Spherical NTO crystal and preparation method thereof

A technology of crystal and volume ratio, which is applied in the direction of organic chemical methods, offensive equipment, and a single substance as explosives. It can solve the problems of low charge density, poor molding performance of mixed explosives, and restrictions on the use of NTO.

Active Publication Date: 2022-03-18
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the existing NTO crystals are in the form of zigzag rod-like crystals, and its irregular shape makes the mixed explosives poor in molding performance and low in charge density, which limits their application.
[0003] After continuous research, it was found that the shape of NTO changed from rod-like to cubic after recrystallization, which improved the molding performance and charge density of mixed explosives, but still limited the use of NTO in PBX-like formulations.

Method used

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  • Spherical NTO crystal and preparation method thereof
  • Spherical NTO crystal and preparation method thereof
  • Spherical NTO crystal and preparation method thereof

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preparation example Construction

[0030] The present invention provides a kind of preparation method of NTO crystal, comprises the following steps:

[0031] Dissolving NTO in a mixed solvent of dimethyl sulfoxide and water to obtain a saturated solution; the volume ratio of the dimethyl sulfoxide to water is 0.5-1.75:1, and the temperature of the saturated solution is 64-76°C ;

[0032] The saturated solution is cooled to crystallize, and the NTO crystals are precipitated; the cooling rate of the cooled crystallization is 3.0-4.5°C·min -1 ; The cooling crystallization is accompanied by stirring, and the stirring speed is 300-800r / min.

[0033] In the present invention, NTO is dissolved in a mixed solvent of dimethyl sulfoxide and water to obtain a saturated solution; the volume ratio of the dimethyl sulfoxide to water is 0.5 to 1.75:1, and the temperature of the saturated solution is 64 to 76°C. The present invention has no special limitation on the source of the NTO, and conventional commercially available...

Embodiment 1

[0047] The temperature of the double-layer jacketed reactor was adjusted to 70 ° C by means of external circulation temperature control; using the double-layer reactor as a container, 8 g of NTO was dissolved in 20 mL of a mixed solvent consisting of 12 mL of dimethyl sulfoxide and 8 mL of water. To obtain a saturated solution, keep warm for 30min;

[0048] Control the external circulation device of the reactor to make the reactor follow the temperature of 3.5°C·min -1 The cooling rate is lowered to 5°C; the cooling is accompanied by stirring at a speed of 500r / min; after cooling down to 5°C, continue to stir for 60 minutes;

[0049] The suspension obtained after stirring was subjected to suction filtration, washed with a saturated solution, and the filter residue obtained by suction filtration was freeze-dried at -84° C. for 240 min to obtain NTO crystals. The yield of the prepared NTO crystals was 80%.

[0050] The NTO crystal prepared in Example 1 is subjected to scanning...

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Abstract

According to the NTO crystal provided by the invention, the ratio of the short axis to the long axis of the NTO crystal is 0.9 to 1.5. The NTO crystal provided by the invention has a regular morphology, is particularly spherical, and has higher formability and charge density when being used for mixed explosives, so that the application range of the NTO crystal is further expanded. The preparation method of the NTO crystal provided by the invention comprises the following steps: dissolving NTO in a mixed solvent of dimethyl sulfoxide and water to obtain a saturated solution; the volume ratio of the dimethyl sulfoxide to the water is (0.5-1.75): 1, and the temperature of the saturated solution is 64-76 DEG C; cooling and crystallizing the saturated solution, and separating out the NTO crystal; the cooling rate of the cooling crystallization is 3.0-4.5 DEG C * min <-1 >; the cooling crystallization is accompanied by stirring, and the rotating speed of stirring is 300-800r / min. The spherical NTO crystal is prepared by limiting parameters such as the type of the solvent, the temperature of the saturated solution, the cooling rate and the stirring rate.

Description

technical field [0001] The invention belongs to the technical field of energetic materials, and in particular relates to a spherical NTO crystal and a preparation method thereof. Background technique [0002] 3-nitro-1,2,4-triazol-5-one (3-nitro-1,2,4-triazol-5-one, NTO), is a new type of high density, high energy, low sensitivity, Easy-to-form elemental explosives. Its density is as high as 1.93g / cm 3 , the theoretical detonation energy is close to RDX, the sensitivity is close to TATB, the safety performance is better than B explosive, the energy is close to B explosive, and the price is low. It is a high-energy and low-sensitivity single-substance explosive with great application prospects. However, most of the existing NTO crystals are zigzag-like rod-like crystals, and their irregular shapes lead to poor molding performance and low charge density of mixed explosives, which are limited in application. [0003] After continuous exploration, it was found that the shape ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/14C06B25/00C06B49/00
CPCC07D249/14C06B49/00C06B25/00C07B2200/13
Inventor 李小东刘慧敏刘文杰孙彦涛王晶禹牛昶尧
Owner ZHONGBEI UNIV
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