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A heat-resistant compound 2-fluro-1,3,5-triamino-4,6-dinitrobenzene and a preparing method thereof

A technology for dinitrobenzene and dinitroaniline, which is applied in the field of compound preparation, can solve the problems of insufficient stability of explosives, easy evaporation and the like, and achieves the effects of superior performance, easy recrystallization and simple equipment

Inactive Publication Date: 2018-12-14
XINYANG NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the influence of aerodynamic effects and the vacuum environment of space and the moon during the flight of the spacecraft, the spacecraft needs to be heated to sterilize before entering the space and returning to the earth, but conventional explosives (such as Hesogen) It is not stable enough under high temperature or low pressure for a long time, and even easy to evaporate under aerodynamic effect, which cannot meet the above requirements

Method used

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  • A heat-resistant compound 2-fluro-1,3,5-triamino-4,6-dinitrobenzene and a preparing method thereof
  • A heat-resistant compound 2-fluro-1,3,5-triamino-4,6-dinitrobenzene and a preparing method thereof
  • A heat-resistant compound 2-fluro-1,3,5-triamino-4,6-dinitrobenzene and a preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation of a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene comprises the following steps:

[0030] Step 1: Preparation of 3,4,5-trifluoro-2,6-dinitroaniline:

[0031] Under magnetic stirring, add 125mmol potassium nitrate and 10.95 grams of N-ethylcarbonate-3,4,5-trifluoroaniline (50mmol) successively in 100 milliliters of concentrated sulfuric acid (98% by mass) in an ice-water bath, and react After completion, the reaction system was slowly poured into ice water, continued to stir for 1 hour until the system returned to room temperature, filtered, washed, and dried to obtain 11.02 g of a light yellow solid with a yield of 93%. The light yellow solid was 3 ,4,5-Trifluoro-2,6-dinitroaniline.

[0032] Step 2: Preparation of 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene:

[0033] Accurately weigh 5.0 grams of 3,4,5-trifluoro-2,6-dinitroaniline, put it into a 100 ml eggplant-shaped bottle, add 50 ml of concentrated ammonia water with a mass perc...

Embodiment 2

[0035] The preparation of a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene comprises the following steps:

[0036] Step 1: Preparation of 3,4,5-trifluoro-2,6-dinitroaniline:

[0037]Under magnetic stirring, add 10.95 g of N-ethylcarbonate-3,4,5-trifluoroaniline (50 mmol) in 100 ml of concentrated sulfuric acid (98% by mass) in an ice-water bath, then slowly add 15 Milliliter fuming nitric acid (mass percentage is 95%), after the reaction is complete, the reaction system is slowly poured into ice water, continue to stir for 1 hour until the system returns to room temperature, filter, wash, and dry to obtain 10.95 grams of light yellow solid. The yield was 92.4%, and the light yellow solid was 3,4,5-trifluoro-2,6-dinitroaniline.

[0038] Step 2: Preparation of 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene:

[0039] Accurately weigh 5.0 grams of 3,4,5-trifluoro-2,6-dinitroaniline, put it into a 100 ml eggplant-shaped bottle, add 50 ml of concentrated ammonia wa...

Embodiment 3

[0041] The preparation of a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene comprises the following steps:

[0042] Step 1: Preparation of 3,4,5-trifluoro-2,6-dinitroaniline:

[0043] Under magnetic stirring, add 125mmol sodium nitrate and 10.95 grams of N-ethylcarbonate-3,4,5-trifluoroaniline (50mmol) successively in 100 milliliters of concentrated sulfuric acid (98% by mass) in an ice-water bath, and react After completion, the reaction system was slowly poured into ice water, continued to stir for 1 hour until the system returned to room temperature, filtered, washed, and dried to obtain 11.02 g of a light yellow solid with a yield of 93%. The light yellow solid was 3 ,4,5-Trifluoro-2,6-dinitroaniline.

[0044] Step 2: Preparation of 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene:

[0045] Accurately weigh 5.0 grams of 3,4,5-trifluoro-2,6-dinitroaniline, put it into a 100 ml eggplant-shaped bottle, add 10 ml of 40% by mass concentrated ammonia water under m...

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Abstract

The structure formula of 2-fluro-1,3,5-triamino-4,6-dinitrobenzene of the invention is shown in the description. A preparing method of the compound includes 1) subjecting N-(3,4,5-trifluoro phenyl)carbamate to nitration to obtain 3,4,5-trifluro-2,6-dinitroaniline; and 2) mixing aqueous ammonia or an alcohol solution of ammonia with the 3,4,5-trifluro-2,6-dinitroaniline, stirring the mixture, performing filtration after the reaction is finished, and washing and drying a product to obtain the target compound. Compared with TATB, the 2-fluro-1,3,5-triamino-4,6-dinitrobenzene has better detonationperformance, and is a heat resistant explosive having sensitivity similar to sensitivity of the TATB. The synthetic method is simple, high in yield and prone to industrial production. The disclosed compound is insoluble in water, environmentally friendly and easy to recrystallize so that the potential industrialization value is higher.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a heat-resistant compound 2-fluoro-1,3,5-triamino-4,6-dinitrobenzene and a preparation method thereof. Background technique [0002] Precise strike, high-efficiency damage capability and high survivability are the goals pursued by modern weapons. To achieve these goals, high-energy-density materials (HEDM) as weapon energy carriers must meet high energy, high density, low vulnerability, and environmental adaptability. and high thermal stability requirements. In recent years, with the development of the aerospace industry and the exploitation of underground resources such as oil and gas, there is an increasingly urgent need for a class of explosives that can withstand high pressure (or low pressure) and high temperature, referred to as heat-resistant explosives. Heat-resistant explosives refer to a class of explosives that can maintain appropriate mechani...

Claims

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Application Information

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IPC IPC(8): C07C209/10C07C211/52C06B25/04
CPCC06B25/04C07C209/00C07C209/10C07C211/52
Inventor 张行程胡文祥姚磊
Owner XINYANG NORMAL UNIVERSITY
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