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Synthesizing method of deuterated octogen

A technology of octogen and synthesis method, which is applied in the field of preparation of organic compounds and can solve problems such as synthesis that has not yet been reported.

Inactive Publication Date: 2017-07-25
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are many synthetic methods about non-deuterated HMX, but for deuterated Octojin (abbreviated as HMX-d) with high purity and high deuterated rate 8 ) synthesis has not been reported yet

Method used

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  • Synthesizing method of deuterated octogen
  • Synthesizing method of deuterated octogen
  • Synthesizing method of deuterated octogen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] A kind of synthetic method of deuterated Octogen, the steps are as follows:

[0070] 1) Put 1.0g of deuterated paraformaldehyde in a 25mL two-neck round bottom flask, add 2.0mL of deionized water, add 3.0mL of ammonia water, and control the temperature at 15-50°C during the addition. After the feeding is completed, the temperature of the oil bath is controlled at 15-50°C to react for 68 hours. After the reaction is completed, part of the tert-butanol solution is added to the reaction solution. 95%.

[0071] 2) Put 0.4g of the synthesized deuterated urotropine in a 25mL two-necked round-bottomed flask, add 0.2g of ammonium acetate, and dropwise add 0.8g of acetic anhydride. The reaction was carried out for 1 h at room temperature, and then the reaction was continued for 1 h at room temperature. Heat in an oil bath and keep the system temperature at 25-35°C for 40 hours. Cool to get DAPT-d 10 The reaction solution can be directly used in the next reaction without puri...

Embodiment 2

[0075] A kind of synthetic method of deuterated Octogen, the steps are as follows:

[0076] a. Dissolve deuterated formaldehyde substances in the solvent at 0°C, add ammonia compounds, keep the reaction temperature at 0°C, and react for 100 hours. After the reaction is completed, the solvent is distilled off, and the residue is the prepared deuterated urethane Tropin (referred to as HMTA-d 12 );

[0077] The deuterated formaldehyde substance can be a 5% deuterated formaldehyde aqueous solution or deuterated paraformaldehyde;

[0078] The solvent may be one or a mixture of two or more of water, alcohol, halogenated hydrocarbon, ether, amide, sulfoxide, and hydrocarbon compounds;

[0079] The ammonia compound can be ammonium salt, ammonia gas, ammonia water, liquid ammonia or an organic solution of ammonia gas;

[0080] Convert deuterated formaldehyde substances into deuterated formaldehyde measurement, the molar amount of deuterated formaldehyde and NH 3 The ratio of the mo...

Embodiment 3

[0094] A kind of synthetic method of deuterated Octogen, the steps are as follows:

[0095] a. Dissolve deuterated formaldehyde substances in the solvent at 70°C, add ammonia compounds, keep the reaction temperature at 70°C, and react for 1h. After the reaction is completed, the solvent is distilled off, and the residue is the prepared deuterated urethane Tropin (referred to as HMTA-d 12 );

[0096] The deuterated formaldehyde substance can be deuterated formaldehyde aqueous solution or deuterated paraformaldehyde with a mass percentage content of 60%;

[0097] The solvent may be one or a mixture of two or more of water, alcohol, halogenated hydrocarbon, ether, amide, sulfoxide, and hydrocarbon compounds;

[0098] The ammonia compound can be ammonium salt, ammonia gas, ammonia water, liquid ammonia or an organic solution of ammonia gas;

[0099] Convert deuterated formaldehyde substances into deuterated formaldehyde measurement, the molar amount of deuterated formaldehyde a...

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Abstract

The invention discloses a synthesizing method of deuterated octogen. The synthesizing method is characterized by comprising the following steps of enabling a deuterated formaldehyde matter and an ammonia compound to react, so as to obtain an intermediate, namely deuterated urotropine; further acetylizing and nitrifying, so as to obtain an intermediate, namely 1,5-diacetyl-3,7-binitro-1,3,5,7-teraazamacrocycle octane; using nitric acid / phosphorus pentoxide to nitrify, so as to obtain the product with high selectivity, namely deuterated octogen. The deuterated octogen synthesized by the method has the advantages that the purity is high, the deuterating rate is high, and the deuterated octogen can be applied to the fields of neutron diffraction, energetic material study, analysis and detection, and the like.

Description

technical field [0001] The invention belongs to the preparation of organic compounds, and relates to a synthesis method of deuterated octogen. The deuterated octogen prepared by the invention has high purity and high deuteration rate, and is suitable for the fields of neutron diffraction, energetic material research, analysis and detection, and the like. Background technique [0002] Octogen, whose code name is abbreviated as HMX, and its chemical name is ammonium cyclotetramethylene tetranitrate. HMX is relatively stable in chemical properties and is a simple explosive with excellent thermal stability, so it can be used to prepare heat-resistant explosives and gunpowder. When the density is 1.89~1.90g / cm 3 , the detonation velocity is 9110m / s, and the detonation pressure is 29.5GPa. HMX can be used to prepare various high-energy explosives, high-energy solid propellants and high-energy propellants, and can also be used to prepare high-energy solid propellants with high s...

Claims

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Application Information

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IPC IPC(8): C07D257/02
CPCC07D257/02C07B2200/05
Inventor 杨海君白亮飞邹林孙光爱龚建胡刚
Owner SOUTHWEAT UNIV OF SCI & TECH
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