5-磺基水杨酸与胺类衍生物系列共晶盐的筛选和性质研究

发布时间：2018-03-30 21:02

本文选题：机械化学　切入点：溶剂辅助研磨　出处：《辽宁大学》2017年硕士论文

【摘要】：近些年共晶及其盐在药物学、材料化学等领域受到越来越多的关注,共晶可以在不改变分子化学结构的同时达到改善物质的物理化学性能。如,在药学领域,可以通过共晶改善药物稳定性、水溶性、生物利用度等物理化学性质增强药效;在材料学领域,可以通过共晶改善光学活性,制备热致变色、光致变色和光致发光等的材料,为功能材料的研发提供新的途径。本文结合传统的溶液法和机械化学方法,应用于5-磺基水杨酸的系列共晶盐的形态筛选和制备,并探索晶体结构、晶型的转化、热力学和光学等性质。机械化学应用到共晶盐的筛选符合绿色化学‖的理念,与传统的溶液法相比,可以显著提高晶体筛选效率,并可以节省溶剂使用,减少副产物及环境污染。具体内容包括:(1)微量溶剂辅助研磨筛选5-磺基水杨酸(SA)与六次甲基四胺(B)的共晶盐,采用机械化学控制其相转变过程。用溶剂辅助研磨法和溶液法相结合,确定了1:1和1:2的2种不同化学计量比的共晶盐及其水合物的结构,TGA和PXRD发现其水合物和无水化物在一定条件下可以相互转化,进一步利用溶剂辅助研磨探索了不同化学计量比的晶型转化。(2)5-磺基水杨酸(SA)与三羟甲基氨基甲烷(THAM)不同计量比共晶盐的筛选及其结构转变。采用微量溶剂辅助的机械研磨法筛选出SA与THAM化学计量比为1:1的水合物(SA)1(THAM)1·0.5H2O的共晶盐;(SA)1(THAM)1·0.5H2O呈现可逆的失水吸水性能,即在加热时经历一个固态相变后失去水分子。通过粉末X-衍射解析了(SA)1(THAM)1的结构,直观的观察到结构转变过程中氢键的变化。(3)5-磺基水杨酸(SA)与4,4-二氨基二苯甲烷(DDM)共晶盐的筛选及其热致变色现象。由单晶衍射确定了SA与DDM的系列共晶盐的结构,发现了其一维孔道结构里包容了不同溶剂分子,探索了这些共晶盐的稳定性和热致变色性质,而且微小的结构变化可能导致了热致变色现象。
[Abstract]:In recent years, eutectic and its salts have attracted more and more attention in the fields of pharmacology, material chemistry, etc. Eutectic can improve the physical and chemical properties of substances without changing the molecular chemical structure. It can improve the drug stability, water solubility, bioavailability and other physical and chemical properties through eutectic. In the field of materials science, it can improve optical activity through eutectic to prepare thermochromic, photochromic and photoluminescence materials. This paper, combined with traditional solution method and mechanochemical method, has been applied to the morphological screening and preparation of a series of eutectic salts of 5-sulfosalicylic acid, and to explore the transformation of crystal structure and crystal form. Thermodynamic and optical properties. The application of mechanochemistry to the screening of eutectic salts accords with the idea of green chemistry. Compared with the traditional solution method, the efficiency of crystal screening can be improved significantly, and the use of solvent can be saved. Reducing byproducts and environmental pollution. Specific contents include: 1) screening of eutectic salts of 5-sulfosalicylic acid (SAA) and hexamethyltetramine (B) by solvent assisted grinding. The phase transition process is controlled by mechanochemistry. The solvent assisted grinding method is combined with the solution method. The structures of two kinds of eutectic salts with different stoichiometric ratios, 1:1 and 1:2, and their hydrates have been determined. TGA and PXRD show that hydrates and anhydrous compounds can be converted to each other under certain conditions. The crystal transformation of different stoichiometric ratios (SAA) and trihydroxymethyl aminomethane (THAM) were further investigated by solvent-assisted grinding. The structural transformation of the eutectic salts with different stoichiometric ratios was investigated. Mechanical grinding method was used to screen out the eutectic salt (SA1 / THAM) with a stoichiometric ratio of 1:1 (SA / THAM) of SA1 and THAM1 0.5H2O, which showed reversible water loss and water absorption. That is to say, the water molecule is lost after a solid phase transition during heating. The structure of THAM1 is analyzed by powder X-ray diffraction. The changes of hydrogen bonds in the process of structural transformation. The selection and thermochromic phenomenon of eutectic salts of SAA and 4DDBM) were observed. The structure of the series of eutectic salts of SA and DDM was determined by single crystal diffraction. It is found that different solvent molecules are contained in the one-dimensional pore structure, and the stability and thermochromic properties of these eutectic salts are explored, and tiny structural changes may lead to thermochromic phenomena.
【学位授予单位】：辽宁大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O621.3

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