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Synthetic method of hexanitrostilbene

A technology for the synthesis of hexanitrostilbene, which is applied in the fields of chemical instruments and methods, single substance as explosives, preparation of organic compounds, etc., and can solve problems such as difficult treatment and measurement

Inactive Publication Date: 2017-07-14
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the above literature reports, the process of making hexanitrostilbene by the dehydrogenation of hexanitrobibenzyl all obtains a yield of more than 94%, but the dehydrogenation agent liquid bromine is easy to volatilize and difficult to measure, and the strong irritating smoke produced is harmful to the human body. Injuries that are difficult to treat and have high quality requirements for the liquid bromine used, often require imported reagents to meet

Method used

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  • Synthetic method of hexanitrostilbene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under stirring, add 1g of hexanitrobibenzyl into 10ml of benzene / pyridine mixed solvent with a volume ratio of 1:1. After the addition, heat up to 40°C. After the solid matter is completely dissolved, add 1g of tribromopyridinium and continue to heat up Heat the reaction at 80°C for 4 hours, then cool the system down to 25°C, filter, wash with water, wash with ethanol, and dry to obtain 0.915g of solid with a yield of 91.9%.

[0021] Melting point: 315~324℃

[0022] Infrared spectrum (KBr, cm -1 )γ: 3100, 1617, 1601, 1539, 1348, 724

[0023] 1 H NMR (DMSO-d6, 500MHz, ppm): 9.123, 7.139

[0024] The above identification data confirm that the substance obtained in this step is hexanitrostilbene.

Embodiment 2

[0026] Under stirring, add 1g of hexanitrobibenzyl into 6ml of 1,2-dichloroethane / pyridine mixed solvent with a volume ratio of 10:1. After the addition, the temperature is raised to 40°C. After all the solid substances are dissolved, add 2g Tetrabutylammonium tribromide, continue to heat up to 70°C, keep warm for 6h, then cool the system down to 25°C, filter, wash with water, wash with ethanol, and dry to obtain 0.93g of solid with a yield of 93.4%.

Embodiment 3

[0028] Under stirring, add 1g of hexanitrobibenzyl into 10ml of 1,2-dichloroethane / pyridine mixed solvent with a volume ratio of 12:1. g tribromopyridinium, continue to heat up to 80°C, keep the temperature for 3h, then cool the system down to 25°C, filter, wash with water, wash with ethanol, and dry to obtain 0.900g of solid with a yield of 90.4%.

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Abstract

The invention discloses a method for synthesizing hexanitrostilbene (HNS), which aims to solve the problems of high quality requirement of liquid bromine, difficulty in weighing and generation of irritating gas in the process of synthesizing hexanitrostilbene from hexanitrobibenzyl. The invention uses hexanitrobibenzyl as raw material, uses mixed solvent as solvent, and prepares hexanitrostilbene under the action of solid dehydrogenation agent. The present invention is mainly used for synthesizing hexanitrostilbene.

Description

technical field [0001] The invention relates to a method for synthesizing hexanitrostilbene, which belongs to the field of energetic materials. Background technique [0002] Hexanitrostilbene is a new type of high-energy, low-sensitivity, heat-resistant single-substance explosive with excellent performance. It has a melting point of 318°C and has the characteristics of good high-low temperature detonation performance. The ultra-high temperature perforating bomb charge explored is currently the only heat-resistant explosive that can meet the industrial production value and fuze safety design specifications. [0003] At present, the industrial preparation of hexanitrostilbene mainly adopts a two-step method, using TNT as a raw material, oxidizing it with sodium hypochlorite to obtain hexanitrobibenzyl, and then preparing hexanitrostilbene under the action of a dehydrogenation reagent. The literature "Research on the Oxidation of Hexanitrobibenzyl to Hexanitrostilbene" (Journa...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/06C06B49/00
CPCC07C201/12C06B49/00
Inventor 张蒙蒙王友兵李媛周杰文胡琳琳黄凤臣汪强席伟
Owner XIAN MODERN CHEM RES INST
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