl ester(FAME) content.Under the conditions at 165 ℃,0.06%(by mass) H2SO4 of the oil mass,1.6 MPa and 20:1 methanol/oil ratio,the yield of glycerol reached 84.8% in 2 hours.FFA and FAME showed positive effect on the transesterification in certain extent.The water mass content below 1.0% did not show a noticeable effect on trans-esterification.Reaction kinetics in the range of 155 ℃ to 175 ℃ was also measured. 相似文献