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Method for synthesizing 1,1-diamino-2,2-dinitroethylene

A technology of dinitroethylene and synthesis methods, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, etc., which can solve the problems of severe heat release in nitration reactions, large environmental pollution, and high processing costs, and achieve processing costs. High, environmental pollution, good heat dissipation effect

Active Publication Date: 2018-01-19
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the process of adding nitric acid, the nitrification reaction exotherms violently and is highly dangerous; at the same time, a large amount of waste water containing nitric acid and sulfuric acid is produced after the hydrolysis reaction, causing greater environmental pollution and higher treatment costs

Method used

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  • Method for synthesizing 1,1-diamino-2,2-dinitroethylene
  • Method for synthesizing 1,1-diamino-2,2-dinitroethylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of 1,1-diamino-2,2-dinitroethylene with nitric-sulfur mixed acid directly prepared

[0019] At 15°C, 50.0g of sulfuric acid with a mass fraction of 98% was added to the reaction flask, and then 100.0g of nitric acid with a mass fraction of 98% was added dropwise. After the dropwise addition, the temperature was lowered to 0°C, and 10.0g of 2 -Methyl-4,6-pyrimidinedione, then heated up to 15°C for 3 hours, cooled to 0°C after the reaction and filtered, collected the nitrating acid filtrate, added the filter cake to 450g of ice water, filtered and dried to obtain 1, 10.2 g of 1-diamino-2,2-dinitroethylene, yield 86.8%.

[0020] Structure Identification:

[0021] IR spectrum (KBr pellet / cm -1 ): υ NH :3422, 3406, 3330, 3298; δ NH :1636; υ C＝C :1608; υ as-NO2 :1517; υ s-NO2 :1226;

[0022] Elemental analysis (C 2 h 4 N 4 o 4 ): Theoretical: C 16.22, H 2.72, N 37.84 Found: C 16.56, H 2.429, N 37.71

[0023] 1 H NMR (DMSO-d 6 , δ, ppm): 8.781;

[0...

Embodiment 2

[0027] Preparation of 1,1-diamino-2,2-dinitroethylene from nitric-sulfur mixed acid prepared from recycled nitrating acid filtrate

[0028] At 20°C, weigh 62.5g of the nitrating acid filtrate that circulates once, add successively 25.0g of oleum with a mass fraction of 50% and 62.5g of nitric acid with a mass fraction of 98%, to prepare 150.0g of nitric acid mixed acid; Cool the sulfur mixed acid to 0°C, add 10.0g of 2-methyl-4,6-pyrimidinedione in batches under stirring, then raise the temperature to 15°C for 3 hours, cool down to 0°C after the reaction and filter, collect the nitrating acid filtrate, filter The cake was added to 450 g of ice water, filtered and dried to obtain 10.2 g of 1,1-diamino-2,2-dinitroethylene with a yield of 86.8%.

[0029] Structure Identification:

[0030] IR spectrum (KBr pellet / cm -1 ): υ NH :3424, 3408, 3331, 3298; δ NH :1638; υC＝C :1608; υ as-NO2 :1518; υ s-NO2 :1225;

[0031] Elemental analysis (C 2 h 4 N 4 o 4 ): Theoretical: C 16...

Embodiment 3

[0036] Preparation of 1,1-diamino-2,2-dinitroethylene from nitric-sulfur mixed acid prepared from nitrating acid filtrate which has been circulated three times

[0037] At 0°C, weigh 62.5 g of the nitrating acid filtrate circulated three times, add successively 25.0 g of oleum with a mass fraction of 50% and 62.5 g of nitric acid with a mass fraction of 98%, to prepare 150.0 g of nitric acid mixed acid; Cool the sulfuric acid to -10°C, add 10.0g of 2-methyl-4,6-pyrimidinedione in batches under stirring, then raise the temperature to 10°C for 3 hours, cool down to 0°C after the reaction and filter, collect the nitrating acid filtrate, The filter cake was added to 450 g of ice water, filtered and dried to obtain 9.8 g of 1,1-diamino-2,2-dinitroethylene with a yield of 83.4%.

[0038] Analytical data confirmed that the compound obtained was 1,1-diamino-2,2-dinitroethene.

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Abstract

The invention discloses a method for synthesizing 1,1-diamino-2,2-dinitroethylene. The method comprises the steps as follows: sulfuric acid is added to a reaction flask firstly, nitric acid is then added dropwise, and mixed nitric-sulfuric acid is prepared; 2-methyl-4,6-pyrimidinedione or 2-methyl-4,6-hydroxypyrimidine is added to the mixed nitric-sulfuric acid in batch, filtering is performed after reaction, a nitrating acid filtrate is collected, a filter cake is added to ice water, filtering and drying are performed, and 1,1-diamino-2,2-dinitroethylene is obtained; fuming sulfuric acid withmass fraction of 50% and nitric acid with mass fraction of 98% are added to the collected nitrating acid filtrate in proportion sequentially, and the prepared mixed nitric-sulfuric acid can be recycled directly. The method is used for synthesizing 1,1-diamino-2,2-dinitroethylene.

Description

technical field [0001] The invention relates to a synthesis method of 1,1-diamino-2,2-dinitroethylene, which belongs to organic synthesis. Background technique [0002] 1,1-diamino-2,2-dinitroethylene (FOX-7) is a high-energy insensitive elemental explosive with a crystal density of 1.885g / cm 3 , friction sensitivity is 10% (3.92MPa 90° pendulum angle), explosion percentage is 6% (10kg drop hammer 25cm drop height), characteristic drop height H 50 It is 89.1cm (5kg drop weight), the detonation velocity is 8870m / s, and the detonation pressure is 33.96GPa. Its energy density is equivalent to RDX, its sensitivity is similar to TNT, and its thermal stability is good. Sweden reported a PBX explosive formulation containing 1,1-diamino-2,2-dinitroethylene, which is insensitive to friction and impact. Slow heating (3.3°C / h) does not react violently. When ignited at 220°C, it only burns without detonation, has no flame propagation, and has no damage to the projectile and the enviro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/24
Inventor 周诚李祥志常佩王伯周周群陈涛李亚南
Owner XIAN MODERN CHEM RES INST
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