3-nitro-1,2,4-triazole-5-ketone superfining process

An ultra-fine, nitro-based technology, applied in the direction of organic chemistry, can solve the problems of large particle size, wide particle size distribution, and high cost of NTO, and achieve the effect of reducing labor intensity and production costs, and narrow particle size distribution.

Inactive Publication Date: 2006-02-15
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a kind of 3-nitro-1 in order to solve the problems in the prior art that the NTO recrystallization preparation process is complicated, the cost is high, especially the prepared NTO particle size is relatively large, and the particle size distribution is wide. Ultrafine process of 2,4-triazol-5-one

Method used

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  • 3-nitro-1,2,4-triazole-5-ketone superfining process

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Embodiment 1

[0020] A superfine process of 3-nitro-1,2,4-triazol-5-one, the solvent selected is acetone. First, dissolve the NTO raw material with large particle size and rod shape or needle shape in acetone and heat the acetone solution in a water bath. The temperature of the water bath is controlled at 48°C; After the oxazol-5-one was completely dissolved, the temperature of the water bath was raised to 59° C.; vacuum distillation was started, and the vacuum degree was controlled at 0.03 MPa during the vacuum distillation. When 75% of the acetone is evaporated, the stirring is stopped, and the distillation is continued until the acetone is completely evaporated, so that ultra-fine NTO particles can be obtained.

[0021] The evaporated acetone can be condensed and collected for reuse.

Embodiment 2

[0023] A superfine process of 3-nitro-1,2,4-triazol-5-one, the solvent selected is acetone. First, dissolve the NTO raw material with large particle size and rod shape or needle shape in acetone and heat the acetone solution in a water bath. The temperature of the water bath is controlled at 50°C; After the oxazol-5-one is completely dissolved, the temperature of the water bath is raised to 61°C to start vacuum distillation. During the process of vacuum distillation, the vacuum degree is controlled at 0.035MPa; when the acetone evaporates 80%, stop stirring and continue the distillation until the acetone is completely evaporated , that is, ultra-fine NTO particles can be obtained.

[0024] The evaporated acetone can be condensed and collected for reuse.

Embodiment 3

[0026] A superfine process of 3-nitro-1,2,4-triazol-5-one, the solvent selected is acetone. First, dissolve the NTO raw material with large particle size and rod shape or needle shape in acetone and heat the acetone solution in a water bath. The temperature of the water bath is controlled at 52°C; After the azole-5-one is completely dissolved, the temperature of the water bath is raised to 62°C to start vacuum distillation. During the process of vacuum distillation, the vacuum degree is controlled at 0.034MPa; when the acetone is evaporated to 85%, stop stirring and continue the distillation until the acetone is completely evaporated , that is, ultra-fine NTO particles can be obtained.

[0027] The evaporated acetone can be condensed and collected for reuse.

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Abstract

The invention provides a recrystallization process for refining 3-nitro-1,2,4-triazole-5-one, which comprises heating acetone through water-bath, controlling the temperature between 48-52 deg. C, completely dissolving 3-nitro-1,2,4-triazole-5-one, vacuum distilling, controlling the vacuity between 0.03-0.04 MPa, finally evaporating acetone completely to obtain the ultra-fine NTO particles.

Description

technical field [0001] The invention relates to a recrystallization process for refining 3-nitro-1,2,4-triazole-5-one, specifically a 3-nitro-1,2,4-triazole-5-one Ultrafine process of ketones. Background technique [0002] 3-Nitro-1,2,4-triazol-5-one (NTO for short) is a new type of high-density, low-sensitivity, easy-to-form elemental explosive. Its energy is close to that of RDX, and its sensitivity is close to that of TNT. It is mainly used to manufacture low-vulnerability plastic bonded explosives. Its safety performance is better than that of B explosives (the mixed explosive of TNT and RDX), and its energy is close to that of B explosives. It can replace TATB as an active desensitizer for HMX-based mixed explosives. The preparation of metal 3-nitro-1,2,4-triazol-5-one salts from 3-nitro-1,2,4-triazol-5-one can be used as energetic catalysts in propellants, Therefore, it is more attractive than ordinary explosives RDX, TNT and HMX in practical applications. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/10
Inventor 柴涛张景林宋小兰
Owner ZHONGBEI UNIV
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