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Ferrocenetetrazolium high-nitrogen energetic ion compound and preparation method thereof

A technology of ferrocene tetrazolium and ionic compounds, which is applied in the field of ferrocene tetrazolium high-nitrogen energetic ionic compounds and its preparation, can solve the problem of low iron content in catalysts, poor catalytic effect, and inability to obtain mechanical Performance, process performance and combustion performance, etc., to achieve good thermal stability, low synthesis cost, and non-volatile effects

Inactive Publication Date: 2017-10-20
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this catalyst contains low iron content and introduces non-energy silicon oxide, so the catalytic effect is not very good.
In addition, people have introduced reactive functional groups such as oxirane, mercapto, and aza groups into ferrocene compounds, and through testing these compounds in solid propellants, they have found that they can partially solve the problem of migration, but none of them can A perfect combination of mechanical properties, process properties and combustion properties

Method used

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  • Ferrocenetetrazolium high-nitrogen energetic ion compound and preparation method thereof
  • Ferrocenetetrazolium high-nitrogen energetic ion compound and preparation method thereof
  • Ferrocenetetrazolium high-nitrogen energetic ion compound and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Ferrocene Tetrazole High Nitrogen Energetic Ionic Compounds with the Following Structural Formula

[0032]

[0033] Dissolve 0.443g (1.6mmol) of compound A completely in a 50mL round-bottomed flask filled with 20mL of distilled water. After the solution is completely transparent, add 0.195g (1.6mmol) of guanidine nitrate solution dissolved in 20mL of distilled water dropwise, and immediately a yellow Precipitation is formed, stirred and reacted at room temperature for 5 hours, filtered with suction, washed with distilled water for 3 times, recrystallized with methanol / ether, and then dried in a vacuum oven at 70°C for 24 hours to obtain ferrocene tetrazole as a yellow solid Nitrogen-containing energetic ionic compound 0.42g, its melting point is 200°C, and the yield is 83%.

[0034] The spectral data of the resulting product is: 1 H NMR (400MHz, DMSO) δ (ppm): 7.12 (s, 6H), 4.69 (t, J = 1.8Hz, 2H), 4.21 (d, J = 3.5Hz, 2H), 3.96 (s, 5H); 13 C NMR (400...

Embodiment 2

[0040] Preparation of Ferrocene Tetrazole High Nitrogen Energetic Ionic Compounds with the Following Structural Formula

[0041]

[0042]0.302g (0.4mmol) of compound A was completely dissolved in a 50mL round bottom flask filled with 20mL of distilled water. After the solution was completely transparent, 0.100g (0.4mmol) of aminoguanidine sulfate dissolved in 20mL of distilled water was added dropwise. Precipitate formed, stirred at room temperature for 5 hours, filtered with suction, washed the filter cake with distilled water for 3 times, recrystallized with acetone / ether, and then dried in a vacuum oven at 70°C for 24 hours to obtain ferrocene tetrazole as a yellow solid 0.21 g of a nitrogen-containing energetic ionic compound, the melting point of which is 190° C., and the yield is 70%.

[0043] The spectral data of the resulting product is: 1 H NMR (400MHz, DMSO) δ (ppm): 8.87 (s, 1H), 7.22 (d, J = 129.6Hz, 4H), 4.71 (dd, J = 4.4, 2.6Hz, 4H), 4.23 (t, J =1.8Hz, 2H), ...

Embodiment 3

[0048] Preparation of Ferrocene Tetrazole High Nitrogen Energetic Ionic Compounds with the Following Structural Formula

[0049]

[0050] Completely dissolve 0.400g (1.45mmol) of compound A in a 50mL round-bottomed flask containing 20mL of distilled water. After the solution is completely transparent, add 0.182g (1.45mmol) of 1,3-diaminoguanidine dissolved in 20mL of distilled water dropwise Hydrochloride solution, a precipitate formed immediately, stirred and reacted at room temperature for 8 hours, suction filtered, the filter cake was washed with distilled water 3 times, recrystallized with methanol / ether, and then dried in a vacuum oven at 70°C for 24 hours to obtain a yellow solid 0.43 g of ferrocene tetrazolium high-nitrogen energetic ionic compound, the melting point is 171° C., and the yield is 86%.

[0051] The spectral data of the resulting product is: 1 H NMR (400MHz, DMSO) δ(ppm): 8.78(s, 2H), 7.28(s, 2H), 4.74(d, J=1.6Hz, 2H), 4.62(s, 3H), 4.29-4.23(m , 2H), ...

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Abstract

The invention discloses ferrocene tetrazole high nitrogen energy containing ionic compound. A structural formula is as follows and the formula represents guanidine positive ion and aminoguanidine positive ion or melbine positive ion. A preparation method is simple in operation and low in composition cost and overcomes the defects that the composition technology of ferrocene and ramification thereof is complex in technology, expensive in price and high in cost and the composed ferrocene tetrazole high nitrogen energy containing ionic compound is not easy to volatilize under natural conditions, good in thermal stability, is high in generation heat and combustion heat, can be applied to solid propellant, provides energy for the solid propellant, is controllable in catalytic performance and can satisfy recipe requirements of solid propellants in different types.

Description

technical field [0001] The invention belongs to the technical field of solid propellants, and in particular relates to a class of ferrocene tetrazolium high-nitrogen energetic ion compounds and a preparation method thereof. Background technique [0002] Ferrocene and its derivatives, because of their excellent combustion regulation function, have been widely used in strategic and tactical weapon systems as the most important burning rate catalysts of solid propellants (especially composite propellants). Ballistic missiles (including theater, short-range, medium-range, intercontinental ballistic missiles, etc.), airborne tactical missiles, anti-missile high-speed kinetic energy missiles and sea-based mines, torpedoes and other weapons play a huge role. [0003] Due to the problems of easy migration, volatilization, and low-temperature crystallization of the currently used ferrocene-based burning rate catalysts, it has seriously affected the storage life, reliability, and envi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02B01J31/22
CPCB01J31/2295B01J2531/842C07F17/02
Inventor 张国防高晓妮赵凤起樊学忠安亭李吉祯邵二莎
Owner SHAANXI NORMAL UNIV
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