磁性纳米磺酸的制备及催化的有机化学反应
发布时间：2018-11-13 17:08
【摘要】：酸是化学物质中一类重要的物质,可以参加多种化学反应,可以作为溶剂,最重要的是作为催化剂,加快反应的速率。磺酸作为酸的代表,是常用的酸催化剂的一种,可以参加氧化还原反应、聚合反应、加成反应等。由于磺酸应用广泛,但其污染严重,需要研究一种新型磺酸。近几年,磁性纳米材料成为化学领域的一个热点,受到人们的广泛关注。它们是一种不溶性的载体,具有颗粒小、比表面大、表面带有可修饰的基团等优点。磁性纳米材料有很多种,铁酸钴(Co Fe2O4)是一种较为理想的磁性纳米材料载体,它具有较好的化学稳定性,同时具有廉价、易得、低毒、磁性强等优点。本文将磺酸与磁性纳米材料铁酸钴(Co Fe2O4)结合制得一种高效可循环的磁性纳米磺酸催化剂-铁酸钴壳聚糖磺酸(Co Fe2O4@Cs-SO3H),用扫描电镜(SEM)、透射电镜(TEM)、X-射线衍射(XRD)等对其进行了表征。在无溶剂条件下,催化水合肼、邻苯二酸酐、芳香醛和1,3-二酮一锅四组分反应,在较短时间内合成酞嗪衍生物。反应完成后,利用磁铁将催化剂从粗产物中分离,避免了传统的离心、过滤等繁琐的步骤。并对催化剂进行了多次重复利用,且不失活性。酰胺衍生物作为重要的物质,对多种药物的合成具有重要的意义。本文制备了磁性纳米材料铁酸钴负载磺酸(Co Fe2O4@Si O2-DASA),通过扫描电镜(SEM)、透射电镜(TEM)、X-射线衍射(XRD)等对其进行了表征。研究表明,该催化剂可在无溶剂条件下催化腈和醇的反应,制备了一系列酰胺衍生物。反应完后,催化剂可通过磁性分离,重复使用6次,此后反应活性没有降低,从而发展了一种制备酰胺的新方法。喹唑啉衍生物是一类非常重要的有机化合物,它是许多天然生物碱的结构单元。近几年,由于它们巨大的生物活性和药物活性而受到化学药剂师的青睐。我们制备了催化剂Co Fe2O4@Si O2-SBSAN,对制得的催化剂进行了表征,重复实验的验证。研究表明,该催化剂可在乙醇为溶剂的条件下催化靛红、2-氨基二苯甲酮和草酸铵一锅三组分反应合成喹唑啉衍生物。催化剂经可以很容易地通过用磁铁分离回收和再循环利用。
[Abstract]:Acid is an important class of chemical substances, which can take part in many chemical reactions, can be used as a solvent, and most importantly, as a catalyst, to accelerate the reaction rate. Sulfonic acid, as the representative of acid, is one of the commonly used acid catalysts. It can participate in redox reaction, polymerization, addition reaction and so on. Because sulfonic acid is widely used, but its pollution is serious, it is necessary to study a new type of sulfonic acid. In recent years, magnetic nanomaterials have become a hot spot in the field of chemistry. They are insoluble carriers with the advantages of small particle size, large surface size and modifiable groups on the surface. There are many kinds of magnetic nanomaterials. Cobalt ferrate (Co Fe2O4) is an ideal carrier of magnetic nanomaterials. It has good chemical stability, cheap, easy to obtain, low toxicity and strong magnetic properties. In this paper, a high efficient magnetic nanometer sulfonic acid catalyst, cobalt ferrate chitosan sulfonic acid (Co Fe2O4@Cs-SO3H), was prepared by combining sulfonic acid with magnetic nano-material cobalt ferrate (Co Fe2O4). (SEM), transmission electron microscopy (TEM),) was used to prepare the catalyst. It was characterized by X-ray diffraction (XRD) et al. Phthalazine derivatives were synthesized by catalytic reaction of hydrazine hydrate, phthalic anhydride, aromatic aldehydes and 1-tetanedione in a short time under solvent-free conditions. After the reaction was finished, the catalyst was separated from the crude product by magnets, avoiding the complicated steps of centrifugation and filtration. The catalyst was reused many times without losing its activity. As an important substance, amide derivatives play an important role in the synthesis of many drugs. In this paper, cobalt ferrate supported sulfonic acid (Co Fe2O4@Si O2-DASA) was prepared and characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and so on. The results showed that the catalyst could catalyze the reaction of nitrile and alcohol without solvent, and a series of amide derivatives were prepared. After the reaction, the catalyst can be separated by magnetic separation and reused for 6 times. After that, the activity of the catalyst has not decreased, so a new method of preparing amides has been developed. Quinazoline derivatives are very important organic compounds, which are the structural units of many natural alkaloids. In recent years, they have been favored by chemical pharmacists because of their great bioactivity and drug activity. The catalyst Co Fe2O4@Si O 2 SBSAN was prepared, and the catalyst was characterized and verified by repeated experiments. The results showed that the catalyst could be used to synthesize quinazoline derivatives from indigo red, 2-aminobenzophenone and ammonium oxalate. The catalyst can be easily recovered and recycled by magnets.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O621.251;TB383.1
