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作 者:徐进云[1,2] 贾辉[1,2] 杨俊玲[1] 齐东来[1]
机构地区:[1]天津工业大学环境与化学工程学院,天津300387 [2]天津工业大学天津市纺织纤维界面处理技术工程中心,天津300270
出 处:《天津工业大学学报》2017年第2期25-30,共6页Journal of Tiangong University
基 金:国家自然科学基金资助项目(21202117)
摘 要:为了探究壳寡糖铁(Ⅲ)的配位结构和最佳合成条件,通过自制壳寡糖(黏均相对分子质量<1 000)与FeCl_3溶液的反应,合成了壳寡糖铁(Ⅲ)配合物.采用可见分光光度计测定反应前后溶液中Fe^(3+)浓度的变化,探究溶液pH值、反应温度以及反应时间对Fe^(3+)与壳寡糖配位反应的影响.利用紫外光谱(UV)、红外光谱(IR)、差热与热重分析(TGA-DSC)、元素分析(EI)等方法对配合物进行表征.结果表明:Fe^(3+)参与反应的配位量随着pH增加而增大,当pH>3.5时Fe^(3+)形成沉淀导致配位反应无法进行;Fe^(3+)参与反应的配位量随着反应时间的延长和反应温度的提高而增大,直至配位反应趋于平衡,考虑到实际生产周期和能源消耗,选择最佳反应时间为60 min,最适宜反应温度为40℃;形成的配合物热稳定性较壳寡糖本身的热稳定性有所提高,配合物中壳寡糖与Fe^(3+)的摩尔配位比为3∶1,并由此确定了配合物的结构式.In order to investigate the coordination structure and synthesis conditions of chitooligosaccharide- Fe ( Ⅲ ), ferric trichloride and self-made chitooligosaccharide whose viscosity-average molecular weight was less than 1 000 were used to synthesize chitooligosaccharide-Fe ( Ⅲ)complex. The concentration of Fe^3+ before and after reaction was measured by vis-spectrophotometer, and the effects of pH, temperature and reaction time on the complexation reaction were explored. The structure of chitooligosaccharide-Fe ( Ⅲ)complex was characterized by IR,visible ultraviolet (UV) ,thermogravimetric analysis and differential scanning calorimetry (TGA-DSC) and elemental analysis (EA). The experimental results showed that the amount of Fe^3+ involved in coordination reaction increased with augment of pH,and when the pH of solution was beyond 3.5,the coordination reaction could not be carried out due to Fe^3+ forming precipitate. With the increase of the reaction time and temperature,Fe^3+ coordination quantity increased until the coordination reaction gradually tended to be balanced. Considering the actual production cycle and energy consumption, the optimum reaction time and temperature were 60 min and 40 ℃,respectively. Relative to the thermal stability of chitooligosaccharide, the thermal stability of complexes improved. The ratio of Fe ( Ⅲ )to chitooligosaccharide was 3: 1,therefore the structural fomula of complex was determined.
关 键 词:壳寡糖铁(Ⅲ)配合物 pH值影响 Fe^3+浓度 表征 配位比
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