CHINESE JOURNAL OF ENERGETIC MATERIALS
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喷雾结晶法制备高堆积密度球形硝基胍
作者:
作者单位:

(中北大学化工与环境学院, 山西 太原 030051)

作者简介:

王晶禹(1967-),男,教授,主要从事兵器科学与技术研究 。e-mail: wjywjy67@163.com 通信联系人: 李小东(1978-),男,副教授,主要从事火工药剂技术研究。e-mail: lixd78@126.com

通讯作者:

李小东(1978-),男,副教授,主要从事火工药剂技术研究。e-mail: lixd78@126.com

基金项目:

武器装备预先研究项目(51305120201)


Preparation of High Bulk Density Spherical NQ by Spray Crystallization Method
Author:
Affiliation:

(School of Chemical and Environment Engineering, North University of China, Taiyuan 030051, China)

Fund Project:

Weapons and equipment pre research project

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    摘要:

    为了提高硝基胍 (NQ) 的堆积密度和流散性, 以N-甲基吡咯烷酮作为NQ的溶剂, 无水乙醇作为非溶剂, 六水硝酸镍作为晶型控制剂, 采用喷雾结晶法制备了球形硝基胍晶体。单因素法确定制备高堆积密度球形NQ的最优工艺条件为:室温, 溶剂与非溶剂体积比为1:10, 晶型控制剂质量分数为0.5%, 喷雾压力为0.6 MPa, 超声频率为40 Hz, 搅拌速度为450 r·min-1, 喷雾完毕继续超声震荡搅拌20 min。用标准容器法、扫描电子显微镜 (SEM)、差热扫描量热法 (DSC) 和X-射线衍射仪 (XRD) 对最优球形NQ进行分析。结果表明:制备的NQ呈球形, 堆积密度为1.232 g·cm-3, 较原料NQ提高0.943 g·cm-3, DSC测得分解温度为258.71 ℃, 较原料NQ提高8.03 ℃。

    Abstract:

    To improve the bulk density and fluidity of nitroguanidine (NQ), spherical NQ crystal was prepared by spray crystallization method using N-methyl pyrrolidone as the solvent of NQ, anhydrous ethanol as a nonsolvent, nickel nitrate as crystal control agent. The optimal processing conditions of preparing high bulk density spherical NQ determined by single factor method were room temperature, volume ratio of solvent and nonsolvent of 1:10; mass fraction of the crystal control agent, spray pressure, bounce frequency and stirring speed were 0.5%, 0.6 MPa, 40 Hz and 450 r·min-1, respectively; when spray finished, ultrasonic vibration should be continued for another 20 min. The optimal spherical NQ was analyzed by standard container method, scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The results show that the prepared NQ is spherical and the bulk density is 1.232 g·cm-3, which is improved by 0.943 g·cm-3 compared with raw material NQ, decomposition temperature determined by DSC is 258.71 ℃, which is improved by 8.03 ℃ compared with that of raw material NQ.

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引用本文

王晶禹,边红莉,李小东,等.喷雾结晶法制备高堆积密度球形硝基胍[J].含能材料, 2017, 25(1):53-58. DOI:10.11943/j. issn.1006-9941.2017.01.009.
WANG Jing-yu, BIAN Hong-li, LI Xiao-dong, et al. Preparation of High Bulk Density Spherical NQ by Spray Crystallization Method[J]. Chinese Journal of Energetic Materials, 2017, 25(1):53-58. DOI:10.11943/j. issn.1006-9941.2017.01.009.

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历史
  • 收稿日期: 2016-05-10
  • 最后修改日期: 2016-07-18
  • 录用日期: 2016-08-19
  • 在线发布日期: 2017-01-19
  • 出版日期: 2017-01-20