本文编号：2329791
[Abstract]:Acid is an important class of chemical substances, which can take part in many chemical reactions, can be used as a solvent, and most importantly, as a catalyst, to accelerate the reaction rate. Sulfonic acid, as the representative of acid, is one of the commonly used acid catalysts. It can participate in redox reaction, polymerization, addition reaction and so on. Because sulfonic acid is widely used, but its pollution is serious, it is necessary to study a new type of sulfonic acid. In recent years, magnetic nanomaterials have become a hot spot in the field of chemistry. They are insoluble carriers with the advantages of small particle size, large surface size and modifiable groups on the surface. There are many kinds of magnetic nanomaterials. Cobalt ferrate (Co Fe2O4) is an ideal carrier of magnetic nanomaterials. It has good chemical stability, cheap, easy to obtain, low toxicity and strong magnetic properties. In this paper, a high efficient magnetic nanometer sulfonic acid catalyst, cobalt ferrate chitosan sulfonic acid (Co Fe2O4@Cs-SO3H), was prepared by combining sulfonic acid with magnetic nano-material cobalt ferrate (Co Fe2O4). (SEM), transmission electron microscopy (TEM),) was used to prepare the catalyst. It was characterized by X-ray diffraction (XRD) et al. Phthalazine derivatives were synthesized by catalytic reaction of hydrazine hydrate, phthalic anhydride, aromatic aldehydes and 1-tetanedione in a short time under solvent-free conditions. After the reaction was finished, the catalyst was separated from the crude product by magnets, avoiding the complicated steps of centrifugation and filtration. The catalyst was reused many times without losing its activity. As an important substance, amide derivatives play an important role in the synthesis of many drugs. In this paper, cobalt ferrate supported sulfonic acid (Co Fe2O4@Si O2-DASA) was prepared and characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and so on. The results showed that the catalyst could catalyze the reaction of nitrile and alcohol without solvent, and a series of amide derivatives were prepared. After the reaction, the catalyst can be separated by magnetic separation and reused for 6 times. After that, the activity of the catalyst has not decreased, so a new method of preparing amides has been developed. Quinazoline derivatives are very important organic compounds, which are the structural units of many natural alkaloids. In recent years, they have been favored by chemical pharmacists because of their great bioactivity and drug activity. The catalyst Co Fe2O4@Si O 2 SBSAN was prepared, and the catalyst was characterized and verified by repeated experiments. The results showed that the catalyst could be used to synthesize quinazoline derivatives from indigo red, 2-aminobenzophenone and ammonium oxalate. The catalyst can be easily recovered and recycled by magnets.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O621.251;TB383.1
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