【作者】 鲍碧清；

【导师】 章文贡；

【作者基本信息】 福建师范大学 ， 材料加工工程， 2007， 硕士

【摘要】 采用Kiliani氧化—Wolff-kishner还原路线合成酮式胆汁酸及胆烷酸，产物经红外光谱、薄层色谱、元素分析、核磁共振谱等表征确证。采用共沉淀法、水热法实现了胆烷酸根在Zn-Al水滑石(LDHs)层间的超分子组装，并用XRD、FT-IR、DSC-TG、TEM和变温磁化强度(SQUID)等手段对样品进行表征，结果表明，直接共沉淀法得到的胆烷酸根插层LDHs结晶度较高、晶相较单一，胆烷酸根在LDHs层间呈与LDHs板层接近平行的有序排列，其磁化率与温度关系表明样品呈现反铁磁交换作用；水热法得到的胆烷酸根插层LDHs，胆烷酸根在LDHs层间呈单层、上下交叉且垂直于层板高度有序排列。采用水热法制备了脱氧胆酸根插层Zn-Al水滑石(LDHs)，建立了脱氧胆酸根插层水滑石的超分子结构模型，即脱氧胆酸根阴离子通过静电力和氢键与LDHs层板相互作用，在层间呈单层、倾斜于层板有序排列。制备了各类正相及反相组装态胆烷酸盐，采用变温磁化强度(SQUID)对其磁学性能进行表征与分析，结果表明，样品主要呈反铁磁性。更多还原

【Abstract】 The synthesis of cholanic acid was studied using cholic acid as starting material. Structure of the product is characterized by IR, TLC, elementary analysis, and ¹H NMR. Then cholanic acid was succefully intercalated into the Zn-Al Hydrotalcite compound by coprecipition method and hydrothermal method, the sample thereby obtained was characterized using several physicochemical techniques, i.e., XRD、FT-IR、DSC-TG、TEM and SQUID. Results indicated that cholanic acid-pillared Zn-Al hydrotalcite compound with good crystallinity cound be prepared by coprecipition method. Experimental data suggest the anion molecules form a paralleled layer, with the carboxylate groups pointing towards the brucite layers.χ^-1～T pattern of the samples show that they all bear antiferromagnetic exchange effect. While the LDH-cholanic intercalation compound synthesized by novel hydrothermal reaction show a different orientation, the cholanic anion form a single perpendicular layer in the interlayer space where the anionic substituents are thought to orient crosswise with each other to the surface of the cationic brucite-like sheet by electrostatic interactions. For the sample with deoxycholate prepared by hydrothermal method, we propose a supramolecular structure which the cholate anions form a tilted layer with their carboxylate groups pointing toward the brucite layer by electrostatic attraction and hydrogen bonding. In addition, the self-assemble cholanic salts are prepared, and their magnetic properties are characterized using SQUID, results show that there are antiferromagnetic exchange effect.更多还原