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Simple preparation method for explosive solvate

A technology for solvates and explosives, applied in the direction of organic chemistry, etc., can solve the problems such as the bonding of explosive powder particles into blocks, affecting the assembly effect of solvates, and being prone to desolvation, etc., so as to avoid dissolution or agglomeration. Good experimental reproducibility, beneficial to mass production

Active Publication Date: 2018-03-23
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method tries to heat the solvent by means of water bath, oil bath or electric heating to generate hot solvent vapor, and then form a solvate with the explosive, but the solvent molecules in the solvate of many explosives have a large solubility for the explosive itself, if When assembling with hot solvent vapor, the concentration of solvent vapor is very high, which will dissolve the surface of explosive crystals, causing many explosive powder particles to stick into blocks or dissolve, thus affecting the assembly effect of solvates
In addition, some solvates are unstable under the action of thermal stimulation, and desolvation is very easy to occur, so it is very likely that solvates cannot be formed or the purity of the solvates formed is not high under such hot solvent conditions.

Method used

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  • Simple preparation method for explosive solvate
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  • Simple preparation method for explosive solvate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Spread 10g of Oktogen (HMX) explosives on a surface dish with a diameter of 120mm, and measure 40g of N,N-dimethylformamide (DMF) solvent in a 150ml conical flask , and then put the watch glass and Erlenmeyer flask together in a glass desiccator with a volume of 2 L.

[0034] (2) Use a vacuum pump to vacuumize the desiccator. After the vacuum reaches 0.5 bar, stop vacuuming and close the valve.

[0035] (3) At room temperature, DMF solvent vapor and HMX explosives undergo gas-solid reaction in a desiccator for 8 hours, then open the vacuum valve to restore the desiccator to normal pressure, and then take out the solid sample, which is the obtained HMX / DMF explosive solvent compounds.

[0036] as attached figure 2 , 3 shown, with figure 2 Shown in a and b are the X-ray powder diffraction spectrograms of the HMX raw material and the solvate, and it can be seen that the raw material HMX has all been converted into the solvate at this time. attached image 3A an...

Embodiment 2

[0038] (1) Spread 10g of Octojin (HMX) explosives on a surface dish with a diameter of 120mm, measure 60g of N-methylpyrrolidone (NMP) solvent in a 150ml conical flask, and then surface The dish and Erlenmeyer flask were placed together in a glass desiccator with a volume of 2 L.

[0039] (2) Use a vacuum pump to vacuumize the desiccator. After the vacuum degree reaches 0.01 bar, stop vacuuming and close the valve.

[0040] (3) At room temperature, NMP solvent vapor and HMX explosives undergo gas-solid reaction in a desiccator for 1 day, then open the vacuum valve to restore the desiccator to normal pressure, and then take out the solid sample, which is the obtained HMX / NMP explosive solvent compounds. as attached figure 2 Shown in c is the X-ray powder diffraction spectrogram of this solvate, shows that raw material HMX has all been converted into solvate at this moment. attached image 3 Where c is the topography of the solvate, it can be seen that the solvate crystal p...

Embodiment 3

[0042] (1) Spread 10 g of hexanitrohexaazaisowurtzitane (CL-20) explosives on a surface dish with a diameter of 120 mm, and measure 100 g of hexamethylphosphoryl trisulfite in a 150 ml conical flask Amine (HMPT) solvent, and then put the watch glass and Erlenmeyer flask together in a glass desiccator with a volume of 2L.

[0043] (2) Use a vacuum pump to vacuumize the desiccator. After the vacuum degree reaches 0.001 bar, stop vacuuming and close the valve.

[0044] (3) At room temperature, after the gas-solid reaction between HMPT solvent vapor and CL-20 explosive in the desiccator for 1 day, open the vacuum valve to restore the desiccator to normal pressure, and then take out the solid sample, which is the obtained CL-20 / HMPT explosive solvate. attached Figure 4 Shown in a and b are the X-ray powder diffraction spectra of the CL-20 raw material and the solvate. It can be seen that the raw material CL-20 has been completely converted into a solvate at this time. attached...

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Abstract

The invention discloses a simple preparation method for explosive solvate. The simple preparation method comprises the following key steps: under a normal temperature condition, placing explosive rawmaterials and a solvent in a sealed environment separately, slowly volatilizing the solvent through vacuuming, generating solvent steam of low pressure and low concentration, enabling the solvent steam to freely diffuse to the surface of explosive crystal, and inducing a gas-solid reaction, thereby obtaining the explosive solvate. The explosive solvate prepared by using the method is of a micro crystal cluster structure and has relatively low temperature, and a primary template can be provided for later explosive micro structure regulation and control. The method has the characteristics of being simple in process procedure, gentle in experiment condition, rapid and efficient in preparation, free of pollution, low in cost, and the like, and is particularly applicable to on-scale preparation.

Description

technical field [0001] The invention relates to a preparation method of explosive crystals, in particular to a simple preparation method of explosive solvate. Background technique [0002] Explosive solvates belong to the field of supramolecular chemistry. They are supramolecular compounds composed of explosives as the main molecule and solvent as the guest molecule. They are also called pseudopolymorphs, solvent adducts, complexes or molecular intercalations. Explosive solvates have broad application prospects. Explosive solvates can be used as initial templates for the disassembly of supramolecular compounds, thereby realizing the regulation of the microstructure of explosives. Moreover, after the explosive and the solvent form a solvate, it has certain application value in the process of purifying, separating and recovering the explosive. In addition, some explosives have high sensitivity and poor safety. After the formation of solvate crystals, their sensitivity may be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/02C07D487/22
CPCC07D257/02C07D487/22
Inventor 徐金江孙杰田勇刘渝张浩斌
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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