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A nitrogen-rich condensed ring compound, its derivatives, and its preparation method

A compound, fused ring technology, applied in the direction of nitrated acyclic/alicyclic/heterocyclic amine explosive compositions, organic chemistry, etc. energy boosting effect

Active Publication Date: 2021-11-05
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Also in the preparation of energetic compounds, high performance and low sensitivity remain concerns

Method used

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  • A nitrogen-rich condensed ring compound, its derivatives, and its preparation method
  • A nitrogen-rich condensed ring compound, its derivatives, and its preparation method
  • A nitrogen-rich condensed ring compound, its derivatives, and its preparation method

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preparation example Construction

[0039] A kind of preparation method of nitrogen-rich condensed ring compound of the present invention comprises the following steps:

[0040] Step 1: Add 0.25 to 5.08 grams of 1-(2H-tetrazol-5-yl)guanidine to 60ml of 0.5 to 2M hydrochloric acid in an ice-water bath at -5 to 5°C, and stir for 5 to 60 minutes to obtain a suspension , and then add BrCN in the amount of 1-(2H-tetrazol-5-yl) to the suspension, stir for 5 to 60 minutes, remove the ice-water bath, let it slowly return to room temperature, and continue to close the ring at this temperature React for 6-48 hours, hydrochloric acid is a catalyst and provides an acidic environment. After the reaction, cool the reaction liquid at 0-5°C, and then adjust the pH to 4-7 with 0.1-2M NaOH. At this time, a large amount of white precipitates are precipitated. Filter the obtained solid powder, rinse with deionized water, and dry. A white powder was obtained, which was denoted as compound 1, namely tetrazolo[1,5-a][1,3,5]-triazine-...

Embodiment 1

[0048] The specific synthetic steps of compound 1, compound 2, compound 3 and compound 4 are shown in figure 1 as shown,

[0049] Step 1: In an ice-water bath, add 2.54 grams (20 mmol) of 1-(2H-tetrazol-5-yl) guanidine to 60 ml of 1M HCl solution and stir for 20 minutes to obtain a suspension, then add 2.12 grams of ( 20 mmol) of BrCN was stirred for 10 minutes, the ice-water bath was removed, and it was slowly returned to room temperature, and the temperature was maintained to continue the reaction for 24 hours. After the reaction, the reaction solution was cooled in a refrigerator at 5°C for 12 hours, and the pH was adjusted to 7 with 1M NaOH. A large amount of white precipitates were precipitated. The obtained solid powder was filtered, rinsed with deionized water, and dried in air to obtain a white powder. Compound 1, tetrazolo[1,5-a][1,3,5]-triazine-5,7-diamine, yield 63.2%.

[0050] The obtained compound 1 was recrystallized with ethanol, filtered, and the filtrate was...

Embodiment 2

[0061] Step 1: In an ice-water bath, add 0.25 g of 1-(2H-tetrazol-5-yl)guanidine to 60 ml of 0.5M HCl solution and stir for 5 minutes to obtain a suspension, then add 1-(2H -Tetrazol-5-yl) BrCN with the same molar number of guanidine was stirred for 5 minutes, then the ice-water bath was removed, and it was slowly returned to room temperature, and the temperature was maintained to continue the reaction for 6 hours. After the reaction, the reaction solution was cooled in the refrigerator at 0°C for 12 hours, and the pH was adjusted to 4 with 1M NaOH. A large amount of white precipitates were precipitated. The resulting solid powder was filtered, rinsed with deionized water, and dried in air to obtain a white powder. Compound 1, tetrazolo[1,5-a][1,3,5]-triazine-5,7-diamine.

[0062] Step 2: In the ice-water bath, first add 3ml of concentrated nitric acid to the flask to cool it down. After 15 minutes, add 0.02 g of the compound 1 prepared above, stir and react for 10 minutes, ta...

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Abstract

A kind of nitrogen-rich fused ring compound and its derivatives of the present invention, preparation method thereof, the preparation method of nitrogen-rich condensed ring compound comprises step 1, hydrochloric acid, 1-(2H-tetrazol-5-yl ) Mix the mixed system of guanidine and BrCN uniformly; step 2, react the mixed system at room temperature for 6-48 hours, separate the products in the reaction solution, wash and dry in sequence, and obtain the nitrogen-rich condensed ring compound. Dissolve the nitrogen-rich fused ring compound in fuming nitric acid at -5-5°C for 10-60 minutes, then react at 10-25°C for 30-90 minutes, drop the reaction liquid on ice to precipitate nitrogen-rich fused-ring ammonium nitrate compound. After the compound is dissolved, an organic base and a metal base are added respectively, and the mixed system is reacted at -5-5°C for 5-15 minutes, and finally reacted at room temperature for 5-30 minutes. Organic and inorganic salts of ammonium compounds.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a nitrogen-rich condensed ring compound and its derivatives, and a preparation method. Background technique [0002] In the study of explosives in modern science, explosives are often referred to as energetic materials. Energetic materials are metastable substances with high energy density. After being excited by a specific stimulation method, it will quickly release a large amount of energy to damage the surrounding objects. Based on this principle, energetic materials are designed for various tasks and provide convenience for production and life. Energetic materials are widely used in the fields of national defense, military industry and civil blasting, and their application in mining and other fields has greatly reduced labor costs; with the development of the automobile industry, energetic materials as gas generating agents are widely used in airbags, and the applicati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04C06B25/34
CPCC06B25/34C07D487/04
Inventor 郭兆琦耶金程彦飞王煜杨娜马海霞
Owner NORTHWEST UNIV
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