火炸药学报

为了改善FOX-7的性能,采用喷雾重结晶法制备了细化FOX-7,研究了溶剂与非溶剂种类、药液质量浓度及搅拌速率对重结晶细化FOX-7晶体形貌的影响,确定了最佳工艺条件; 采用扫描电子显微镜(SEM)及粒度分析软件对细化FOX-7进行了粒径形貌表征; 采用X射线粉末衍射系统(XRD)、傅里叶变换红外光谱仪(FT-IR)、差示扫描量热仪(DSC)、12型落锤仪及WM-1型摩擦感度仪对微米级FOX-7晶体进行表征及性能测试。结果表明,最佳工艺条件为:溶剂-非溶剂为NMP-H2O,药液质量浓度为0.4g/mL,搅拌速率为450r/min,可获得平均粒径为1.81μm的微米级FOX-7晶体; 微米级FOX-7晶型与原料FOX-7相比未发生改变; 微米级FOX-7表观活化能比原料FOX-7提高了88.74kJ/mol,热爆炸临界温度提高了19℃,特性落高从82.3cm提升至136.1cm,摩擦感度从12%降至0; 表明微米级FOX-7比原料FOX-7具有更好的热安定性及更低的机械感度。

In order to improve the performance of FOX-7, the refined FOX-7 was prepared by the spray recrystallization method. The effects of solvent and non-solvent types, liquid mass concentration and stirring rate on the crystal morphology of refined FOX-7 were studied, and the optimal process conditions for the refined FOX-7 were determined. The morphology and particle size of the refined FOX-7 was characterized by using the scanning electron microscope(SEM)and particle size analysis software. The properties of micron FOX-7 were characterized and tested by using X-ray powder diffraction system(XRD), Fourier transform infrared spectrometer(FT-IR), differential scanning thermometer(DSC), type 12 drop hammer instrument and WM-1 friction sensitivity meter. The results showed that the optimal process conditions for obtaining the refined FOX-7 are as follows: solvent-nonsolvent is NMP-H2O, the liquid mass concentration is 0.4g/mL, the stirring rate is 450 r/min, and the micron FOX-7 crystals with an average particle size of 1.81μm can be obtained. The crystal form of micron FOX-7 has no change compared to the raw FOX-7. The apparent activation energy of micron FOX-7(88.74kJ/mol)is higher than that of the raw FOX-7, and the critical temperature of the thermal explosion is increased by 19℃. The characteristic drop height is increased from 82.3cm to 136.1cm, and the friction sensitivity decreased from 12% to 0. It shows that the micron FOX-7 has better thermal stability and lower mechanical sensitivity than that of the raw FOX-7.

引言
1 实验
2 结果与讨论
3 性能分析
4 结论

图1 喷雾重结晶法装置简图<br/>Fig.1 Diagram of spray recrystallization device

图1 喷雾重结晶法装置简图
Fig.1 Diagram of spray recrystallization device

图2 原料FOX-7的SEM照片<br/>Fig.2 SEM image of raw FOX-7

图2 原料FOX-7的SEM照片
Fig.2 SEM image of raw FOX-7

图3 以H2O为非溶剂,不同溶剂重结晶FOX-7的SEM照片<br/>Fig.3 SEM images of recrystallized FOX-7 in different solvents with H2O as non-solvent

图3 以H2O为非溶剂,不同溶剂重结晶FOX-7的SEM照片
Fig.3 SEM images of recrystallized FOX-7 in different solvents with H2O as non-solvent

图4 以NMP为溶剂,不同非溶剂重结晶FOX-7的SEM照片<br/>Fig.4 SEM images of refined FOX-7 in different non-solvents with NMP as solvent

图4 以NMP为溶剂,不同非溶剂重结晶FOX-7的SEM照片
Fig.4 SEM images of refined FOX-7 in different non-solvents with NMP as solvent

图5 不同药液质量浓度时重结晶的FOX-7的SEM照片及粒径分布图<br/>Fig.5 SEM images and particle size distribution of recrystallized FOX-7 at different mass concentrations

图5 不同药液质量浓度时重结晶的FOX-7的SEM照片及粒径分布图
Fig.5 SEM images and particle size distribution of recrystallized FOX-7 at different mass concentrations

图6 不同搅拌速率重结晶的FOX-7的SEM照片及粒径分布图<br/>Fig.6 SEM images and particle size distribution of recrystallized FOX-7 at different stirring rates

图6 不同搅拌速率重结晶的FOX-7的SEM照片及粒径分布图
Fig.6 SEM images and particle size distribution of recrystallized FOX-7 at different stirring rates

图7 原料FOX-7及微米级FOX-7的XRD图谱<br/>Fig.7 XRD patterns of raw FOX-7 and micron FOX-7

图7 原料FOX-7及微米级FOX-7的XRD图谱
Fig.7 XRD patterns of raw FOX-7 and micron FOX-7

图8 原料FOX-7及微米级FOX-7的FT-IR图谱<br/>Fig.8 FT-IR patterns of raw FOX-7 and micron FOX-7

图8 原料FOX-7及微米级FOX-7的FT-IR图谱
Fig.8 FT-IR patterns of raw FOX-7 and micron FOX-7

图9 原料FOX-7和微米级FOX-7的DSC曲线<br/>Fig.9 DSC curves of raw FOX-7 and micron FOX-7

图9 原料FOX-7和微米级FOX-7的DSC曲线
Fig.9 DSC curves of raw FOX-7 and micron FOX-7

表1 原料FOX-7和微米级FOX-7的表观活化能<br/>Table 1 Apparent activation energies of raw FOX-7 and micron FOX-7

表1 原料FOX-7和微米级FOX-7的表观活化能
Table 1 Apparent activation energies of raw FOX-7 and micron FOX-7

表2 原料FOX-7和微米级FOX-7的热动力学参数<br/>Table 2 Thermodynamic parameters of raw FOX-7 and micron FOX-7

表2 原料FOX-7和微米级FOX-7的热动力学参数
Table 2 Thermodynamic parameters of raw FOX-7 and micron FOX-7

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备注

引言

1 实验

2 结果与讨论

3 性能分析

4 结论

期刊信息

备注

引言

1 实 验

2 结果与讨论

3 性能分析

4 结 论

期刊信息

1 实验

4 结论