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On the thermal decomposition of zinc hydroxide nitrate, Zn5(OH)8(NO3)2⋅2H2O
Journal of Solid State Chemistry ( IF 3.3 ) Pub Date : 2020-03-06 , DOI: 10.1016/j.jssc.2020.121311
Amir Moezzi , Pin-Shyan Lee , Andrew M. McDonagh , Michael B. Cortie

The layered basic hydroxide Zn5(OH)8(NO3)2⋅2H2O can be thermally decomposed to ZnO via a series of intermediary compounds. Application of in situ X-ray diffraction to dry powder samples reveals three reactions: formation of anhydrous Zn5(OH)8(NO3)2, then de-hydroxylation to Zn3(OH)4(NO3)2 and, finally, decomposition of the latter to ZnO. In contrast, thermal analysis and mass spectroscopy of the evolved volatiles suggests that four reactions take place. Whereas de-hydroxylation reactions only produce H2O, there is also a distinctive pulse of NOx and O2 at the end of the sequence of reactions. The evidence points to the formation of an intermediate, poorly crystalline phase with a stoichiometry of [Zn(OH)2-x]⋅[NO3]x (1 < x < 2) during the final stages of the reaction sequence. Isothermal calcination of Zn5(OH)8(NO3)2⋅2H2O at 120 °C showed that the anhydrous Zn5(OH)8(NO3)2 compound is unstable, rehydrating very rapidly on cooling or decomposing within 6 or 7 h at 120 °C to Zn3(OH)4(NO3)2 (at a rate of 1.33 × 10-4 s-1). Zn3(OH)4(NO3)2 itself decomposes slowly to ZnO at 120 °C, but the process is slower (5.33 × 10-6 s-1) and there was still considerable Zn3(OH)4(NO3)2 present even after 140 h. The mixtures of Zn3(OH)4(NO3)2 and ZnO prepared by calcination are unstable under ambient conditions and react with moisture to reform Zn5(OH)8(NO3)2⋅2H2O.



中文翻译:

硝酸氢氧化锌的热分解,锌5(OH)8(NO 32 ⋅2H 2 ö

层状碱性氢氧化物的Zn 5(OH)8(NO 32 ⋅2H 2 O可被热经由一系列中间化合物的分解的ZnO。的应用原位X射线衍射到干粉样品揭示了三个反应:形成无水的Zn 5(OH)8(NO 32,然后脱羟基化对于Zn 3(OH)4(NO 32最后,后者分解为ZnO。相反,对析出的挥发物的热分析和质谱表明发生了四个反应。脱羟基反应仅产生H 2 O,但在反应序列结束时还有一个独特的NO x和O 2脉冲。证据表明 ,在反应序列的最后阶段,形成了化学计量比为[Zn(OH)2- x ]·[NO 3 ] x(1 <  x <2)的中间结晶性较弱的相。锌等温煅烧5(OH)8(NO 32 ⋅2H在120°C下的2 O表明无水Zn 5(OH)8(NO 32化合物不稳定,在冷却后迅速复水或在120°C下6或7 h内分解为Zn 3(OH)4(NO 32(速率为1.33×10 -4 s -1)。Zn 3(OH)4(NO 32本身在120°C时缓慢分解为ZnO,但过程较慢(5.33×10 -6 s -1),并且仍然存在大量的Zn 3(OH)4(NO 32即使在140小时后仍然存在。Zn组成的混合物3(OH)4(NO 32和ZnO制备通过煅烧在环境条件下是不稳定的,并与水分反应的Zn改革5(OH)8(NO 32 ⋅2H 2 O.

更新日期:2020-03-06
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