High-pressure preparation method of sodium pentazole

A technology of sodium pentazole and high pressure is applied in the field of high temperature and high pressure preparation of sodium pentazole to achieve the effects of saving synthesis cost and simple method

Pending Publication Date: 2020-11-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the preparation of simple binary pentazole materials is still a challenging work
However, there is no research report on the dissociation and recombination of sodium azide under high pressure.

Method used

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  • High-pressure preparation method of sodium pentazole
  • High-pressure preparation method of sodium pentazole
  • High-pressure preparation method of sodium pentazole

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preparation example Construction

[0021] The invention provides a high-pressure preparation method of sodium pentazole, comprising the following steps:

[0022] Sodium azide is filled in the diamond anvil sample cavity, and then the sodium azide in the sample cavity is pressurized to obtain sodium pentazole; the pressurized pressure is above 21.6 GPa.

[0023] In the present invention, the method for forming the sample cavity is preferably: use a diamond counter-anvil press to pre-press the steel sheet, and drill a hole in the center of the indentation, using the hole as the sample cavity; the diamond counter-anvil press The diameter of the anvil surface is preferably 300 μm, and the diameter of the sample cavity is preferably 50-100 μm.

[0024] After the sample cavity is formed, the present invention fills the sodium azide in the sample cavity. In the present invention, the sodium azide is preferably sodium azide powder; when filling sodium azide, make sodium azide completely fill the sample cavity, without...

Embodiment 1

[0029] A diamond counter-anvil press with an anvil surface of 300 μm was used to pre-press the steel sheet, and a circular hole with a diameter of 100 μm was drilled in the center of the indentation, which was used as a sample cavity for loading raw materials. First add a ruby ​​ball doped with a small amount of chromium as a pressure mark, then fill the excess sodium azide powder into the sample cavity, completely fill the sample cavity, and pressurize without adding any other medium as the pressure transmission medium. When the pressure increased to 21.6GPa, part of the sodium azide dissociated and recombined to obtain sodium pentazole (NaN 5 ) and sodium diazide (NaN 2 ). The Raman scattering spectrum and X-ray diffraction spectrum of gained product see figure 1 and figure 2 .

[0030] according to figure 1 It can be seen that the Raman scattering spectrum of the product at 21.6GPa is located at 180-600cm -1 Range and 1446cm -1 represents NaN 3 Outside the Raman vi...

Embodiment 2

[0033] The filling method of the press, the sample cavity and the sodium azide powder is the same as in Example 1. When the pressure increased to 31.2GPa, part of the sodium azide dissociated and recombined to obtain sodium pentazole (NaN 5 ) and sodium diazide (NaN 2 ). The Raman scattering spectrum and X-ray diffraction spectrum of the product are shown in image 3 and Figure 4 .

[0034] according to image 3 It can be seen that: at 31.2GPa, the Raman scattering spectrum of the product is located at 180-600cm -1 range represents NaN 3 The Raman vibrational peaks broaden, from five vibrational peaks to three peaks and a large broad package, at 845 and 1180cm -1 The slightly enhanced intensity of the wide packet at the position indicates that the NaN 5 The amount has increased, a small amount of NaN 5 Appear.

[0035] according to Figure 4 It can be seen that in the XRD diffraction pattern of the product at 31.2GPa, the positions at 16.6° and 17.5° belong to NaN ...

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Abstract

The invention relates to the technical field of nitrogen-rich material preparation, and provides a high-pressure preparation method of sodium pentazole. The method comprises the following steps: filling a diamond anvil cell sample cavity with sodium azide, and pressurizing sodium azide in the sample cavity to obtain sodium pentazole; wherein the pressure of the pressurization is 21.6 GPa or more.According to the method provided by the invention, sodium pentazole can be obtained through simple one-step pressurizing treatment without heating or adding any pressure transmission medium, other impurities are not introduced in the whole process, the synthesis cost is saved, the environment is not polluted, and the method is simple, safe and reliable.

Description

technical field [0001] The invention relates to the technical field of preparation of nitrogen-rich materials, in particular to a high-temperature and high-pressure preparation method of sodium pentazole. Background technique [0002] Early studies on pentazole chemistry mainly focused on the substituent effect of aryl pentazoles and the stability of compounds, but they failed to prepare pentazole compounds that are stable at room temperature. In 2017, Chinese scientists prepared stable pentazolium ion salt (N 5 ) 6 (H 3 O) 3 (NH 4 ) 4 Cl has attracted extensive attention in the field of nitrogen-rich energetic materials. At present, the research on pentazole materials has made a series of breakthroughs, and two simple binary pentazole ion salts have been successfully prepared. In 2017, Oleynik et al. successfully obtained the pentazole metal salt (CsN 5 ) crystals. In 2018, Loubeyre et al. reported the synthesis of pentazole metal salts (LiN 5 ) crystals, and conf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06C01B21/08
CPCC01B21/0607C01B21/08C01P2002/72C01P2002/82
Inventor 刘冰冰周淼刘波刘然王鹏
Owner JILIN UNIV
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