本文選題：單分散 + 二氧化硅微球�。� 參考：《華東理工大學(xué)》2017年碩士論文

【摘要】：隨著高效液相色譜(HPLC)在化工、醫(yī)藥、環(huán)境等領(lǐng)域的廣泛應(yīng)用,人們對(duì)HPLC提出了更高的要求,色譜填料作為HPLC的核心,是色譜研究中最為關(guān)鍵的部分。單分散介孔硅膠微球依然是應(yīng)用最為廣泛的高效液相色譜基質(zhì)材料。為了提高色譜柱的分離效率,選擇性和穩(wěn)定性,小顆粒硅膠和雜化硅膠等新型材料成為液相色譜填料新的發(fā)展方向。本論文研究了新型的亞2 μm小顆粒介孔二氧化硅微球和有機(jī)-無機(jī)雜化介孔硅膠微球的合成方法及其在高效液相色譜中的應(yīng)用。在溶膠-凝膠法的基礎(chǔ)上,采用非離子表面活性劑十二胺為模板劑,十二胺聚氧乙烯醚為擴(kuò)孔劑,制備了亞2 μm單分散介孔二氧化硅微球,用十八烷基二甲基氯硅烷鍵合后作為反相色譜固定相,應(yīng)用于超高效液相色譜(UPLC)。詳細(xì)考察了溶膠-凝膠過程中,醇水比例和反應(yīng)溫度對(duì)硅膠微球形貌的影響,老化溫度和時(shí)間等因素對(duì)孔徑的影響。其中,通過控制甲醇和水的比例在2.4:1到4:1的范圍內(nèi),可以得到粒徑為0.4～2 μm單分散二氧化硅微球;通過調(diào)節(jié)老化溫度和時(shí)間,可在4.4～11.6 nm范圍內(nèi)調(diào)節(jié)孔徑的大小,對(duì)制備的反相C18柱進(jìn)行了動(dòng)力學(xué)和反相保留行為的評(píng)價(jià)。參照單分散介孔二氧化硅微球合成的實(shí)驗(yàn)條件,以乙烯基三甲氧基硅烷和正硅酸乙酯為混合硅源,通過共縮聚法制備了乙烯基有機(jī)-無機(jī)雜化介孔硅膠微球,研究了硅源比例TEOS/VTMS對(duì)雜化硅膠形貌和孔徑的影響。在水熱后處理的過程中,以AC1210為擴(kuò)孔劑的基礎(chǔ)上,并加入一定濃度的氟化銨來進(jìn)一步擴(kuò)大孔徑。最終采用TEOS/VTMS為5:1的硅源比例合成乙烯基雜化材料,將制備的2.3 μm雜化硅膠微球在100℃下老化12小時(shí),得到了比表面積351 m2/g,孔徑7.2 nm的乙烯基有機(jī)-無機(jī)雜化介孔硅膠微球。通過巰基-烯點(diǎn)擊化學(xué)反應(yīng)在硅膠表面引入半胱氨酸,制備了親水色譜固定相,并對(duì)色譜柱在親水模式下對(duì)極性化合的保留行為進(jìn)行了研究。
[Abstract]:With the wide application of high performance liquid chromatography (HPLC) in the fields of chemical industry, medicine, environment and so on, people put forward higher requirements for HPLC. As the core of HPLC, chromatographic packing is the most important part of chromatographic research. Monodisperse mesoporous silica gel microspheres are still the most widely used matrix materials for high performance liquid chromatography (HPLC). In order to improve the separation efficiency, selectivity and stability of chromatographic column, new materials, such as small particle silica gel and hybrid silica gel, have become the new development direction of liquid chromatographic packing. In this paper, a new type of mesoporous silica microspheres with sub2 渭 m particles and organic-inorganic hybrid mesoporous silica microspheres were synthesized and their applications in high performance liquid chromatography (HPLC) were studied. Based on the sol-gel method, the monodisperse mesoporous silica microspheres of 2 渭 m were prepared by using dodecylamine as template and dodecylamine polyoxyethylene ether as pore expander. Octadecyl dimethyl chlorosilane was used as a stationary phase in reversed phase chromatography and applied to ultra-high performance liquid chromatography (UPLC). The effects of alcohol-water ratio and reaction temperature on the morphology of silica gel microspheres, aging temperature and time on the pore size were investigated in detail. By controlling the ratio of methanol to water in the range of 2.4: 1 to 4:1, the monodisperse silica microspheres with a particle size of 0.4 渭 m can be obtained, and the pore size can be adjusted in the range of 4.4 渭 m 11.6 nm by adjusting the aging temperature and time. The kinetics and retention behavior of the prepared reversed C 18 column were evaluated. According to the experimental conditions for the synthesis of monodisperse mesoporous silica microspheres, vinyl trimethoxysilane and ethyl orthosilicate were used as the mixed silica source to prepare vinyl organic-inorganic hybrid mesoporous silica microspheres by co-condensation. The effect of silicon source ratio TEOS / VTMS on the morphology and pore size of hybrid silica gel was studied. In the process of hydrothermal treatment, the pore size was further expanded by adding a certain concentration of ammonium fluoride on the basis of AC1210 as the pore expander. Finally, the vinyl hybrid material was synthesized by using the ratio of TEOS / VTMS at 5:1. The prepared 2.3 渭 m hybrid silica gel microspheres were aged at 100 鈩，

本文編號(hào)：2053798