水热体系合成锂皂石结构的演化和影响规律研究
Structure Development of Hectorite in Hydrothermal Crystallization Synthesis Process
作者单位
周春晖 浙江工业大学化工与材料学院, 杭州 310032 
杜泽学 石油化工科学研究院 北京 100083 
李小年 浙江工业大学化工与材料学院, 杭州 310032 
卢春山 浙江工业大学化工与材料学院, 杭州 310032 
葛忠华 浙江工业大学化工与材料学院, 杭州 310032 
摘要: 以氟化锂、氯化镁、水玻璃、氨水为主要原料,采用水热体系合成了锂皂石(Hectorite)。通过化学成分分析、粉末X-射线衍射(XRD)、场发射扫描电镜(SEM)、 傅立叶变换红外光谱(FTIR)、 热重和差示扫描量热(TG-DSC)、激光纳米粒度分析等技术,考察了晶化时间、原料比、晶化温度对锂皂石产物结构演化的影响规律。实验结果表明,采用水热晶化体系合成锂皂石,6 h后体系中即能生成锂皂石。在实验的6~49 h晶化时间范围内,体系为锂皂石、硅酸锂、氟化锂、氢氧化镁等组成的多相共存体系。经72 h晶化后生成结晶好的锂皂石。在水热晶化体系增加锂盐的量,有利于提高锂皂石结晶性,并能促进Li取代片层上六配位Mg,导致产生更高的层电荷和更多的层间可交换离子。提高水热晶化温度,对提高锂皂石产物结晶性有利。晶化时间短,锂皂石产物粒径小,结晶性差,但颗粒分布窄。晶化时间长,锂皂石产物粒径增大,结晶性好,热稳定性提高。
关键词: 锂皂石  水热合成  结晶性  粘土
基金项目: 
Abstract: Hectorite was synthesized in hydrothermal system by using lithium fluoride, magnesium chloride, water glass, and ammonium hydroxide as starting materials. The structure development in synthesis processes was investigated by chemical composition analysis, powder X-ray diffraction(XRD), field emission scanning electron microscopy(SEM),Fourier transform infrared spectroscopy(FTIR), thermogravimetry and differential scanning calorimetry(TG-DSC)and laser nano particle size analyzer. The influences of synthesis parameters such as crystallization time, hydrothermal temperature and reactant ratio on the structure development of hectorite were explored and discussed. Some hectorite could be formed in 6 h, and the crystallization was completed in 72 h. Between 6 and 49 h the hydrothermal systems comprised hectorite, lithium silicate, lithium fluoride, and magnesium hydroxide. The crystallinity of hectorite could be enhanced with more Li substitution for octahedral Mg when the amount of lithium fluoride increased, leading to somewhat higher layer charge, thus more exchangeable cations in the interlayers. With the increasing of the temperature of hydrothermal crystallization the crystallinity of hectorite increased accordingly. Under less crystallization time, the obtained hectorite had smaller particle sizes and narrow size distribution with poor crystallinity, on the contrary, the products was in better crystallinity with larger grain sizes and higher thermal stability when the crystallization time was long enough.
Keywords: hectorite  hydrothermal synthesis  crystallinity  clay
投稿时间:2005-03-06 修订日期:2005-05-19
摘要点击次数:  1747
全文下载次数:  1883
周春晖,杜泽学,李小年,卢春山,葛忠华.水热体系合成锂皂石结构的演化和影响规律研究[J].无机化学学报,2005,21(9):1327-1332.
查看全文  查看/发表评论  下载PDF阅读器
Support information: