Ferrocene tetrazolium ion compound with high iron content and preparation method thereof

A technology of ferrocene tetrazolium and ionic compounds, which is applied in the field of high iron content ferrocene tetrazolium ionic compounds and their preparation, can solve the problem of low iron content of catalysts, inability to obtain mechanical properties, process performance and combustion performance, Catalytic effect is not very good and other problems, to achieve the effect of improved catalytic performance, less volatilization, and low synthesis cost

Inactive Publication Date: 2017-07-11
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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  • Ferrocene tetrazolium ion compound with high iron content and preparation method thereof
  • Ferrocene tetrazolium ion compound with high iron content and preparation method thereof
  • Ferrocene tetrazolium ion compound with high iron content and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Taking the high-iron-content ferrocene tetrazolium ion compound with the following structural formula as an example, the preparation method is as follows:

[0035]

[0036] Completely dissolve 0.286g (1.03mmol) of compound A in a 50mL round-bottomed flask filled with 20mL of distilled water. After the solution is completely transparent, add 0.331g (0.86mmol) of dioxane dissolved in a mixture of 30mL of distilled water and 1mL of methanol dropwise. Iron methyl quaternary ammonium salt solution, a yellow precipitate formed immediately, stirred at room temperature for 4 hours, filtered with suction, washed the filter cake with distilled water 3 times, recrystallized with dichloromethane / ether, and then dried in a vacuum oven at 70°C After 24 hours, 0.30 g of a yellow solid ferrocene tetrazolium ion compound with high iron content was obtained, with a yield of 70%.

[0037] The spectral data of the obtained product are 1 H NMR (600MHz, DMSO) δ (ppm): 4.67 (t, J = 1.6Hz,...

Embodiment 2

[0042] Taking the high-iron-content ferrocene tetrazolium ion compound with the following structural formula as an example, the preparation method is as follows:

[0043]

[0044] Completely dissolve 0.286g (1.03mmol) of compound A in a 50mL round-bottomed flask filled with 20mL of distilled water. After the solution is completely transparent, add 0.351g (0.86mmol) of dioxane dissolved in a mixture of 30mL of distilled water and 1mL of methanol dropwise. Iron methyl quaternary ammonium salt solution, a yellow precipitate formed immediately, stirred at room temperature for 3 hours, filtered with suction, washed the filter cake with distilled water 3 times, recrystallized with dichloromethane / ether, and then dried in a vacuum oven at 70°C After 24 hours, 0.35 g of a yellow solid ferrocene tetrazolium ion compound with high iron content was obtained, with a yield of 70%.

[0045] The spectral data of the resulting product is: 1 H NMR (600MHz, CDCl 3 )δ (ppm): 5.06-4.94 (m, 2...

Embodiment 3

[0050] Taking the high-iron-content ferrocene tetrazolium ion compound with the following structural formula as an example, the preparation method is as follows:

[0051]

[0052] Dissolve 0.286g (1.03mmol) of compound A completely in a 50mL round-bottomed flask filled with 20mL of distilled water. After the solution is completely transparent, add 0.363g (0.86mmol) of ferrocenemethyl quaternary ammonium dissolved in 30mL of distilled water dropwise. Salt solution, a yellow precipitate formed immediately, stirred at room temperature for 3 hours, suction filtered, the filter cake was washed 3 times with distilled water, recrystallized with dichloromethane / ether, and then dried in a vacuum oven at 70°C for 24 hours to obtain yellow The ferrocene tetrazolium ion compound with high iron content in solid was 0.36g, and the yield was 70%.

[0053] The spectral data of the resulting product is: 1 H NMR (600MHz, CDCl 3 )δ(ppm): 5.03(t, J=1.8Hz, 2H), 4.48(s, 2H), 4.36(s, 2H), 4.29(...

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Abstract

The invention discloses a ferrocene tetrazolium ion compound with high iron content, its structural formula is where a is 1 or 2, Represents a mononuclear ferrocenemethyl quaternary ammonium cation with one unit of positive charge or a dinuclear ferrocenemethyl quaternary ammonium cation with two units of positive charge. The method of the invention is simple in operation and low in synthesis cost, overcomes the disadvantages of complex synthetic process of ferrocene and its derivatives, high price, high cost, etc., and the synthesized ferrocene tetrazolium ion compound with high iron content is not easy to volatilize under natural conditions, Good thermal stability, due to the introduction of nitrogen-rich groups, it has high heat of formation and combustion, used in solid propellants, can contribute energy to solid propellants, and the catalytic performance of the compound can be adjusted to meet The formulation requirements of different types of solid propellants, and increased iron content, the catalytic performance is expected to improve.

Description

technical field [0001] The invention belongs to the technical field of solid propellants, in particular to a class of ferrocene tetrazolium ion compounds with high iron content 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 environmental ada...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02B01J31/22
Inventor 张国防高晓妮赵凤起安亭李吉祯赵凯
Owner SHAANXI NORMAL UNIV
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