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Binuclear ferrocene hexacyanoferrate and preparation method thereof

A technology of ferrocene hexacyano, potassium hexacyanoferrate, applied in the field of binuclear ferrocene hexacyanoferrate and preparation thereof, can solve problems such as non-volatile, achieve non-volatile, strong migration resistance, The effect of increasing iron content

Active Publication Date: 2019-06-28
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the shortcomings of the existing ferrocene-based burning rate catalysts as composite solid propellant additives, and to provide a non-volatile, strong migration resistance, and adjustable catalytic performance under natural conditions. Binuclear ferrocene hexacyanoferrate, and a preparation method with simple operation and low cost is provided for the binuclear ferrocene hexacyanoferrate

Method used

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  • Binuclear ferrocene hexacyanoferrate and preparation method thereof
  • Binuclear ferrocene hexacyanoferrate and preparation method thereof
  • Binuclear ferrocene hexacyanoferrate and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Preparation of hexacyanoferrate of 1,3-propylene bis[(1-ferrocenylmethyl)dimethylammonium with the following structural formula, the specific preparation method is:

[0030]

[0031] Dissolve 0.076g (0.8mmol) potassium hexacyanoferrate completely in a 50mL round bottom flask containing 20mL of distilled water. After the solution is completely transparent, add the transparent solution dropwise to 5mL to dissolve 0.478g (1mmol) of 1 , In the methanol solution of 3-propylene bis[(1-ferrocenylmethyl)dimethylammonium iodide, a dark blue precipitate was formed immediately, stirred and reacted at room temperature for 4 hours, filtered, and the filter cake was washed with distilled water for 3 and then dried in a vacuum oven at 45°C for 48 hours to obtain hexacyanoferrate of dark blue solid powder 1,3-propylenebis[(1-ferrocenylmethyl)dimethylammonium 0.566 g, the yield is 85%.

[0032] The spectral data of the product is: IR (cm -1 ): 3012 (C=C-H), 2998 (-CH 3 ), 2864 (-C...

Embodiment 2

[0037] Preparation of hexacyanoferrate of 1,4-butylene bis[(1-ferrocenylmethyl)dimethylammonium with the following structural formula, the specific preparation method is:

[0038]

[0039] Dissolve 0.076g (0.8mmol) potassium hexacyanoferrate completely in a 50mL round bottom flask containing 20mL of distilled water. After the solution is completely transparent, add the transparent solution dropwise to 5mL to dissolve 0.492g (1mmol) of 1 , In the methanol solution of 4-butylenebis[(1-ferrocenylmethyl)dimethylammonium iodide, a black precipitate was formed immediately, stirred and reacted at room temperature for 4 hours, filtered, and the filter cake was washed 3 times with distilled water, Then place it in a vacuum oven and dry it at 45° C. for 48 hours to obtain 0.592 g of hexacyanoferrate of black solid powder 1,4-butylene bis[(1-ferrocenylmethyl) dimethyl ammonium, which The yield was 87%.

[0040] The spectral data of the product is: IR (cm -1 ): 3063 (C=C-H), 2919 (-C...

Embodiment 3

[0045] Preparation of hexacyanoferrate of 1,5-pentylidene bis[(1-ferrocenylmethyl)dimethylammonium with the following structural formula, the specific preparation method is:

[0046]

[0047] Dissolve 0.076g (0.8mmol) potassium hexacyanoferrate completely in a 50mL round bottom flask containing 20mL of distilled water. After the solution is completely transparent, add the transparent solution dropwise to 5mL to dissolve 0.506g (1mmol) of 1 , In the methanol solution of 5-pentylidene bis[(1-ferrocenylmethyl) dimethyl ammonium iodide, a yellow-green precipitate is generated immediately, and other steps are the same as in Example 1 to obtain a yellow-green solid powder 1 , 0.597 g of hexacyanoferrate of 5-pentylidene bis[(1-ferrocenylmethyl)dimethylammonium, the yield was 86%.

[0048] The spectral data of the product is: IR (cm -1 ): 3057 (C=C-H), 2966 (-CH 3 ), 2881 (-CH 2 ), 2112 (C≡N), 1632 (C=C). Elemental analysis (theoretical calculation values ​​in brackets): C% 59...

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Abstract

The invention discloses bisferrocene hexacyanoferrate and a preparation method thereof. The structural formula of the compound is as shown in the specification. In the formula, X<(+)> indicates bisferrocene methyl quaternary ammonium cation or bisferrocene methyl alkyl imidazolium cation. The method is simple to operate, has low synthesis cost and overcomes the defect that a ferrocene and its derivative synthesis process is complex, price is high and cost is high. The synthesized bisferrocene hexacyanoferrate is not easy to volatile under natural conditions and has strong migration resistance. In addition, catalytic performance of the compound can be regulated such that the compound can meet formula requirements of different solid propellants. As iron content is increased, catalytic performance of the compounds is expected to be raised.

Description

technical field [0001] The invention belongs to the technical field of solid propellants, and in particular relates to a class of binuclear ferrocene hexacyanoferrate and a preparation method thereof. Background technique [0002] Ferrocene and its derivatives have been widely used in strategic and tactical weapon systems as the most important burning rate catalysts of solid propellants (especially composite propellants) due to their excellent combustion regulation functions. 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 and volatilization of the currently used ferrocene-based burning rate catalysts, it has seriously affected the storage life, reliability and environmental adaptability of various missile propellant charges in my countr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02B01J31/22
CPCB01J31/2295B01J2531/0205B01J2531/0225B01J2531/842C07F17/02
Inventor 张国防贾铎张娜邵二莎李婷刘漫漫许镭
Owner SHAANXI NORMAL UNIV
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