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Textural and Structural Modification of Homo-ionic Montmorillonite

机译:均质蒙脱石的结构和结构改性

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The textural and structural modifications of calcium bentonite (CaB) induced by ion exchange, heat treatment and acid leaching were studied by infrared spectroscopy (IR), scanning electron microscopy (SEM) and nitrogen adsorption/desorption methods. The cation-exchange capacities (CEC) and the spontaneous and mechanical dispersion of the heat-treated samples were also measured. CaB taken from the northern coast of Egypt consisting of calcium montmorillonite (85%) and kaolinite, in addition to traces of quartz, was used in this study. CaB and its sodium and lithium forms, NaB and LiB, were calcined at 600 °C for times ranging from 2 h to 20 h, while selected calcined samples were leached with H_2SO_4 for 1 h. Upon heating, the decrease in the layer charge caused by the fixation of Ca~(2+), Na~+ and Li~+ ions in the structure, as revealed by the CEC values, led to an upward shift of the Si-0 stretching band in the IR spectrum to the frequency at which the Si-0 groups of pyrophyllite absorb. The CEC values showed that the layer charge of the homo-ionic montmorillonite decreased with increasing thermal treatment time and that the amounts of fixed cations were in the order: Li~+ > Na~+ > Ca2~+. The dispersability of the thermally-treated CaB was higher than that of NaB and LiB, both before and after mechanical dispersion. The high dispersability of CaB arises from the inability of the large Ca~(2+) cation to penetrate further into the lattice. The textural parameters of heated samples showed that the zig-zag alignment of the silicate chains varied as a function of the heat-treatment time, irrespective of the nature of the exchangeable cations. A significant increase in the amount of pores with diameters in the range 13-38 A was detected in the case of LiB. Heating LiB further for up to 20 h led to a slight increase in the specific surface area and pore volume, but with a considerable reduction in microporosity. On the other hand, thermal treatment after leaching led to a considerable increase in the specific surface areas, pore volumes and microporosities for those samples subjected to heating for a short time, but decreased progressively with increasing heating time, with no difference being observed to the exchangeable cations. This increase in surface area was mainly due to the presence of micropores whose formation was attributed to the leaching of octahedral cations. On the other hand, following calcination for a long time, the magnitude of the textural parameters diminished due to the gradual collapse of the microporous structure.
机译:通过红外光谱(IR),扫描电子显微镜(SEM)和氮吸附/解吸方法研究了离子交换,热处理和酸浸引起的膨润土钙(CaB)的组织和结构改性。还测量了热处理样品的阳离子交换容量(CEC)以及自发和机械分散性。在这项研究中,使用了来自埃及北部海岸的CaB,其中包括蒙脱石钙(85%)和高岭石,此外还有微量的石英。 CaB及其钠和锂形式的NaB和LiB在600°C下煅烧2 h至20 h,而选定的煅烧样品则用H_2SO_4浸提1 h。加热时,由CEC值揭示的结构中Ca〜(2 +),Na〜+和Li〜+离子的固定所引起的层电荷的减少导致Si-0向上移动红外光谱中的扩展带到叶蜡石的Si-0基团吸收的频率。 CEC值表明,随着热处理时间的增加,同离子蒙脱土的层电荷减少,固定阳离子的数量顺序为:Li〜+> Na〜+> Ca2〜+。在机械分散前后,热处理过的CaB的分散性均高于NaB和LiB。 CaB的高分散性源于大的Ca〜(2+)阳离子无法进一步渗透到晶格中。加热样品的结构参数表明,硅酸盐链的锯齿形排列随热处理时间而变化,而与可交换阳离子的性质无关。在LiB的情况下,发现直径在13-38 A范围内的孔数量显着增加。进一步加热LiB达20小时导致比表面积和孔体积略有增加,但微孔率显着降低。另一方面,浸出后的热处理导致那些短时间加热的样品的比表面积,孔体积和微孔率显着增加,但随着加热时间的增加而逐渐降低,与可交换阳离子。表面积的增加主要归因于微孔的存在,其形成归因于八面体阳离子的浸出。另一方面,长时间煅烧后,由于微孔结构的逐渐塌陷,质地参数的大小减小了。

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