中孔徑分子篩SBA-15之合成、鑑定及陰離子交換層析應用

Synthesis, characterization and application of anion exchangeable SBA-15 mesoporous molecular sieves

曾建霖(Chien-Lin Tseng)

指導教授 ： 鄭吉豐

中原大學/理學院/化學研究所/碩士(2011年)

https://doi.org/10.6840/cycu201101063

摘要

以後修飾直接在鍛燒過的中孔徑分子篩SBA-15孔洞表面修飾上四級胺的官能基，經由計算其值為1.39、1.62 mequiv./g ，相較於參考文獻上值(1.14 mequiv/g )高出許多，且RSD的都在2%以下，表示所測得有相當的精確度；應用在HPLC上，我們可以發現鍵結兩種修飾劑中孔徑分子篩靜其理論板數都高達50000左右，然而含單邊四級胺矽烷靜相在拖尾係數上表現較好。
另以共縮合的方法，在一鍋反應中，成功直接鍵結不同含量、不同矽烷修飾劑於中孔徑分子篩。鍵結較高比例矽烷產物有較高陰離子交換當量，一般而言，共縮合產物比後修飾產物具有較高陰離子交換當量，經由計算其exchange capacity其值可高達 2.43、3.06 mequiv./g，且RSD的表現都在2%以下，表示有相當的精確度；應用在HPLC靜相上，可以發現雙邊四級胺矽烷產物在理論板數與拖尾係數都比單邊好，有30000左右的理論板數，且在拖尾係數在1.2和1.5之間，相較於後修飾法產物在拖尾係數表現較佳。

關鍵字

陰離子交換 ； 層析

並列摘要

Silanes of unilateral and bilateral quaternary amine were successfully synthesized, characterized and surface-modified inside channels of SBA-15 as the ion-exchange and separation stationary phase of anions. Silane-functionalized mesoporous silicas materials were prepared and characterized using post-synthesis and co-condensation.
In post-synthesis, calcined SBA-15 mesoporous sieves were surfaced modified with the synthesized unilateral and bilateral silane. The ion-exchange capacities of SBA-15- unilateral and bilateral quaternary amine were 1.39 and 1.62 meq/g, respectively.
In co-condensation, silane-functionalized mesoporous silicas have been synthesized using co-condensation of silane containing quaternary amine and tetraethoxysilane (TEOS) in acidic medium with the block copolymer Pluronic 123 as the structure directing agent. The influence of synthesis parameters, the molar ratio of X = silane /( silane + TEOS) was studied. Ion-exchange capacities of SBA-15- unilateral and bilateral quaternary amine were 2.43 and 3.06 meq/g for silane containing unilateral and bilateral amine, respectively.
Products from both methods of modifications were used as HPLC stationary phase for the separation of anions having theoretical plate of about 50000 for post-synthesis and 30000 for co-condensation.

並列關鍵字

anion-exchange chromatography

參考文獻

1. McBain, J. W., The Sorption of Gases and Vapours by Solids, Rutledge and Sons, London, ch. 5, 1932.

2. IUPAC Manual of Symbols and Terminology, Appendix 2, Part 1,

8. Zuna, R. Colloids Surf. 1997, 27, 123.

9. Chen, C.; Li, H.; Daris, M. E. Microporous Mater. 1993, 2, 17.

17. Han, Y.; Wu, S.; Sun, Y. Y.; Li, D. S.; Xiao, F. S.; Liu, J.; Zhang, X. Z. Chem. Mater. 2002, 14, 1144.