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以四氢硼酸四乙基铵为原料,通过热解反应合成了十氢十硼酸双四乙基铵,并采用红外光谱(IR),核磁共振波谱(1H NMR,11B NMR)及元素分析对其结构进行了表征.采用差热-热重(DSC-TG)分析研究了其在氩气及氧气气氛下的热稳定性,发现其在氩气中仅发生热分解反应,放热量较小,而在氧气中则先分解,再发生氧化反应并放出大量的热.采用Kissinger方法及Coat-redfern方程得到其热分解主反应的动力学方程,并进一步通过热裂解原位池-傅里叶变换红外光谱(FTIR)联用技术和同步热分析-红外-质谱(DSC-TGFTIR-MS)联用技术研究了其热分解机理,推测在加热升温过程中,化合物在303.2℃下快速分解,气相产物主要为乙烷与少量氨气及氢气,固相产物为单质硼.
Using tetraethylammonium tetrahydroborate as raw material, bistetraethylammonium decahydrate was synthesized by pyrolysis reaction, and its content was determined by IR, 1HNMR and 11B NMR Structure was characterized.The thermal stability under argon and oxygen was studied by DSC-TG analysis, and it was found that only thermal decomposition reaction occurred in argon, the heat release was small, In oxygen, it decomposes first, then the oxidation reaction takes place and a large amount of heat is released.Kinetics equations of the thermal decomposition main reaction are obtained by Kissinger method and Coat-redfern equation, and further analyzed by pyrolysis in situ pool-Fourier transform infrared The mechanism of thermal decomposition was studied by FTIR and DSC-TG-MS. It is speculated that during heating and heating, the compound decomposed rapidly at 303.2 ℃. The main products of gas phase were For ethane and a small amount of ammonia and hydrogen, the solid phase product is elemental boron.