生物兼容法制备钛胶整体柱及在糖类分离中的应用
发布时间：2018-07-25 17:36
【摘要】：二氧化钛机械强度高,pH稳定性好,具有离子交换和配体交换的性质,能够选择性吸附带磷酸基团的物质,不存在硅胶固定相对碱性化合物不可逆吸附的问题,被认为是一种新兴的、有着光明应用前景的HPLC基质。 本课题的研究包括三个部分: (1)通过溶胶-凝胶方法合成钛胶基质整体材料,严格控制起始原料中各组分的配比、加水时的条件、水的浸泡处理以及干燥速率。实验表明,GT14~18,R=14~18,PEO为0.4%~0.6%这样范围的原料配比均有可能合成外貌特征理想的整体材料。 (2)对所制得的整体材料进行宏观乃至微观的表征。结果表明,我们所合成的整体材料外观形貌较好,介孔的比表面积很大;SEM电镜照片也较为理想,呈现出大孔-中孔的连续网络结构,且颗粒间交联紧密;经X-射线衍射后发现其内部晶型结构比较均匀,主要以锐钛矿型存在;唯一不足的可能是材料内部的孔径分布比较宽泛,不甚理想,还需改进实验条件。 (3)用钛胶基质色谱柱分析糖类化合物,优化出最佳洗脱条件,即以pH9.7的NaOH水溶液为流动相,柱温40℃进样量为20μL,流速为1.0mL/min。并变化柱温,探究柱温变化对糖在钛胶上保留的影响,并计算出相应的物理化学常数。研究揭示了:糖在钛胶上的保留能力随柱温上升而减弱。
[Abstract]:Titanium dioxide has high mechanical strength and good pH stability, it has the properties of ion exchange and ligand exchange, it can selectively adsorb substances with phosphoric acid group, and there is no problem of irreversible adsorption of silica gel immobilized relative basic compounds. It is considered to be a new HPLC substrate with bright application prospects. The research includes three parts: (1) Titanium matrix material is synthesized by sol-gel method, the proportion of each component in the starting material is strictly controlled, the conditions of adding water, the soaking of water and the drying rate are strictly controlled. The experimental results show that the ratio of raw materials in the range of 0. 4% to 0. 6% can be used to synthesize the whole material with ideal appearance. (2) the whole material is characterized macroscopically and microscopically. The results show that the synthesized materials have good appearance, and the mesoporous surface area is very large. The SEM SEM photos are also ideal, showing the continuous network structure of macroporous and mesoporous, and the intergranular crosslinking is close. After X-ray diffraction, it is found that the crystal structure of the material is relatively uniform, which mainly exists in anatase type, but the only deficiency is that the pore size distribution inside the material is relatively broad and not ideal. (3) the optimum elution conditions were obtained by using titanium gel matrix chromatography column to analyze the sugar compounds. The optimum elution conditions were as follows: the NaOH aqueous solution of pH9.7 was used as mobile phase, the injection amount was 20 渭 L at 40 鈩，
本文编号：2144543
[Abstract]:Titanium dioxide has high mechanical strength and good pH stability, it has the properties of ion exchange and ligand exchange, it can selectively adsorb substances with phosphoric acid group, and there is no problem of irreversible adsorption of silica gel immobilized relative basic compounds. It is considered to be a new HPLC substrate with bright application prospects. The research includes three parts: (1) Titanium matrix material is synthesized by sol-gel method, the proportion of each component in the starting material is strictly controlled, the conditions of adding water, the soaking of water and the drying rate are strictly controlled. The experimental results show that the ratio of raw materials in the range of 0. 4% to 0. 6% can be used to synthesize the whole material with ideal appearance. (2) the whole material is characterized macroscopically and microscopically. The results show that the synthesized materials have good appearance, and the mesoporous surface area is very large. The SEM SEM photos are also ideal, showing the continuous network structure of macroporous and mesoporous, and the intergranular crosslinking is close. After X-ray diffraction, it is found that the crystal structure of the material is relatively uniform, which mainly exists in anatase type, but the only deficiency is that the pore size distribution inside the material is relatively broad and not ideal. (3) the optimum elution conditions were obtained by using titanium gel matrix chromatography column to analyze the sugar compounds. The optimum elution conditions were as follows: the NaOH aqueous solution of pH9.7 was used as mobile phase, the injection amount was 20 渭 L at 40 鈩，
本文编号：2144543
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