We synthesized tetramethylammonium silicate octamer and preliminarily studied its thermal stability by means of thermograrimetric analysis （TGA） and FTIR at different temperature. The putative mechanism for the dewatering mechanism of tetramethylammonium silicate octamer was explored based on TGA and temperature program-IR （TP-IR）. It is found that the composition and structure oftetramethylammonium silicate octamer changed as all its crystal water was lost. The optimal preparation conditions of tetramethylammonium silicate octamer were obtained： heated at 135 ℃, most of crystal water can be removed and the chemical composition and structure of tetramethylammonium silicate octamer can remain unchanged.%合成了水合八聚（四甲基铵）硅酸盐,通过热重分析法初步研究了八聚（四甲基铵）硅酸盐的热稳定性,利用热重分析法和升温红外法探讨了水合八聚（四甲基铵）硅酸盐的热稳定性和失水机理。结果表明：水合八聚（四甲基铵）硅酸盐失去全部结晶水会导致其化学组成和结构的变化。同时,在此基础上获得了加热干燥法制备无水八聚（四甲基铵）硅酸盐的优化工艺条件：在135℃下加热除水,不仅能够除掉体系中大部分的结晶水,还能保证八聚（四甲基胺）盐的化学组成和构型不发生变化,使其不发生分解。
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