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Spherical NTO (3-nitro-1,2,4-triazol-5-one) crystal with high crystalline density and preparation method

A technology of crystal density and spheroidization, applied in chemical instruments and methods, crystal growth, single crystal growth, etc., can solve the problems that NTO crystals cannot be directly applied, achieve mild reaction conditions, simple operation, and increase energy output.

Inactive Publication Date: 2016-01-27
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] U.S. Patent USH000990 points out that NTO is dissolved in DMSO solution at 70°C, and the DMSO solution of NTO is injected into methylene chloride solution at room temperature through a special nozzle to obtain 0.4-0.7mm spherical NTO crystals, which are directly synthesized in the prior art. Crystals cannot be directly applied due to reasons such as particle size and morphology

Method used

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  • Spherical NTO (3-nitro-1,2,4-triazol-5-one) crystal with high crystalline density and preparation method

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preparation example Construction

[0016] The present invention also provides a method for preparing the high crystal density spheroidized NTO crystal, the method comprising the following steps:

[0017] (1) Add NTO and solvent into the reactor for full dissolution, and the temperature of the reactor is 40-80°C;

[0018] (2) Lower the temperature of the reactor while stirring, and form a supersaturated solution to generate and grow crystal nuclei;

[0019] (3) After the crystals are completely precipitated, stir at a low temperature of -5-0°C for 1-5 hours;

[0020] (4) Filtration, drying and weighing.

[0021] The present invention has no special limitation on the heating method of the reactor, as long as it can play the role of heating the materials in the reactor. Preferably, a jacket can be provided outside the reactor, and hot water is introduced into the jacket for heating the reactor.

[0022] Preferably, the solvent in step (1) is at least one of absolute ethanol, dimethyl sulfoxide, nitrogen methylp...

Embodiment 1

[0036] 500 g of NTO, 3 L of nitrogen methyl pyrrolidone and 7 L of absolute ethanol were added into a 20 L reactor, and the reactor was placed in a constant temperature water bath at 40°C. Turn on the stirrer, the stirring rate is 300rpm, and at the same time, control the cooling device to circulate the cooling liquid to the jacket of the reaction kettle, and the cooling rate is 5°C / min. When the temperature of the solution in the reaction kettle drops to 0°C, the cooling is stopped, and the temperature is kept and stirred for 2 hours. Filter, dry and weigh. The crystal weight is about 420 g, and the yield is 84%. According to the experimental determination, the NTO content is ≥99.9%, and the crystal density is 1.922g / cm 3 , the ratio of short and long axes of the crystal is 0.95; the median particle size of the crystal is 180 μm, and the particle size distribution is narrow. figure 1 It is an electron micrograph of the high crystal density spheroidized NTO crystal obtained...

Embodiment 2

[0038] Add 1000 g of NTO, 3.1 L of nitrogen methyl pyrrolidone and 9.3 L of distilled water into a 20 L reactor, which is placed in a constant temperature water bath at 50°C. Turn on the stirrer, the stirring rate is 200rpm, and at the same time, control the cooling device to circulate the cooling liquid to the jacket of the reaction kettle, and the cooling rate is 6°C / min. When the temperature of the solution in the reaction kettle drops to 0°C, the cooling is stopped, and the temperature is kept and stirred for 2 hours. Filter, dry and weigh. The crystal weight is about 780 g, and the yield is 78%. According to the experimental determination, the NTO content is ≥99.9%, and the crystal density is 1.92g / cm 3 , the ratio of the short and long axes of the crystal is 0.90; the median particle size of the crystal is 150 μm, and the particle size distribution is narrow. Appearance Observation The crystal has high sphericity, smooth surface and no cracks on the crystal plane.

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Abstract

The invention provides a spherical NTO (3-nitro-1,2,4-triazol-5-one) crystal with high crystalline density and a preparation method of the spherical NTO crystal. The content of NTO in the crystal is larger than or equal to 99.9%, the crystal density is larger than or equal to 1.92 g / cm<3>, the short and long axis ratio of the crystal is larger than or equal to 0.90, and the range of the median particle diameter of the crystal ranges from 150 mu m to 200 mu m. The preparation method of the spherical NTO crystal with the high crystalline density comprises steps as follows: (1), NTO and a solvent are added into a reaction kettle for complete dissolution, and the temperature of the reaction kettle is 40-80 DEG C; (2), the temperature of the reaction kettle is reduced while stirring is performed, a super-saturated solution is formed, and a crystal nucleus is generated and grows; (3), after the crystal is completely separated out, stirring is performed for 1-5 hours at the low temperature ranging from subzero 5 DEG C to zero DEG C; (4), filtering, drying and weighing are performed. The crystal grain fineness distribution is narrow, appearance observation proves that the sphericity of the crystal is high, the crystal has a smooth surface, and no crack is formed on the surface of the crystal.

Description

technical field [0001] The invention relates to the field of energetic crystal materials, in particular to a high crystal density spheroidized 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) was first synthesized by Manchot and Loll in 1905, But it was not until 1983 that it was developed into an energetic material by the Los Alamos Laboratory in the United States. With the emphasis on high-energy and low-sensitivity single-mass explosives, NTO has gradually become one of the hot spots of researchers. NTO density up to 1.93g / cm 3 , it is reported that its detonation energy is close to that of RDX, and its sensitivity is close to that of triaminotrinitrobenzene (TATB). The NTO crystals directly prepared by the reaction are typical jagged rod-like crystals, and are easy to aggregate, which will cause NTO crystals to be sensitive to sudden impact. [0003] When NTO is used in mixed ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/54C30B7/08
Inventor 郭学永卢佳骥焦清介张静元张朴崔超张洪垒李航
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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