水热反应工艺条件对5,5’-联四唑-1,1’-二氧羟铵盐晶体尺寸的影响

Influence of Hydrothermal Reaction Conditions on Crystal Size of Dihydroxylammonium 5,5-Bistetrazole-1,1-diolate

工业品5,5’-联四唑-1,1’-二氧羟铵盐(TKX-50)的晶体尺寸较小,形貌不规则,直接影响TKX-50的广泛使用。针对TKX-50为羟胺盐的特性,实验选择了水热法对TKX-50进行重结晶,结果表明:水热法制备工艺简单,受外界条件影响小,制得的TKX-50晶体形貌较为统一规整,为菱形块状晶体;通过改变工艺条件还能够实现对晶体尺寸的可控。升温速率25℃·h^-1,保温时间0.5 h,降温速率5℃·h^-1时,制得的TKX-50晶体尺寸为0.3~0.4 mm;升温速率为25℃·h^-1,保温时间2 h,降温速率为3℃·h^-1时,制得的TKX-50晶体平均尺寸为2.4546 mm,最大晶体尺寸可达3.5 mm,通过水热法对TKX-50重结晶的收率为68%。

The application of dihydroxylammonium 5,5-bistetrazole-1,1-diolate(TKX-50)in industry is directly affected by its crystal size and morphology.Our experiment chose hydrothermal method to recrystallize TKX-50 based on the characteristics of TKX-50.The result showed that the hydrothermal method required less steps and was less dependent on the external conditions.The crystal morphology of TKX-50 was uniform and regular,and it was a diamond block crystal.Changing the process conditions could subsequently change the crystal size.When the heating rate was 25℃·h^-1,the holding time was 0.5 h,and the cooling rate was 5℃·h^-1,the size of the TKX-50 crystal was 0.3~0.4 mm.When the heating rate was 25℃·h^-1,the holding time was 2 h,and the cooling rate was 3℃·h^-1,the average size of TKX-50 crystal was 2.5 mm with a maximum up to 3.5 mm.The final yield of recrystallization of TKX-50 by hydrothermal method was of 68%.