【摘要】：二氧化鈦機(jī)械強(qiáng)度高,pH穩(wěn)定性好,具有離子交換和配體交換的性質(zhì),能夠選擇性吸附帶磷酸基團(tuán)的物質(zhì),不存在硅膠固定相對(duì)堿性化合物不可逆吸附的問題,被認(rèn)為是一種新興的、有著光明應(yīng)用前景的HPLC基質(zhì)。 本課題的研究包括三個(gè)部分: (1)通過溶膠-凝膠方法合成鈦膠基質(zhì)整體材料,嚴(yán)格控制起始原料中各組分的配比、加水時(shí)的條件、水的浸泡處理以及干燥速率。實(shí)驗(yàn)表明,GT14~18,R=14~18,PEO為0.4%~0.6%這樣范圍的原料配比均有可能合成外貌特征理想的整體材料。 (2)對(duì)所制得的整體材料進(jìn)行宏觀乃至微觀的表征。結(jié)果表明,我們所合成的整體材料外觀形貌較好,介孔的比表面積很大;SEM電鏡照片也較為理想,呈現(xiàn)出大孔-中孔的連續(xù)網(wǎng)絡(luò)結(jié)構(gòu),且顆粒間交聯(lián)緊密;經(jīng)X-射線衍射后發(fā)現(xiàn)其內(nèi)部晶型結(jié)構(gòu)比較均勻,主要以銳鈦礦型存在;唯一不足的可能是材料內(nèi)部的孔徑分布比較寬泛,不甚理想,還需改進(jìn)實(shí)驗(yàn)條件。 (3)用鈦膠基質(zhì)色譜柱分析糖類化合物,優(yōu)化出最佳洗脫條件,即以pH9.7的NaOH水溶液為流動(dòng)相,柱溫40℃進(jìn)樣量為20μL,流速為1.0mL/min。并變化柱溫,探究柱溫變化對(duì)糖在鈦膠上保留的影響,并計(jì)算出相應(yīng)的物理化學(xué)常數(shù)。研究揭示了:糖在鈦膠上的保留能力隨柱溫上升而減弱。
[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，

本文編號(hào)：2144543