论文标题:NMR新技术的应用研究
The Applied Study of the New Technologies to NMR
论文作者 陆方
论文导师 严宝珍,论文学位 硕士,论文专业 分析化学
论文单位 北京化工大学,点击次数 119,论文页数 83页File Size1635k
2004-04-14论文网 http://www.lw23.com/lunwen_454741322/ 核磁共振;苯并恶嗪;笼型倍半硅氧烷;铝一有机配合物
NMR;benzoxazine;cage--like silsesquioxane;aluminum--organic matter complex
核磁共振波谱是当代化学中一种重要的谱学研究手段,随着各种新技术的诞生,已成为21世纪科学研究不可缺少的工具。本课题利用超导核磁共振的新技术进行了1H、13C、29Si、27A1 NMR以及异核多量子相关二维谱的应用研究。 在对十种苯并恶嗪类化合物微观结构的研究中,利用1H NMR、13CNMR,系统而详细的讨论了这类化合物的主体结构及其取代基质子与碳原子化学位移的影响因素,得出了这类化合物的NMR谱特征。将HMQC、HMBC两种多量子相关二维实验应用于这类化合物的结构研究并用于确认取代基较为复杂的苯并恶嗪类化合物。 通过对一类新型含硅材料一笼形倍半硅氧烷结构的研究,总结了这类化合物中29si NMR的影响因素,即取代基R的电负性是影响29si化学位移的主要因素,R电负性增强29Si化学位移移向高场。实验过程中,首先利用1H NMR、13C NMR确认了笼上硅原子取代基的结构;然后通过29Si NMR研究了取代基对29Si化学位移的影响。 本课题利用27A1 NMR对A1(III)的水解反应、与有机物的配合反应进行了初步研究。主要是选取水杨酸、邻苯二酚、问苯二酚、对苯二酚这四种简单有机酚类作为官能团模拟化合物,讨论了水溶液pH值、L/M这两种因素对铝与有机物配位反应的影响,为以后研究AI(III) 与有机物配合反应提供了有力的实验依据。
With the arising of new technology,NMR(nuclear magneticresonance spectroscopy)is becoming one of the important approaches tothe study of chemistry.We studied the application of NMR technologies by1H,13C,29Si,27A1 NMR and HMQC(Heteronuclear Multiple QuantumCoherence)spectrum. We studied the structures of a series of benzoxazine compounds by 1HNMR and 13C NMR,and discussed the influences to the chemicaldisplacement of the hydrogen and carbon on the main parts of thesecompounds.We also studied two kinds of benzoxazine compounds,whosesubstituent is complex,by HMBC and HMQC spectrum. Cage--like silsesquioxane is a kind of polyhedral compound,which iscomposited of organic and inorganic molecules.The structures of the cage—like silsesquioxane can be determined by 29Si NMR,effectively.Westudied the structures of six kinds of cage—like octa silsesquioxane by NMR. By the means of semiempirical calculations and empirical treatment,cornbining with the data we got,we could know that during the influenceof the silicon chemical shifts,the electronegativity of the substituent is themost important one.From the 1H,13C NMR,we could verdict the stuctureof the substituent of Cage--like silsesquioxane. We studied the hydrolysis and coordinating with some organiccompounds;such as salicylic acid,catechol et a1.;of Al(III)by 27A1 NMR.Several factors influencing the complexation of aluminum--organic matterwere discussed:the pH value of the solution,the L/M(1igand/metal)value;offering a reference to this study afterwards.
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