含R2(dabco)及R(dabco)官能基SBA-15中孔分子篩的合成、鑑定及陰離子交換的應用

Synthesis,characterization and anion-exchangeable application of SBA-15 tethered with R2(dabco) and R(dabco)

梁維翰(Wei-Han Liang)

指導教授 ： 鄭吉豐

中原大學/理學院/化學研究所/碩士(2013年)

https://doi.org/10.6840/cycu201300969

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。應用在陰離子層析上，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63000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，應用在HPLC靜相上，有30000至50000左右的理論板數。
而以共縮合法合成雙邊結構來做六價鉻的離子交換，吸附一分鐘，吸附量為71%至88%Cr(VI)平衡吸附量(qe)，約在30分鐘內就以已達吸附平衡，材料快速吸附行為是文獻上少見，主要由於吸附材具有利於擴散及輸送大奈米孔洞及高表面積、Si-OH親水性，不同於傳統高分子結構特性。在不同pH值的條件下，在pH值3時1kg材料可以交換192g的Cr(VI)，證明具有吸附六價鉻的交換能力。

關鍵字

陰離子交換 ； 離子層析

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 anion-exchange stationary phase in HPLC and absorbents for hexavalent chromium anion. Silane-functionalized mesoporous silicas materials were prepared using the post-synthesis and co-condensation and characterized by X-ray diffraction, N2 adsorption/desorption isotherm, fourier transform infrared spectrometry, elemental analysis, thermogravimetric analysis, scanning electron microscopy, solid-state nuclear magnetic resonance.
In post-synthesis, calcined SBA-15 mesoporous sieves were surface-modified with the synthesized unilateral and bilateral amine silane. In one pot reaction, silane-functionalized mesoporous silicas were also prepared via the co-condensation of amine silane and tetraethoxylsilane(TEOS) with different ratio of X = silane/(silane + TEOS).
The anion-exchange liquid chromatrography using above home-made stationary phase have higher separation efficiency with the number of theoretical plates about 30000 to 63000 compared with literature report. The parameters of the pH and flow rate of mobile phase were systematiclly studied in our anion-exchange liquid chromatrography.
Functionalized SBA-15 with bilateral amine was also used for hexavalent chromium ion exchange. The exchange capacities of amine-SBA-15 for Cr (VI) and chromate were 192 and 428 mg/g respectively. Its thermodynamics and kinetics were carefully examined.

並列關鍵字

ion chromatography ； ion-exchange

參考文獻

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

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