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Ferrocene high-nitrogen energetic eutectic

A high-nitrogen-containing, eutectic technology, applied in the preparation of metallocenes, aromatic nitration compositions, organic compounds, etc., can solve the problems of easy migration and volatility.

Inactive Publication Date: 2015-07-22
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the problem of easy migration and volatilization of ferrocene derivatives in the prior art, to provide a simple synthesis method, not easy to volatilize under natural conditions, good thermal stability, high Heat of Formation and Heat of Combustion of Ferrocene High Nitrogen Energetic Eutectic Compounds

Method used

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  • Ferrocene high-nitrogen energetic eutectic

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Taking the preparation of N,N-dimethylaminomethyl ferrocene and tetrazole co-crystal as an example, the reaction equation and preparation method are as follows:

[0019]

[0020] Add 0.070g (1mmol) of tetrazole into a round-bottomed flask containing 15mL of acetone, and stir until the solution is completely transparent; dissolve 0.243g (1mmol) of N,N-dimethylaminomethylferrocene in 15mL of acetone, Then it was slowly added dropwise to a round-bottomed flask with a constant pressure funnel, an orange precipitate was formed immediately, filtered with suction, the filter cake was washed 3 times with acetone, and then placed in a vacuum drying oven at 70°C for 24 hours to obtain N, N-dimethylaminomethyl ferrocene and tetrazolium eutectic powder, its structural characterization data are as follows:

[0021] FT-IR (KBr, cm -1 ): 3300, 2649, 1473, 1025; 1 H NMR (600MHz, DMSO) δ: 8.55(s, 1H), 4.31(s, 2H), 4.23(s, 2H), 4.19(s, 5H), 3.77(s, 2H), 2.42(s, 6H) ; 13 C NMR (600...

Embodiment 2

[0024] Taking the preparation of N,N-dimethylaminomethyl ferrocene and picric acid cocrystal as an example, the reaction equation and preparation method are as follows:

[0025]

[0026] Add 0.229g (1mmol) of picric acid into a round-bottomed flask containing 15mL of methanol, and stir until the solution is completely transparent; dissolve 0.243g (1mmol) of N,N-dimethylaminomethylferrocene in 15mL of methanol, and then Slowly drop it into a round-bottomed flask with a constant pressure funnel, a red precipitate formed immediately, filter it with suction, wash the filter cake with methanol three times, and then dry it in a vacuum oven at 70°C for 24 hours to obtain N,N- Dimethylaminomethyl ferrocene and picric acid eutectic powder, its structural characterization data are as follows:

[0027] FR-IR (KBr, cm －1 ): 3021, 1551, 1326; 1 H NMR (600MHz, DMSO) δ: 8.59(s, 2H), 4.41(s, 2H), 4.32(s, 2H), 4.23(s, 5H), 4.10(d, J=4.2Hz, 2H), 2.65 (s, 6H); 13C NMR (600 MHz, DMSO) δ: 1...

Embodiment 3

[0030] Taking the preparation of N,N-dimethylaminomethylferrocene and trinitrotoluene cocrystal as an example, the reaction equation and preparation method are as follows:

[0031]

[0032] Add 0.227g (1mmol) trinitrotoluene into a round bottom flask filled with 15mL chloroform, and stir until the solution is completely transparent; dissolve 0.243g (1mmol) N,N-dimethylaminomethylferrocene in 15mL chloroform , and then slowly drop it into a round bottom flask with a constant pressure funnel. After the dropwise addition, spin dry with a rotary evaporator, and then place it in a vacuum drying oven at 70°C for 24 hours to obtain N,N-dimethyl Aminomethylferrocene and trinitrotoluene eutectic powder, its structural characterization data are as follows:

[0033] FR-IR (KBr, cm －1 ): 3676, 3195, 1148, 1541, 1471, 815; 1 H NMR (400MHz, DMSO) δ: 9.03(s, 2H), 4.23(t, 9H), 3.82(s, 2H), 3.52(s, 3H), 2.56(s, 6H); 13 C NMR (600 MHz, DMSO) δ: 161.29, 142.35, 125.66, 124.67, 75.31, 71.44...

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Abstract

The invention discloses a ferrocene high-nitrogen energetic eutectic. The ferrocene high-nitrogen energetic eutectic is an eutectic formed by using N,N-dimethylaminomethylferrocene and an energetic compound, wherein the energetic compound is tetrazole, picric acid, trinitrotoluene or 5-aminotetrazole. The ferrocene high-nitrogen energetic eutectic is synthesized through eutectic formation of the energetic compound and a ferrocene burning rate catalyst N,N-dimethylaminomethylferrocene through using an eutectic technology, so a synthetic method of the eutectic has the advantages of simplicity and low cost; and the synthesized ferrocene high-nitrogen energetic eutectic has the advantages of non-volatility and good heat stability under natural conditions, high formation heat and combustion heat, great reduction of the migration and the volatility of the catalyst, and improvement of the energy level of a propellant during decomposition due to energy containing of the eutectic.

Description

technical field [0001] The invention belongs to the technical field of synthesis of burning rate catalysts in solid propellant formulations, and in particular relates to a ferrocene high-nitrogen energy-containing eutectic compound and a preparation method thereof. Background technique [0002] Burning rate catalysts, also known as combustion modifiers, are one of the essential components in solid propellant formulations. Among the many burning rate catalysts, ferrocene burning rate catalysts are widely used in composite solid propellants due to their excellent combustion regulation function, in various ballistic missiles, airborne tactical missiles, anti-missile high-speed kinetic energy missiles and Sea-based mines, torpedoes and other weapons play an important role. However, ferrocene-based burning rate catalysts have the defects of volatilization and sublimation in the production of solid propellants, and there are problems of easy migration during storage. [0003] In...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02C07D257/06C07D257/04C07C201/16C07C205/24C07C205/06C06B23/00
CPCC06B25/04C06B25/34C07B2200/13C07C205/06C07C205/24C07D257/04C07D257/06C07F17/02
Inventor 张国防许瑞丽冉露李吉祯李婷高晓妮
Owner SHAANXI NORMAL UNIV
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