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New method for synthesizing hexanitrobibenzyl

A technology of hexanitrobibenzyl and a new method, which is applied in the field of energetic material preparation, can solve the problems of multiple reaction steps, complex reaction conditions and processes, and achieve the effects of stable reaction, shortened reaction time, and increased product yield

Inactive Publication Date: 2012-04-04
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has many reaction steps, complex reaction conditions and process
The yields of the first two steps are respectively 90% (crude product), 77%, and the third step yield is lower than 35%
[0011] So far, there is no domestic research report on the synthesis of hexanitrobibenzyl with bibenzyl as raw material

Method used

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  • New method for synthesizing hexanitrobibenzyl
  • New method for synthesizing hexanitrobibenzyl

Examples

Experimental program
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Effect test

Embodiment 1

[0041] At 20°C, bibenzyl was added to 98% fuming nitric acid, and the mass ratio of bibenzyl to 98% fuming nitric acid was 1:13; the reaction was stirred for 4 hours, and then the reaction solution was poured into ice water to precipitate pale Yellow solid, filtered under a vacuum of 0.08MPa, washed with water until neutral, soaked in 20 times the amount of boiling ethanol, and then crystallized twice in an equal volume mixture of benzene and toluene, dried at 80°C for 4 hours under normal pressure to obtain 14.1 g pure product of tetranitrobibenzyl, melting point: 171-172°C, yield 70.9%.

[0042] The tetranitrobibenzyl that 10g last step obtains is joined in the nitrating agent, and the mass ratio of tetranitrobibenzyl and the nitrating agent is 1: 20, and the oleum of 20% and the fuming nitric acid volume of 98% in the nitrating agent The ratio is 1:3, the oil bath is heated to 100°C, stirred, and refluxed for 6 hours. Then, the reaction solution is poured into ice water, an...

Embodiment 2

[0044] At 25°C, add bibenzyl to 98% fuming nitric acid, the mass ratio of bibenzyl to 98% fuming nitric acid is 1:10; stir and react for 5 hours, then pour the reaction solution into ice water to precipitate Pale yellow solid, filtered under a vacuum of 0.08MPa, washed with water until neutral, soaked in 20 times the amount of boiling ethanol, then crystallized twice in an equal volume mixture of benzene and toluene, dried at 80°C for 4 hours under normal pressure to obtain Tetranitrobibenzyl.

[0045]10g of tetranitrobibenzyl obtained in the last step is added to the nitrating agent, the mass ratio of tetranitrobibenzyl and nitrating agent is 1: 24, 20% fuming sulfuric acid and 98% fuming nitric acid in the nitrating agent The volume ratio was 1:2.5, the oil bath was heated to 110°C, stirred, and refluxed for 7 hours. Then, the reaction solution was poured into ice water, and a pale yellow solid was precipitated. Filtered under a vacuum of 0.08MPa, washed with water until neu...

Embodiment 3

[0047] At 25°C, add bibenzyl to 98% fuming nitric acid, the mass ratio of bibenzyl to 98% fuming nitric acid is 1:15; stir and react for 6 hours, then pour the reaction solution into ice water to precipitate Pale yellow solid, filtered under a vacuum of 0.08MPa, washed with water until neutral, soaked in 20 times the amount of boiling ethanol, then crystallized twice in an equal volume mixture of benzene and toluene, dried at 80°C for 4 hours under normal pressure to obtain Tetranitrobibenzyl.

[0048] The tetranitrobibenzyl that 10g last step obtains is joined in the nitrating agent, and the mass ratio of tetranitrobibenzyl and the nitrating agent is 1: 30, and the oleum of 20% and the fuming nitric acid volume of 98% in the nitrating agent The ratio is 1:2, the oil bath is heated to 120°C, stirred, and refluxed for 8 hours. Then, the reaction solution is poured into ice water, and a light yellow solid is precipitated, filtered under a vacuum of 0.08MPa, washed with water unt...

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Abstract

The invention discloses a new method for synthesizing hexanitrobibenzyl, and relates to the technical field of preparation of energetic materials. The method comprises the following steps of: nitrating, separating out, filtering, washing, crystallizing and drying bibenzyl at the temperature of 18-35 DEG C to obtain tetranitrobibenzyl; further nitrating the tetranitrobibenzyl at the temperature of 80-120 DEG C; and separating out, then filtering, washing, crystallizing and drying to finally obtain a hexanitrobibenzyl pure product. In the method, by changing a nitrating agent and nitration reaction temperature, synthetic reaction from the bibenzyl to the tetranitrobibenzyl is finished at normal temperature, so that the yield of crude product is increased by over 5 percent; the synthetic reaction from the tetranitrobibenzyl to the hexanitrobibenzyl is finished in one step, so that the operation process is simplified, the reaction time is shortened by about 24 hours, the yield of the hexanitrobibenzyl pure product is increased by over 13 percent, the cost is reduced by about 20 percent, and the method is safe in operation and stable in reaction.

Description

technical field [0001] The invention relates to the technical field of energetic material preparation, specifically a new method for synthesizing hexanitrobibenzyl (HNBB). Background technique [0002] Hexanitrobibenzyl (HNBB), or dipicrylethane, has a melting point of 212°C. As an important raw material for the synthesis of heat-resistant explosive hexanitrostilbene (HNS), it has attracted the attention of researchers at home and abroad. [0003] Hexanitrostilbene (HNS) is a high-melting-point explosive with good performance. It has good thermal stability and can detonate normally within the temperature range of -193°C to 225°C. It can also be used as an explosive for aerospace, deep well oil Main explosives for mining etc. There are four main types of synthesis methods: [0004] One is to prepare hexanitrostilbene (HNS) by reacting 2,4,6-trinitrotoluene (TNT) with alkali metal or alkaline earth metal hypochlorite. There have been research synthesis reports in this area ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/06C07C201/08
Inventor 陈丽珍郑志花王建龙郭建峰尉志华
Owner ZHONGBEI UNIV
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