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A kind of preparation method of β-phase RDX gold

A RDX and substrate technology, applied in the field of energetic materials, can solve few problems such as sublimation and recrystallization, and achieve the effect of simple and easy operation

Active Publication Date: 2019-02-01
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Almost all energetic materials have a sublimation process before their melting point, but most of the researches focus on the research on the sublimation rate, and the method of sublimation recrystallization is rarely used in sample preparation. The present invention considers the use of sublimation recrystallization Preparation of β-phase RDX by Crystallization

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preparation example Construction

[0028] The invention provides a method for preparing β-phase RDX, characterized in that it comprises:

[0029] A) Place RDX under the substrate, heat it to a temperature greater than or equal to the sublimation temperature of RD, keep it warm, and obtain β-phase RD on the substrate after cooling; the RD is α-phase black Sorkin or a mixture of α-phase RDX and β-phase RDX.

[0030] Among them, the present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0031] The raw material used in the present invention is RDXG, which is α-phase RDXOGIN or a mixture of α-phase RDXOGIN and β-phase RDXOGIN.

[0032] RDX is placed under the substrate; the substrate is preferably a quartz substrate, a silicon wafer substrate or a stainless steel substrate; in the present invention, preferably RDX is placed in the sample heating chamber, and the substrate is placed Above the sample heating chamber.

[0033] Then heated to a sublimat...

Embodiment 1

[0045] Example 1: Using a silicon wafer as a substrate

[0046] 1.1 figure 1 is the thermogravimetric spectrum of RXD particles, figure 2 is the weight evolution spectrum of RXD particles with time at 160°C; from figure 1 and figure 2 It can be concluded that the sublimation point of RDX particles is 160°C.

[0047] 1.2 Use a (111)-oriented silicon wafer as a substrate, place the substrate above the heating chamber, and place two RDX particles in the heating chamber.

[0048] 1.3 According to the heating rate of 20°C / min, heat the RDX particles to 190°C and hold for 5 minutes: adopt the sequential heating mode, follow the normal temperature—100°C for 5 minutes—heat to 120°C for 5 minutes—140°C for 5 minutes—160°C Keep warm for 5 minutes—190°C for 5 minutes. Cool down to room temperature naturally.

[0049] 1.4 Remove the substrate, and do a Raman spectrum test on the crystal on the substrate, such as image 3 ,Such as image 3 is the Raman spectrogram of the crystal ...

Embodiment 2

[0054] Example 2: Using Metal as a Substrate

[0055] 2.1 from figure 1 and figure 2 It can be concluded that the sublimation point of RDX crystal is 160°C.

[0056] 2.2 Use stainless steel as the substrate, place the substrate above the heating chamber, and put two RDX particles in the heating chamber.

[0057] 2.3 According to the heating rate of 20°C / min, heat the RDX particles to 190°C and keep it warm for 5 minutes. We adopted the mode of sequential heating, according to normal temperature—100°C for 5 minutes—120°C for 5 minutes—140°C for 5 minutes—160°C for 5 minutes—190°C for 5 minutes. Cool down to room temperature naturally.

[0058] 2.4 Remove the substrate, do Raman spectrum test on the crystal on the substrate, and adopt statistical method, take 100 data points to analyze that the proportion of β phase is 98%.

[0059] 2.5 Lower the temperature to 160 degrees centigrade, repeat (2) (3) (4), adopt statistical methods, adopt 100 data points to analyze that the ...

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Abstract

The invention provides a preparation method for beta-phase hexogen. The preparation method comprises the following steps: placing hexogen below a substrate, carrying out heating to a temperature greater than or equal to the sublimation temperature of hexogen, then carrying out heat preservation and carrying out cooling so as to obtain beta-phase hexogen on the substrate, wherein the hexogen is alpha-phase hexogen or a mixture of alpha-phase hexogen and beta-phase hexogen. Compared with the prior art, the invention has the following advantages: the method prepares high-purity beta-phase hexogen by using a combination of vapor phase method and a sublimation-recrystallization method since an energy-containing material undergoes sublimation before melting and decomposition and alpha-phase hexogen and beta-phase hexogen are slightly different in the aspect of energy; the method is simple and easy to operate; since the method is implemented at a temperature lower than the decomposition temperature of hexogen and no toxic chemical reagent is used in the whole process of preparation, the method is a safe preparation method; the phase of prepared RDX can be controlled by regulating and controlling time or temperature; and the beta-phase hexogen prepared by using the method can be preserved for a long time under conventional conditions.

Description

technical field [0001] The invention belongs to the technical field of energetic materials, and in particular relates to a preparation method of β-phase RDX. Background technique [0002] Energetic materials refer to compounds or mixtures that can independently undergo chemical reactions and release a large amount of energy without external oxygen supply. Both RDX and HMX are typical and commonly used energetic materials, which are widely used in the production of high explosives and are famous for their good stability and huge explosive power. RDX (C 3 h 6 N 6 o 6 ) is 1,3,5-trinitro-1,3,5-triazacyclohexane, also known as Hexogen, which is currently the main explosive species and is widely used as an important component of propellants and propellants part. Under normal conditions, the RDX crystal structure belongs to the orthorhombic system, and there are four crystal phases α, β, γ, δ, ε, among which the α phase is a normal temperature and pressure phase; It is easy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/06
CPCC07B2200/13C07D251/06
Inventor 张增明郜婵代如成王中平
Owner UNIV OF SCI & TECH OF CHINA