Insensitive energetic metal organic framework and preparation method thereof

A metal-organic framework, a certain amount of technology, applied in the direction of explosives, etc., can solve the problems of increasing the complexity of ECMOF, and achieve the effects of good safety and energetic performance, good safety, and convenient operation

Active Publication Date: 2019-11-05
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be deduced from this that the design and synthesis of these ligands increases the complexity of ECMOF preparation

Method used

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  • Insensitive energetic metal organic framework and preparation method thereof
  • Insensitive energetic metal organic framework and preparation method thereof
  • Insensitive energetic metal organic framework and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: Synthesis of methyl 5-amino-1H-1,2,4-triazole-3-carboxylate (MATC)

[0029] Weigh 12.8g (10mmol) of 3-amino-1H-1,2,4-triazole-5-carboxylic acid and 90mL of anhydrous methanol in a 250mL three-necked bottle, and slowly add 6mL of 50% fuming h 2 SO 4 . The temperature was maintained at 85°C and refluxed for 12 hours. After the reaction was completed, the mixed solution was cooled to room temperature, and then a part of methanol was removed by rotary evaporation to obtain a precipitate. Add 20mL of ice water to dissolve the precipitate with a concentration of 5mol L -1 The pH of the mixed solution was adjusted to 5-6 with NaOH solution, and a white precipitate was obtained immediately. The white precipitate was filtered and washed 2 to 3 times with absolute ethanol. After drying, methyl 3-amino-1H-1,2,4-triazole-5-carboxylate was obtained (yield 73%).

[0030] Step 2: Synthesis of 3-amino-1H-1,2,4-triazole-5-carbohydrazide (ATCA)

[0031] Add 4.26g (30mmol)...

Embodiment 2

[0035]Step 1: Synthesis of methyl 5-amino-1H-1,2,4-triazole-3-carboxylate (MATC)

[0036] Weigh 12.8g (10mmol) of 3-amino-1H-1,2,4-triazole-5-carboxylic acid and 90mL of anhydrous methanol in a 250mL three-necked flask, and slowly add 6mL of 50% fuming H 2 SO 4 . The temperature was maintained at 85°C and refluxed for 12 hours. After the reaction was completed, the mixed solution was cooled to room temperature, and then a part of methanol was removed by rotary evaporation to obtain a precipitate. Add 20mL of ice water to dissolve the precipitate with a concentration of 5mol L -1 The pH of the mixed solution was adjusted to 5-6 with NaOH solution, and a white precipitate was obtained immediately. The white precipitate was filtered and washed 2 to 3 times with absolute ethanol. After drying, methyl 3-amino-1H-1,2,4-triazole-5-carboxylate was obtained (yield 73%).

[0037] Step 2: Synthesis of 3-amino-1H-1,2,4-triazole-5-carbohydrazide (ATCA)

[0038] Add 4.26g (30mmol) of...

Embodiment 3

[0042] Step 1: Synthesis of methyl 5-amino-1H-1,2,4-triazole-3-carboxylate (MATC)

[0043] Weigh 12.8g (10mmol) of 3-amino-1H-1,2,4-triazole-5-carboxylic acid and 90mL of anhydrous methanol in a 250mL three-necked flask, and slowly add 6mL of 50% fuming H 2 SO 4 . The temperature was maintained at 85°C and refluxed for 12 hours. After the reaction was completed, the mixed solution was cooled to room temperature, and then a part of methanol was removed by rotary evaporation to obtain a precipitate. Add 20mL of ice water to dissolve the precipitate with a concentration of 5mol L -1 The pH of the mixed solution was adjusted to 5-6 with NaOH solution, and a white precipitate was obtained immediately. The white precipitate was filtered and washed 2 to 3 times with absolute ethanol. After drying, methyl 3-amino-1H-1,2,4-triazole-5-carboxylate was obtained (yield 73%).

[0044] Step 2: Synthesis of 3-amino-1H-1,2,4-triazole-5-carbohydrazide (ATCA)

[0045] Add 4.26g (30mmol) o...

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Abstract

The invention discloses a silver-based cationic energetic metal organic framework with the chemical formula of [Ag(ATCA)ClO4]n and a preparation method thereof. The preparation method comprises the following steps that step one, a commercial organic intermediate 3-amino-1H-1,2,4-triazole-5-carboxylic acid is taken as a starting raw material, and in absolute methanol, concentrated H2SO4 is taken asa catalyst for synthesis of 5-amino-1H-1,2,4-triazole-3-carboxylic acid methyl ester (MATC); step two, the MATC is utilized for reacting with hydrazine hydrate to prepare a target non-energetic nitrogen-rich ligand 3-amino-1H-1,2,4-triazole-5-carbohydrazide (ATCA); step three, a certain amount of ATCA is suspended in hot water and dissolved through heating, then a silver perchlorate solution withthe certain concentration is added, a certain amount of perchloric acid is dropwise added, then slow cooling evaporative crystallization is conducted, and the target product silver-based cationic energetic metal organic framework with the chemical formula of [Ag(ATCA)ClO4]n is obtained.

Description

technical field [0001] The invention relates to the technical field of novel energetic materials, and more specifically relates to a silver-based cationic energetic metal-organic framework and a preparation method thereof. Background technique [0002] As one of the most widely used materials in military and civilian fields, energetic materials have had a huge impact on human society. Since the invention of black powder in ancient China, oxidation-reduction reactions have been the basic principles for designing new high-energy materials to meet higher requirements. With the in-depth understanding of this concept, people found that implanting oxidized groups such as nitro, nitro, and nitramine in the reducing agent skeleton can not only adjust the nitrogen and oxygen content and oxygen balance, which is directly related to the detonation ability of explosives . This approach makes the oxidized and reduced components more uniform at the molecular level, releasing greater ene...

Claims

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Application Information

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IPC IPC(8): C08G83/00C06B43/00
CPCC06B43/00C08G83/008
Inventor 张祺王霆威
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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