Energy containing ionic salts of 4, 4'-bi [3, 3'-(1-H-5-tetrazolium)] furazan and preparation method thereof

A technology of ionic salt and tetrazole, applied in 4 fields, can solve the problems such as the decrease of oxygen balance, and achieve the effects of easy industrialization, environmental friendliness, and simple synthesis method

Inactive Publication Date: 2014-01-01
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, replacing the oxyfurazan ring with the furazan ring leads to a decrease in the oxygen balance

Method used

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  • Energy containing ionic salts of 4, 4'-bi [3, 3'-(1-H-5-tetrazolium)] furazan and preparation method thereof
  • Energy containing ionic salts of 4, 4'-bi [3, 3'-(1-H-5-tetrazolium)] furazan and preparation method thereof
  • Energy containing ionic salts of 4, 4'-bi [3, 3'-(1-H-5-tetrazolium)] furazan and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Preparation of 4,4'-bis[3,3'-(1-hydrogen-5-tetrazole)]furazan barium salt (2)

[0018] Its structural formula is as follows:

[0019]

[0020] Dissolve 2.000g (6.9mmol) 2 in 20mL hot water, add 2.174gBa(OH) to it 2 ·8H 2 O (6.9 mmol), the reaction mixture was stirred at 100° C. for 2 h, then the insoluble matter was filtered, and the filtrate was concentrated. The resulting solid was recrystallized with water as white crystals, yield: 76%.

[0021] Melting point: 165°C, decomposition temperature: 242°C (DSC). 13 C NMR: δ = 161.0, 148.0, 141.4ppm. IR (neat): = 3200, 3164, 1664, 1538, 1440, 1400, 1358, 1220, 1164, 1080, 1033, 1002, 926, 890, 670, 589, 514, 448, 400cm -1

Embodiment 2

[0022] Example 2 4,4'-bis[3,3'-(1-hydrogen-5-tetrazole)]furazan bis-ammonium salt 2H 2 Preparation of O(3)

[0023] Add 1 mmol ammonium sulfate aqueous solution (5 mL) to 427 mg (1.0 mmol) 2 hot water solution (5 mL), stir the mixture at 60 ° C for 1 h, filter BaSO 4 After precipitation, the filtrate was concentrated to obtain the product with a yield of 93%.

[0024] Its structural formula is as follows:

[0025]

[0026] Decomposition temperature: 215°C (DSC). Density is 1.69g cm -3 . 1 H NMR (400MHz, d 6 -DMSO): δ = 6.07 (br, s, 8H, NH 4 ) ppm; 13 C NMR (100MHz, d 6 -DMSO): δ=161.0, 148.1141.5ppm; IR (neat): 3586, 3525, 3155, 3041, 2899, 1692, 1623, 1541, 1425, 1393, 1221, 1204, 1160, 1142, 1001, 916, 883 , 797, 764, 614, 588, 510, 454cm -1 ;Elemental analysis (%) calcd for C 6 h 8 N 14 o 3 2H 2 O(360.25): calcd. C 20.00, H 3.36, N 54.43%; found: C 19.32, H 3.40, N 53.03%.

Embodiment 3

[0027] Example 3 Preparation of 4,4'-bis[3,3'-(1-hydrogen-5-tetrazole)]furazan dihydrazine salt (4)

[0028] The conditions were the same as in Example 2, except that ammonium sulfate was changed to hydrazine sulfate, and the yield was 90%.

[0029] Its structural formula is as follows:

[0030]

[0031] Melting point: 160°C, decomposition temperature: 242°C (DSC). Density is 1.74g cm -3 . 1 HNMR (400MHz, d 6 -DMSO): δ = 6.96 (br.s, 6H, NH 3 ), 3.74 (br.s, 4H, NH 2 ) ppm; 13 C NMR (100MHz, d 6 -DMSO): δ=161.0, 148.0141.4ppm.IR (neat):=3504, 3431, 3342, 3206, 3167, 1663, 1539, 1439, 1400, 1358, 1220, 1165, 1081, 1033, 1003, 926, 890, 665, 589, 514, 449cm -1 .Elemental analysis for C 6 HN 16 o 3 (354.25): calcd.C 20.34, H 2.85, N 63.26%; found: C 20.44, H 2.88, N 64.15%.

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Abstract

The invention discloses energy containing ionic salts of 4, 4'-bi [3, 3'-(1-H-5-tetrazolium)] furazan and a preparation method thereof, and belongs to the technical field of energy containing materials. The preparation method is as follows: mixing 4, 4'-bi [3, 3'-(1-H-5-tetrazolium)] furazan barium salt with an equal-molar sulfate of a corresponding cation, filtering precipitates, and evaporating out a filtrate to obtain the target product. The preparation method is simple and easy to industrialize. Nine energy containing ionic salts related in the invention are high in thermostability (Td: 213-289 DEG C), the degree of percussion sensitivity of most compounds is greater than 15J, all the energy containing ionic salts have excellent calculation detonation performance and are potential energy containing materials.

Description

technical field [0001] The invention relates to 4,4'-bis[3,3'-(1-hydrogen-5-tetrazole)]furazan energetic ion salt and a preparation method thereof, belonging to the technical field of energetic materials. Background technique [0002] Explosives with improved high temperature properties are often referred to as "heat resistant" or "heat stabilized" explosives. This kind of explosive is an explosive with high thermal stability, appropriate impact sensitivity and high energy, and is widely used in oil well drilling and aerospace. By analyzing some traditional explosives with good thermal stability, it can be found that introducing heterocycles into explosive molecules is an effective way to improve thermal stability. At the same time, the thermal stability of explosives can be further improved and the sensitivity can be reduced by forming energetic salts. [0003] In recent years, energetic ionic salts have become a hotspot in the field of energetic materials research. Compa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D413/14C07C279/02C07C277/00C07C281/16C07C279/24C07C277/08C07C281/06C06B43/00
CPCC07D413/14C06B43/00
Inventor 周智明梁丽轩卞成明黄海丰王凯宋靳红凌黎明
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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