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4-氨基吡啶电化学合成工艺研究 总被引:1,自引:0,他引:1
在阳离子隔膜电解槽用阴极恒电位的方法电化学合成了4-氨基吡啶,并对工艺条件进行了优化。循环伏安法表明,4-硝基氮氧化吡啶的还原过程有多个不稳定的中间产物生成。以铅粒为阴极,钛网镀二氧化铅为阳极阴极液pH=3,4-硝基氮氧化吡啶质量百分浓度为1%,硫酸铵为支持电解质,10%的硫酸溶液为阳极液,还原电量为200%的理论电量及50℃下4-氨基吡啶的收率达88.2%,电流效率44.1%。该工艺过程简单,收率高,是可望取代污染严重的铁粉还原的绿色合成路线。 相似文献
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4—氨基吡啶合成工艺及结构测定研究 总被引:5,自引:0,他引:5
以N-氧化吡啶为原料合成N-氧化-4-硝基吡啶,进而还原合成4-氨基吡啶,总产率达80%,通过质谱,红外光谱和核磁共振谱对产品进行了结构测定,证明了合成工艺的可靠性。 相似文献
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采用原子利用率、环境因子和环境商以及GREENSCOPE法对4-氨基吡啶的不同合成工艺过程进行了绿色评价. 与传统的铁粉还原和催化氢化过程相比,电化学还原方法具有明显的优势:工艺操作简单,反应收率高,生产成本低,具有环境友好和可持续性. 采用电化学方法还原硝基化合物制备氨基化合物符合绿色化学发展的趋势,满足可持续发展要求,在精细化工领域具有良好的应用前景. 相似文献
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2—氯—4—硝基吡啶的制备 总被引:2,自引:0,他引:2
以吡啶为起始原料,经氧化,硝化,氯化反应制得了合成除草剂,吡啶基苯脲类植物生长调节剂和吡啶基医药产品的重要中间体2-氯-4-硝基吡啶。 相似文献
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The product and the oxidative polycondensation reaction conditions of oligo-4-aminopyridine were studied by using NaOCl as oxidant. Oligo-4-aminopyridine (4-OAP) was synthesized from the oxidative polycondensation of 4-aminopyridine (4-AP) in an aqueous solution medium acidic and neutral between 25 and 60 °C by using NaOCl as oxidant. About 85% of 4-AP was converted to 4-OAP. The number average molecular weight, (Mn) mass average molecular weight (Mw) and polydispersity index (PDI) values of 4-OAP synthesized were found to be 270, 850 g mol−1 and 3.15, respectively, using NaOCl. The respective values of the Schiff base were 1721, 2256 g mol−1 and 1.31, respectively, using air oxygen and 2173, 2372 g mol−1 and 1.09, respectively, using NaOCl and 2749, 6432 g mol−1 and 2.33, respectively, using H2O2. At the optimum reaction conditions, the yield of oligo-2-[(pyridine-4-yl-imino) methyl] phenol (OPMP) were found to be 86% (H2O2) and 89% (NaOCl) and 95% (air oxygen). The 4-OAP and OPMP were characterized by 1H NMR, FT-IR, UV-Vis and elemental analysis. TG analysis showed to be stable of 4-OAP against thermo-oxidative decomposition. The weight loss of 4-OAP and its Schiff base oligomer was found to be 50, 86.39 and 71.78% at 525, 625 and 1000 °C, respectively. Also, new oligomeric Schiff base was synthesized from condensation of 4-AP with salicylaldehyde and their structures and properties were determined. During polycondensation reaction, a part of the azomethine (-CHN-) groups oxidized to carboxylic (-COOH) group. Thus, soluble fraction in water of oligo-2-[(pyridine-4-yl-imino) methyl] phenol involved in carboxylic (-COOH) (11%) group. Besides, the structure and properties of oligomer-metal complexes of oligo-2-[(pyridine-4-yl-imino) methyl] phenol (OPMP) with Cu(II), Ni(II) and Co(II) were studied. 相似文献
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采用CuO-ZnO/多孔陶瓷为粒子电极的三维电催化氧化技术,对氨氮与2-氨基吡啶模拟废水的电催化氧化降解中的竞争过程进行研究。考察了氨氮及氨氮与2-氨基吡啶直接氧化和间接氧化降解的情况,并分析了氨氮与2-氨基吡啶的竞争反应过程。结果表明:间接氧化过程更有利于氨氮的去除,并可降低硝酸盐氮的累积率,2-氨基吡啶主要通过直接氧化降解,不受氨氮和氯离子的影响,直接氧化条件下2-氨基吡啶开环产物与氨氮存在强烈的竞争现象,间接氧化对2-氨基吡啶开环产物与氨氮的降解都有提高,且氨氮的去除优先于2-氨基吡啶开环产物。因此,可以通过改变三维电催化体系的直接和间接氧化条件,调整氨氮与有机物的去除效果,并可应用于含氨氮有机废水处理的现场调试。 相似文献
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调吡脲中间体2-氯-4-氨基吡啶的合成技术 总被引:1,自引:0,他引:1
调吡脲是一种重要的植物生长调节剂,其中间体2-氯-4-氨基吡啶的合成研究对于提高调吡脲的品质及降低其价格具有重要意义。本文综述了2-氯-4-氨基吡啶的制备方法,并介绍了2-氯-4-氨基吡啶在调吡脲等杂环化合物合成方面的应用。 相似文献