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High nitrogen dinuclear ferrocene triazole ionic metal complex and preparation method thereof

A technology for nuclear ferrocenetriazole and metal complexes, applied in the field of binuclear ferrocenetriazole ionic metal complexes and their preparation, achieving high yield, excellent catalytic performance, and good thermal stability

Active Publication Date: 2020-08-25
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the shortcomings of the existing solid propellants of ferrocene derivatives, to provide a propellant that is not volatile under natural conditions, has good thermal stability, and has relatively high heat of formation and combustion. A high-nitrogen dinuclear ferrocene triazole ionic metal complex with excellent catalytic performance and controllability, and a preparation method for the complex

Method used

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  • High nitrogen dinuclear ferrocene triazole ionic metal complex and preparation method thereof
  • High nitrogen dinuclear ferrocene triazole ionic metal complex and preparation method thereof
  • High nitrogen dinuclear ferrocene triazole ionic metal complex and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 202mg (0.5mmol) Fe(NO 3 ) 3 9H 2O was completely dissolved in a 50mL round bottom flask filled with 5mL of distilled water. At 70°C, 10mL of methanol solution containing 270g (1.5mmol) of potassium 1,1,3,3-tetracyanoacrylate and 5mL of 316mg (0.5mmol) N,N of 4-amino-3,5-bis(4-ferrocenyl-1,2,3-triazole-1-methyl)-1,2,4-triazole -Dimethylformamide solution, react at constant temperature for 3 hours after the dropwise addition, filter with suction, wash the filter cake twice with N,N-dimethylformamide, then fully wash with distilled water and methanol in turn, and then dry in vacuum Dry at 70° C. for 24 hours in an oven to obtain a high-nitrogen dinuclear ferrocenetriazolium ionic metal complex (referred to as compound 1) with the following structural formula, with a yield of 77%.

[0021]

[0022] The structural characterization data of the obtained complex is: FT-IR (KBr, cm -1 ):3131s, 2955m, 2206s, 1789s, 1711s, 1638s, 1600m, 1542s, 1509s, 1463m, 1378s, 1333s, 12...

Embodiment 2

[0024] In this example, equimolar Cu(NO 3 ) 2 ·3H 2 O replaces Fe(NO in Example 1 3 ) 3 9H 2 O, 1,1,3,3-tetracyanoacrylate potassium consumption is 180g (1.0mmol), and other steps are identical with embodiment 1, obtain the high nitrogen dinuclear ferrocene triazole ionic metal complex ( Denoted as compound 2), the yield was 71%.

[0025]

[0026] The structural characterization data of the obtained complex is: FT-IR (KBr, cm -1 ):3131s, 3001m, 2199s, 1782s, 1704s, 1633s, 1548s, 1502s, 1437m, 1327s, 1197m, 1105s, 1047s, 871s, 818s, 662m; EA: C 84 Cu 2 h 72 Fe 4 N 36 o 6 Theoretical value C 49.65%, H 3.57%, N 24.81%, measured value C 49.68%, H 3.79%, N 24.92%; UV-Vis: 263nm (ε=3.29×10 5 ), 397nm (ε=1.31×10 5 ), 417nm (ε=1.24×10 5 ).

Embodiment 3

[0028] In this example, the potassium 1,1,3,3-tetracyanoacrylate in Example 1 is replaced with equimolar 1,1,2,3,3-pyridine pentacyanoacrylate, other steps are the same as in Example 1 Similarly, a high-nitrogen dinuclear ferrocenetriazole ionic metal complex (referred to as compound 3) with the following structural formula was obtained with a yield of 71%.

[0029]

[0030] The structural characterization data of the obtained complex is: FT-IR (KBr, cm -1 ):3203s, 2949m, 2199s, 1770s, 1698s, 1624s, 1502s, 1431s, 1378vs, 1333s, 1223s, 1105m, 1053s, 962s, 877s, 818s; EA: C 104 h 84 Cr 2 Fe 4 N 50 o 14 Theoretical value C 48.31%, H 3.27%, N 27.09%, measured value C 48.41%, H 3.27%, N 27.23%; UV-Vis: 264nm (ε=3.13×10 5 ), 395nm (ε=1.05×10 5 ), 416nm (ε=9.44×10 4 ).

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Abstract

The invention discloses a high-nitrogen biferrocene triazole ion type metal complex and a preparation method thereof. The structural formula of the complex is as shown in the description, wherein M represents Cr<3+>, Fe<3+>, Cu<2+> or Zn<2+>, and L represents 1,1,3,3-tetracyanoacrylate ion, 1,1,2,3,3-pentacyanoacrylate ion or 1,1,2,5,6,6-hexacyano-3,4-diazahexadienoate ion. The complex disclosed by the invention is simple in preparation method, is not easy to volatilize under natural conditions, is good in thermal stability, has higher formation heat and combustion heat, and has excellent combustion catalysis performance for thermal decomposition of ammonium perchlorate.

Description

technical field [0001] The invention belongs to the technical field of solid propellants, and in particular relates to a class of dinuclear ferrocenetriazole ionic metal complexes and a preparation method thereof. Background technique [0002] The dual-nuclear ferrocene burning rate catalyst has gradually replaced the mononuclear ferrocene burning rate catalyst due to its advantages of high iron content, excellent burning rate catalytic effect, high boiling point, good thermal stability, low volatility, and low mobility. . 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, scientific researchers...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02C07C255/09C07C253/30C06B23/00
CPCC06B23/007C07C255/09C07F17/02
Inventor 张国防刘漫漫姜丽萍张娜高子伟张伟强
Owner SHAANXI NORMAL UNIV
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