High-energy potassium salt, and preparation and use method thereof

A potassium salt and organic technology, applied in the field of novel energy-containing flame suppressant-high-energy organic potassium salt and its preparation, can solve problems such as inability to be widely used, achieve easy industrial production, suppress secondary combustion, and reduce infrared radiation intensity Effect

Inactive Publication Date: 2010-07-14
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of these flame suppressants are water-soluble inorganic inert potassium salts, which cannot be widely used in the solvent-free screw press process.

Method used

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  • High-energy potassium salt, and preparation and use method thereof
  • High-energy potassium salt, and preparation and use method thereof
  • High-energy potassium salt, and preparation and use method thereof

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Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0021] Specifically, the preparation method of energy-containing organic potassium salt of the present invention is:

[0022] (1) First suspend DNMDZ in distilled water, slowly add KOH under stirring condition;

[0023] (2) add methanol after reacting for a certain period of time, and properly heat for a certain period of time;

[0024] (3) Cool the reaction solution, a large number of light yellow crystals precipitate out, filter, wash and vacuum dry to obtain the product.

[0025] The amount of reactant is:

[0026] DNMDZ to KOH molar ratio: 1:1.5-1:2.5;

[0027] The mass ratio of distilled water: DNMDZ is 4:16:1;

[0028] The reaction conditions are:

[0029] Reaction time: 10-30min;

[0030] Methanol: distilled water consumption ratio is 2: 1-4: 1, when methanol consumption is less than 2 times of distilled water consumption, yield is very low and impure or cannot obtain product;

[0031] Temperature: 40-60°C, not exceeding 60°C;

[0032] Cooling, washing and drying...

Embodiment 1

[0038] Embodiment 1: the synthesis of ligand

[0039] Dissolve 2.96g of 1,1-diamino-2,2-dinitroethylene (FOX-7) into 12mL of N-methylpyrrolidone, add 2.96g of ethylenediamine under stirring conditions, and heat to 110°C After stirring and reacting for 48 hours, cool to room temperature, add an appropriate amount of distilled water, a large number of light yellow fine crystals precipitate immediately, filter, wash with distilled water and vacuum dry to obtain the ligand-DNMDZ product. Yield 67% (2.33 g).

Embodiment 2

[0040] Embodiment 2: the synthesis of K (DNMDZ)

[0041] At room temperature, 0.01mol (1.74g) DNMDZ was dispersed in 10mL of distilled water, and 0.02mol (1.12g) KOH was slowly added under stirring conditions. After 30min of reaction, 30mL of methanol was added, heated to 50°C, and put into the freezer of the refrigerator after 10min. That is, a large amount of pale yellow crystals precipitated, filtered, washed with methanol and dried in vacuo to obtain the target product K(DNMDZ), with a yield of 71% (1.24g)

[0042] figure 1 Coordination environment diagram of potassium ions in the synthesized high-energy organopotassium salt; figure 2 It is the infrared spectrum of high-energy organic potassium salt; image 3 It is the DSC spectrum of the high-energy organic potassium salt. The DSC results show that the complex has high thermal stability and begins to decompose at about 200 ° C. The peak temperature is 227 ° C. The heat release is 2095 J / g, and the energy is relatively...

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Abstract

The invention discloses a high-energy organic sylvine and a preparation method thereof. In particular, the preparation processes are as follows: firstly, 2-(1, 1-binitromethylene)-1, 3-diazo heterocyclic pentane are suspended in distilled water and added with KOH while being stirred; after reaction for a certain time, methanol is added and properly heating is carried out; the reaction solution iscooled later, a large amount of light yellow crystal is precipitated, then filtering, washing and drying in vacuum is carried out to obtain a target product K(DNMDZ); the yield is over 65 percent. The compound of the invention has good flame-eliminating capacity, very high thermal decomposition energy and thermal stability and can play double-effectiveness very well in a low characteristic signalpropellant.

Description

technical field [0001] The invention belongs to the technical field of energetic materials, and in particular relates to a novel energetic flame suppressant-high-energy organic potassium salt and its preparation method and application. Background technique [0002] The "secondary combustion" of solid rocket motor exhaust is one of the key technologies to be solved in the development of low signature propellants. "Secondary combustion" refers to the phenomenon that after the engine gas is discharged through the nozzle, its combustible components in the ambient atmosphere are mixed with oxygen in the air and re-combusted, and the plume emits bright visible light radiation and infrared radiation energy at the same time. Secondary combustion has many hazards. It has an important impact on the survivability of missile weapon launch platforms, the precision guidance capability of guidance systems, and the penetration capability of strategic missiles. Therefore, research on suppres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/20C06D5/00
Inventor 徐抗震赵凤起宋纪蓉黄洁王晗
Owner NORTHWEST UNIV
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