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Energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea and its preparation method and application

A technology of dinitrophenyl and urea, applied in the field of compound preparation, can solve the problems of inconvenient transportation, low yield and the like, and achieve the effects of simple equipment, high yield and safe raw materials

Active Publication Date: 2021-10-01
XINYANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of HNFX is low, and the sensitivity and other aspects cause inconvenience in transportation. Therefore, both at home and abroad are vigorously looking for high-energy insensitive energetic materials that can replace HNFX.

Method used

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  • Energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea and its preparation method and application
  • Energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea and its preparation method and application
  • Energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of raw material 1:

[0027] Under stirring in an ice-water bath, add 3,4,5-trifluoroaniline (0.1mol) and N,N-dimethylformamide (150mL) into a 250mL round-bottomed flask in sequence to dissolve the 3,4,5- Trifluoroaniline, then potassium carbonate (16.56g) was added, and ethyl chloroformate (0.12mol) was slowly added dropwise. After the initial exotherm was completed, the ice-water bath was removed, and the temperature was slowly raised to room temperature to react for 24 h, then the reacted mixture was poured into ice water, filtered, washed with water, and dried to obtain a gray solid (19.56 g, yield 89.31%).

Embodiment 2

[0029] A preparation of energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea (ZXC-19), comprising the following steps:

[0030] Accurately weigh 5.56 grams of potassium nitrate (55mmol, 2.2eq), and slowly add it to 50 ml of concentrated sulfuric acid (the concentration of sulfuric acid is 95-98%) under ice-water bath magnetic stirring conditions, and keep the reaction for 10 minutes under ice-water bath conditions , slowly added raw material 1 (5.479g, 25mmol, 1.0eq), after the addition, the system was slowly raised to room temperature and continued to stir until the reaction was complete (TLC detection).

[0031] After the reaction was complete, the reaction mixture was slowly poured into vigorously stirred ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain a light yellow solid with a yield of 89%; the H NMR spectrum of the product was 1 H NMR (600MHz, CDCl 3 -d 1 )δppm: 10.0(s,2H); 13 C NMR (151MHz, C...

Embodiment 3

[0033] A preparation of energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea (ZXC-19), comprising the following steps:

[0034]Accurately take by weighing 5.56 grams of potassium nitrate (55mmol, 2.47eq), under ice-water bath magnetic stirring condition, slowly join in 50 milliliters of vitriol oil, (concentration of sulfuric acid is 95~98%), keep reaction 10 under ice-water bath condition Minutes, raw material 1 (4.89g, 22.3mmol, 1.0eq) was slowly added, after the addition, the system was slowly raised to room temperature and continued to stir until the reaction was complete (TLC detection).

[0035] After the reaction was complete, the reaction mixture was slowly poured into vigorously stirred ice water, a large amount of precipitates were precipitated, filtered, washed with water, and dried to obtain a light yellow solid with a yield of 86.4%.

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Abstract

The structural formula of 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl) urea of ​​the present invention comprises the following steps for its preparation method: 3,4,5-trifluoroaniline is substituted The reaction obtains the intermediate product (3,4,5-trifluorophenyl) ethyl carbamate, and then through nitration reaction to obtain 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl ) urea. ZXC‑19 has poor solubility in water and is soluble in most organic solvents. It has a very high density at 298K, has good thermal stability, high solid-state heat of formation and good detonation performance, low sensitivity, and no combustion products. Small molecular weight, suitable for use as rocket propellant. 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl) urea has a very simple synthesis method, high yield, easy industrial production, environmental friendliness, and easy recrystallization. An important raw material for ZXC‑8.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to energetic material 1,3-bis(3,4,5-trifluoro-2,6-dinitrophenyl)urea and its preparation method and application. Background technique [0002] Simple explosives have been difficult to meet the needs of national defense and civil blasting, so the search for high-energy insensitive explosives has always been a research hotspot. The element fluorine is in the upper right corner of the periodic table, has the strongest electronegativity and oxidizing properties, and is very active. It can react with most inorganic or organic substances at or below room temperature and release more heat. The heat of formation of fluorine-containing explosives is more negative than that of similar conventional explosives of the CHNO class. The study found that after introducing fluorine atoms into CHNO-containing high-energy compounds, due to its strong oxidation and high density...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C275/30C07C273/18C06B25/04
CPCC06B25/04C07C273/1836C07C275/30
Inventor 张行程张梦娇姚磊胡文祥
Owner XINYANG NORMAL UNIVERSITY
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