第 50 卷第 1 期 Vol. 50 No. 1 2020 年 2 月 Feb 2020

所属栏目：功能材料 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

张 瑞，米登峰，和尚杰，申 通，吴晓青* （中北大学 理学院，山西 太原 030051）

摘　要：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2.454 6 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%。

关键词：TKX-50；重结晶；水热反应

中图分类号：TJ55　　文献标识码：A　　文章编号：1009-9212（2020）01-0061-05

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

ZHANG Rui, MI Deng-feng, HE Shang-jie, SHENG Tong, WU Xiao-qing* (North University of China, College of Science, Taiyuan 030051, China)

Abstract：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%.

Key words：TKX-50; recrystallization; hydrothermal reaction

作者简介：张 瑞（1995-），女，山西阳曲人，硕士研究生，主要从事含能材料的研究（E-mail：191090443@qq.com）。

联 系 人：吴晓青，教授（E-mail：1369680249@qq.com）。

收稿日期： 2020-02-1