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Double-core ferrocene high-nitrogen energetic ion compound and preparation method thereof

An ionic compound, high nitrogen-containing energy technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, chemical/physical processes, etc., can solve complex problems, reduce synthesis process, and improve catalytic activity. Obvious problems such as low synthesis cost, good thermal stability and simple operation are achieved

Inactive Publication Date: 2015-05-20
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the mechanical properties of a series of new binuclear ferrocene derivatives synthesized by the above-mentioned many scientific researches have been improved, there are still problems that the catalytic activity is not significantly improved or even decreased under the same amount of addition, and the synthesis process is complicated.

Method used

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  • Double-core ferrocene high-nitrogen energetic ion compound and preparation method thereof
  • Double-core ferrocene high-nitrogen energetic ion compound and preparation method thereof
  • Double-core ferrocene high-nitrogen energetic ion compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Taking the binuclear ferrocene high-nitrogen energetic ionic compound with the following structural formula as an example, the preparation method is as follows:

[0028]

[0029] Dissolve 0.50g (0.65mmol) of compound A completely in a 50mL round-bottomed flask filled with 10mL of methanol. After the solution is completely transparent, add 0.35g (2.07mmol) of AgNO dissolved in 15mL of distilled water dropwise. 3 solution, a yellow precipitate was formed immediately, and N 2 , stirred at room temperature for 1 hour, filtered with suction, washed the filter cake 3 times with distilled water, rinsed with methanol 3 times, and then dried in a vacuum oven at 70°C for 24 hours to obtain a yellow solid binuclear ferrocene with high nitrogen content The ionic compound (denoted as a1) was 0.38g, its melting point was 183.5°C, and the yield was 90%.

[0030] The spectral data of gained product is: IR (cm -1 ): 3033 (double bond C-H stretch on ferrocene), 2919 (methyl C-H stre...

Embodiment 2

[0035] Taking the binuclear ferrocene high-nitrogen energetic ionic compound with the following structural formula as an example, the preparation method is as follows:

[0036]

[0037] Completely dissolve 0.50g (0.61mmol) of compound A in a 50mL round-bottomed flask filled with 10mL of methanol. After the solution is completely transparent, add 0.31g (1.83mmol) of AgNO dissolved in 15mL of distilled water dropwise. 3 solution, other steps were the same as in Example 1, and 0.40 g of a yellow solid binuclear ferrocene high-nitrogen energetic ion compound (referred to as a2) was obtained, with a melting point of 178.5° C. and a yield of 95%.

[0038] The spectral data of the product is: IR (cm -1 ): 3038 (double bond C-H stretch on ferrocene), 3001 (methyl C-H stretch), 835 (methyl C-H bend), 1501 (ferrocene C=C), 1389 (NO 2 Extension), 1105, 1285 (C-N extension); 1 H NMR (DMSO-d6, δ): 1.29 (s, CH 2 , 4H), 1.71(s, CH 2, 4H), 2.86(s, 12H), 3.09(m, 4H), 4.26(s, 10H), 4.39(...

Embodiment 3

[0042] Taking the binuclear ferrocene high-nitrogen energetic ionic compound with the following structural formula as an example, the preparation method is as follows:

[0043]

[0044] Dissolve 0.50g (0.57mmol) of compound A completely in a 50mL round-bottomed flask filled with 10mL of methanol. After the solution is completely transparent, add 0.29g (1.71mmol) of AgNO dissolved in 10mL of distilled water dropwise. 3 solution, other steps were the same as in Example 1, and 0.39 g of a yellow solid binuclear ferrocene high-nitrogen energetic ion compound (referred to as a3) was obtained, with a melting point of 171.5° C. and a yield of 91.3%.

[0045] The spectral data of the product is: IR (cm -1 ): 3040 (double bond C-H stretch on ferrocene), 3005 (methyl C-H stretch), 846 (methyl C-H bend), 1505 (ferrocene C=C), 1395 (NO 2 Extension), 1108, 1288 (C-N extension); 1 H NMR (DMSO-d6, δ): 1.26 (s, CH 2 , 12H), 1.68(s, CH 2 , 4H), 2.74(s, 12H), 3.01(m, 4H), 4.23(s, 10H), 4...

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Abstract

The invention discloses a double-core ferrocene high-nitrogen energetic ion compound with a structural formula as shown in the specification, wherein n is an integer from 2 to 10; in the structural formula, x<theta> is NO3<->, n<3->, nitrophenol negative ion, multi-cyan-group negative ion or bitetrazole negative ion. The double-core ferrocene high-nitrogen energetic ion compound synthesized by the preparation method disclosed by the invention is unlikely to volatilize under the natural condition and good in thermal stability; a nitrogen-rich radial is induced, so that formation heat and combustion heat are higher and can be used in a solid propellant, so that energy is contributed for the solid propellant. Moreover, the compound is adjustable in catalytic performances and capable of satisfying formula needs of different solid propellants. Besides, the preparation method of the double-core ferrocene high-nitrogen energetic ion compound is simple to operate, low in synthesis cost and capable of overcoming the defects that the ferrocene and the derivative therefore are complex in synthesis process, high in price, high in cost and the like.

Description

technical field [0001] The invention belongs to the technical field of solid propellants, and in particular relates to a class of binuclear ferrocene high-nitrogen energetic ion compounds and a preparation method thereof. Background technique [0002] Due to the advantages of high iron content, excellent burning rate catalytic effect, high boiling point, good thermal stability, non-volatile, and difficult migration in solid propellants, dual-nuclear ferrocene catalysts have gradually replaced mononuclear ferrocene catalysts. burn rate catalyst. However, although the dual-nuclear ferrocene-based burning rate catalyst has excellent comprehensive performance, it is easy to oxidize, contains no energy, crystallizes at low temperature, and has a complicated synthesis process, which seriously affects the storage life and reliability of various missile propellant charges in our country. It also greatly increases the expenditure on national defense scientific research. Therefore, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02B01J31/22C06D5/00
Inventor 张国防赵冬梅成志英李平樊学忠赵凤起刘学林毕福强
Owner SHAANXI NORMAL UNIV