微波水熱法合成鋅膨潤石

Synthesis of Zn-smectite with microwave-hydrothermal process

張鎮宇(Chen-Yu Chang)

指導教授 ： 余炳盛

國立臺北科技大學/工程學院/資源工程研究所/碩士(2011年)

摘要

本研究以微波水熱法合成鋅膨潤石，並控制化學式x值、溫度、時間、鈉添加量等條件，比較鋅膨潤石產物之純度、比表面積、陽離子交換容量，探討微波水熱法合成膨潤石較佳參數。
研究結果顯示，根據化學式Na2x[Al2(1-x)M2x□u]Si4O10(OH,F)2∙nH2O配製前驅物，採用SiO2-Al(OH)(CH3COO)2-Zn(CH3COO)2-NaCOOCH3系統，較為容易結晶形成膨潤石，配比x=0.3、0.4、0.5均可合成鋅膨潤石，溫度低於190℃、時間不長於15小時，其結晶成長及性質提升與溫度、時間為正相關，但當溫度達200℃或時間20小時則導致產物結晶性較差與陽離子交換容量較小等負面影響。
使用配比x=0.3、0.4、0.5，鈉適度添加Na=2x+0.2可有效提升產物之鋅膨潤石純度，且相較於鈉過量添加Na=4x+0.2，增加x=0.4產物比表面積高達55.32 m2/g，而產物陽離子交換容量則分別為72.25、84.22、90.63meq/100g，因此鈉添加量Na=2x+0.2有助於提升產物之性質。
本研究以CTAB進行表面改質，以FT-IR檢測產物表面官能基以及以XRD檢測膨潤石層間膨脹情形，顯示成功將產物進行表面改質，而CTAB分子於膨潤石層間則以Pseudo-trilayer排列。

關鍵字

微波水熱法 ； 鋅膨潤石 ； 比表面積 ； 陽離子交換容量 ； 表面改質

並列摘要

Zn-smectite is synthetized by Microwave-hydrothermal process in this study, and control conditions as chemical x-value, temperature, time, the content of sodium. The better parameters of microwave-hydrothermal synthesis Zn-smectite are discussed by comparing Zn-smectite product's purity, specific area, cation exchange capacity.
The results show that, preparation of precursors according to the chemical formula Na 2x [Al2(1-x)M2x□u]Si4O10(OH,F)2∙nH2O, and the use of SiO2 - Al(OH)(CH3COO)2 - Zn(CH3COO)2 - NaCOOCH3 system are more likely to crystallize the formation of Zn-smectite. The parameters are controlled as ratio x = 0.3, 0.4, 0.5, below 190oC, and time of synthesis is no longer than 15 hours, growth of crystal and increase of property are positive to temperature and time. However, temperature reaches 200oC or time reaches 20 hours are resulted in poor crystalline product with smaller cation exchange capacity and other negative effects.
The ratio x = 0.3, 0.4, 0.5 of chemical formula and sodium content of precursor Na=2x+0.2 enhance the purity of Zn-smectite effectively, compared with sodium content of precursor Na=4x+0.2, increases specific area 55.32 m2/g of product(x=0.4), while cation exchange capacity of products are 72.25, 84.22, 90.63 meq/100g. The sodium content Na=2x+0.2 of precursor help to improve the property of product.
In this study, surface modification of product is proceeding by CTAB. FT-IR analyze the surface functional groups of product and XRD analyze Zn-smectite interlayer expansion of the case. The results indicate the success of the product specific area modification, while the CTAB molecules organize Pseudo-trilayer in Zn-smectite interlayer.

並列關鍵字

Microwave-hydrothermal process ； Zn-smectite ； specific area ； cation exchange capacity ； surface modification

參考文獻

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